Method of producing fatty acid esters from squashed oilseed

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method of producing fatty acid esters, which are used as diesel biofuel, from whole oilseeds, involving the following consecutive steps: a) preheating unhulled and cleaned whole seeds; b) squashing the oilseeds together with their shells; c) drying the squashed seeds until achieving water and volatile substance content of 0.5-2.5%; d) re-esterification by bringing the squashed seeds into contact with an alcohol medium in the presence of a catalyst; e) separating the liquid and solid phases obtained from re-esterification; f) neutralising the liquid phase obtained at step (e); and g) removing alcohol and separating glycerol from fatty acid esters, which are then purified. The invention also relates to a method of producing an oil cake, meant for use as animal feed, from the obtained solid phase, which involves the following steps: 1) removing alcohol from said solid phase; and 2) adding glycerol obtained at step (g) of the method on any of the previous claims.

EFFECT: method of obtaining fatty acid esters from squashed oilseeds.

25 cl, 12 tbl, 19 ex

 

The present invention relates to a new method of producing esters of fatty acids used, in particular, as of biodiesel from oilseed plants.

Diesel biofuel is a fuel obtained from vegetable or animal oil, transformed through a chemical process called transesterification, to obtain methyl esters of vegetable oils (MARM), which are derived from methyl alcohol, or a complex of ethyl esters of vegetable oils (EERP), is obtained by using ethyl alcohol. Diesel biofuel superior characteristics of vegetable oils used in its raw form, and petroleum diesel fuel, that is classic diesel fuel. Diesel biofuels can be used in engines alone or in blends with petroleum diesel fuel.

In the known methods of obtaining MARM EERP or crushed seeds either directly subjected to the interesterification reaction, or from seeds extracted oil, make a preliminary refining this oil, then perform step interesterification procedendo neutral oil. However, these known methods cannot be called satisfactory. In the first case, on an industrial scale seeds need to grind all the ü finely, to ensure the highest possible output, but at this stage of the phase separation becomes more difficult the more thinner you want to grind the seeds. In the second case, the extraction of oil and pre-processing makes industrial application of the method is complicated and expensive.

Previously described other methods of obtaining, in particular, proposed by Khalil and co-authors (GEE 2005.0011112) and Haas and co-authors (US 2006.0155138). Instead of grains in the proposed methods use the "flakes", derived from the husked grains. These flakes get in large quantities in agriculture, but their use for the production of biodiesel has certain disadvantages: on the one hand, the flakes are more fragile than whole seeds, which leads to the formation of fine particles must be filtered out to use oil as biodiesel; on the other hand, the output MARM and EERP is reduced due to the lack of shells of seeds; and finally, the formation of these flakes requires the use of expensive plants to bring to the condition.

The object of the present invention is a method of obtaining esters of fatty acids from seeds of oleaginous plants, which provides high output and simultaneously eliminates the disadvantages of the known methods.

The first object of the present is subramania is a method of obtaining esters of fatty acids, used as biodiesel, from the whole seeds of oilseed plants, characterized in that it comprises the following successive stages:

A. Preheating popularnych whole seeds;

b. Crushing oilseeds together with their casing;

Stuchka flattened seeds until the water content and volatile matter from 0.5 to 2.5%, preferably from 1.5% to 2%;

d. Transesterification by contact flattened seeds with an alcoholic medium in the presence of a catalyst;

that is, the Separation of the liquid and solid phases obtained by interesterification;

f. Neutralization of the liquid phase obtained in step e); and

g. Remove alcohol and separating the glycerol from the fatty acid esters.

Under "oil seeds" should be understood any plant seeds containing an oil substance, preferably with a high content of triglycerides. Therefore, this category also includes sprouts, seeds, nuts, and seeds. In addition, oil seeds contain protein, fiber and minerals.

Preferably seeds choose among seeds of cultivated plants. For example, you can use canola seed, Orchid, peanut, castor, sesame, sunflower, Sapporo, soybean, lupine, flax linen, cotton. Preferred are rapeseed, sunflower and Orchid. Most of predpochtitel the tion are rapeseed.

In addition, you can also use rape seed, peanut, castor, sesame, sunflower, Sapporo, soybean, lupine, flax linen, cotton.

In the framework of the method in accordance with the present invention, the seeds can be used fully or partly in the shell. In the framework of the present invention, the term "oleaginous seeds" refers to whole seeds or partially husked seeds. For example, in the case of rapeseed, sunflower and Orchid preferably mostly use whole seeds, i.e. retains at least 80% of its sheath. It forms a fibrous base, to avoid the collapse of flattened grain during contact with the alcohol environment on stage d) interesterification.

However, if the shell is too large compared to the core of the grain (for example, in the case of the shell Australian macadamia nut, Brazil nut, walnut, Andiroba, coconut, walnut oil wood or walnut)), preferably the grain is cleaned from the part of the shell, so as not to disrupt the interesterification reaction. Sometimes it is preferable to grind the kernels of the seeds if they are large (for example, in the case of macadamia nuts, Brazil nut, walnut, Andiroba, coconut, nut tree oil or nuts)).

At the stage b) of the method in accordance with izaberete the receiving produce the crushing of oilseeds. In this case, as a rule, they have the form of thin elongated leaves, flakes or scales.

Before stage flatten preferably the seeds are cleaned, removing solid impurities, such as stones, scraps, metal particles, dust.

Preferably the thickness of the flattened seeds is in the range from 10 μm to 1 mm According to a preferred variant implementation, the thickness of the flattened seeds is in the range from 0.1 mm to 0.3 mm, and more preferably the thickness of the flattened seeds less than 0.2 mm, in particular, in the case of rapeseed.

In addition, the size of the flattened seeds, i.e. their length or width is preferably in the range from 3 to 5 mm, in particular, in the case of rape seed and other seeds of similar size, where size is approximately 4 mm

According to the private option run, oilseeds can be preheated to a temperature of from 40°to 60°C, preferably 50°C to phase b) flatten to improve their ductility. However, the seeds are heated to this temperature only during the time necessary to achieve the desired plasticity. Indeed, it is preferable to avoid drying of seeds, leading to their fragmentation at the time of flattening. Before crushing the seeds in any case be subjected to roasting or drying.

Therefore, oilseeds can be subjected to preliminary heating at a temperature of from 50 to 55°C for 5-60 min, preferably for 30 min before carrying out step b) flatten, if necessary, in the atmosphere of water vapor.

According to the present invention, preferably, the crushing of oilseeds produced with the assistance of the rolls, which may be of any type, in particular, smooth or corrugated, but preferably smooth. Their diameter can reach up to 80 cm Gap between the rollers is preferably less than 0.2 mm and more preferably less than 0.1 mm

The speed of rotation of the rolls define in such a way as to avoid crushing of seeds during flattening. Preferably the diameter and speed of rotation of the rolls are the same, in order to avoid phenomena of rupture and, therefore, the crushing of the seeds.

According to the private option run, crushing oilseeds produced using smooth rolls, preferably in a single pass.

Step b) flattening is the main step of the method, as it allows you to get a much higher yield than without flattening, that is the best solution when interesterification and the best solution at the extraction of ethyl esters.

After the step of flattening the seeds as soon as possible be subjected to drying to stop enzymatic activity and to avoid, therefore, the decomposition of substances contained in them. So about the time, step (C) drying carried out immediately after step b) flatten, not later than 24 hours after step (b) flatten, preferably less than 2 hours after step (b) flatten, and more preferably within one hour after flattening. In addition, due to drying, flattened seeds can be stored up to stage d) interesterification. Drying flattened seeds is carried out in such a way as to obtain the water content and volatile matter in the range from 0.5 to 2.5%, preferably from 1.5% to 2%.

The water content and volatile matter seeds are determined according to method NF V 03-909.

According to the private option execution stage (C) drying is carried out at a temperature in the range of 50 to 100°C., preferably in the range from 70°C to 90°C.

After step (C) carry out drying stage interesterification by contact of the dried, flattened seeds with an alcoholic medium in the presence of a catalyst. The catalyst is a basic or acid, preferably the main one.

Alcoholic medium may contain one or more alcohols selected from alcohols of C1-C6, such as methyl alcohol or ethyl alcohol, if necessary, in a mixture with one or more aliphatic hydrocarbons, such as hexane. Preferably the alcohol environment is ethyl alcohol containing water in an amount less than 5000 frequent the th ppm preferably 3000 parts per million.

Preferred basic catalyst is anhydrous and homogeneous, and it can be selected from the group comprising sodium, potassium, carbonate or bicarbonate of sodium or potassium or sodium carbonate or potassium methylate or ethylate of sodium or potassium.

The acid catalyst may be, for example, sulphuric acid.

Before you begin the stage of transesterification, preferably, in periodic mode, flattened seeds pre-enter in contact with the alcohol environment that leads to their impregnation of this alcohol environment and promotes subsequent transesterification. Pre-impregnation can be carried out during the period from 10 to 30 min, preferably for 30 minutes at a temperature in the range of 40 to 80°C., preferably at a temperature of 75°C. This step is recommended if the reaction is carried out in a continuous mode.

To optimize the output of the interesterification reaction, the mass ratio of catalyst/flattened seeds is preferably from 0.5/100 to 2/100, and/or the mass ratio of alcohol/ flattened seeds is preferably from 100/100 to 500/100.

If the process is periodic, preferably the interesterification reaction is carried out at a temperature of from 45 to 55°C. and preferably at a temperature approximately equal to the 50°C, during the time from 10 min to 2 hours, preferably from 20 to 40 minutes

According to the private option run, contact, flattened seeds with an alcoholic medium during the step d) interesterification is carried out with slow stirring or by wetting and percolation. Preferably it is carried out by percolation alcohol medium containing the catalyst, through the flattened seeds. In practice, the percolation can be achieved by wetting layer flattened seeds, the height of which is preferably approximately 80 cm

After step interesterification produces the separation of the liquid and solid phases obtained in the result of the transesterification, preferably by removal of the liquid. The obtained liquid phase is saturated esters of fatty acids, obtained by the interesterification reaction.

Preferably the residual oil content of the substance in the solid phase, i.e. in the meal should be less than 1 wt.% of the total weight of dry substance.

To extract the rest of the esters of the fatty acids in the solid phase, you can perform the following additional steps:

h) extracting the alcohol from the specified solid phase obtained in step d);

i) collecting the solid phase;

j) filtering and combining the liquid phase obtained in stage e) re is terifically and h) extraction.

The combined liquid phase obtained in stage e), can be filtered, for example, on a grid with a cell diameter of 10 to 50 μm, to remove all small particles.

Preferably step (h) the extraction is carried out by countercurrent percolation with alcohol at a mass ratio of alcohol/flattened seeds that are in the range from 100/100 to 200/100.

In addition, the alcohol used in step (h) extraction, you can choose among the alcohols of C1-C6, for example, ethyl alcohol containing water in an amount of less than 5000 parts per million, preferably less than 3000 parts per million.

After that, the liquid phase resulting from stage (e) interesterification, if necessary, with the addition of the liquid phase obtained in stage h) extraction, neutralize or using acid, if the catalyst of the reaction is the basis, or by using a framework, if the catalyst of the reaction is acid.

Preferably the acid is chosen from the group comprising sulfuric acid, hydrochloric acid, phosphoric acid, citric acid or acetic acid.

The base may be, for example, soda.

The amount of acid added to the liquid phase, determined so that the content of fatty acids in complex ethyl esters of fatty acids remained less than 0.25% (equivalent to an acid number of <0.5 mg KOH/g).

Not what tralization liquid phase produced in part, in order not to increase its content of soap.

According to the private option execution, acid neutralization add in number, leading to the pH close to 10, in particular in amounts of less than 0.04% of the total number of esters of fatty acids present in the specified liquid phase.

After step (f) neutralizing the alcohol is removed from the liquid phase and produce separation from glycerol esters of fatty acids.

Removal of the alcohol is preferably carried out by evaporation at a temperature of from 50 to 100°C. under a pressure of from 200 to 1000 mbar, preferably at a temperature of about 80°C at atmospheric pressure to obtain a residual volume of less than 1%.

The separation of glycerol from esters of fatty acids preferably produced by centrifugation at a temperature of from 60 to 80°C. It can also be done by settling into a calm state. Glycerin draws a major part of the impurities, such as catalyst, soap, phosphate derivatives or sodium sulfate.

After that, esters of fatty acids washed with water, preferably at about 80°C to remove impurities, and then separated from the wash water, in particular, by sedimentation or centrifugation, preferably at a temperature of 80°C, then dried, preferably by steam the cation at a temperature of from 90 to 100°C. under pressure of about 200 mbar to obtain a residual water in quantities of less than 500 ppm relative to the total amount of dry matter. Thus obtained esters of fatty acids then after cooling it is possible to bring to the condition in the atmosphere of nitrogen.

The second object of the present invention is a method of obtaining a meal intended for use as animal feed, from the solid phase resulting from step e) or step i) the above-described method of producing esters of fatty acids, containing the following steps:

1) Removing alcohol from the specified solid phase; and

2) Adding glycerol obtained in stage g) of the specified method of producing esters of fatty acids.

In addition, the solid phase obtained in step 1), you can add the wash water indicated earlier in the production method of esters of fatty acids. The solid phase obtained in step e) or (i) of the specified method of producing esters of fatty acids, contains from 50 to 65 wt.% the alcohol. Removing alcohol from this solid phase can be produced mechanically by means of pressing or squeezing, then heat through entrainment with water vapor to obtain a residual amount of water less than 500 ppm relative to the total dry substance.

The final cake obtained in step 2), you can then bring to the condition in the form of a powder or be subjected to extrusion.

Remote alcohol can be collected, then the subject is the fact dehydration for reuse in the production method of esters of fatty acids.

The following examples illustrate the present invention and its advantages.

Abbreviations used in the examples shown in the following table 1a:

Table 1a
OptionsUnitValueMeasurement method
THRwt.%The content of residual moistureTermbase
THR 95: defined at 95°C
THR 105: determined at 105°C
Iamg KOH/gAcid number (measuring the content of free fatty acids)NFEN14104(T60-702)
IpmEq O2/kgPeroxide number(measuring concentration of peroxide
-oxidized oil substances)
NF T 60-220
TMG% dry matterThe content of oil-based substances (extraction with hexane in to conventional Soxhlet extractions)/td> V 03-908
TMV%The water content and volatile matter (103°C)NF V 03-909
MG extractable with hexane% dry matterThe content of oil-based substancesThe same method as for TMG, but at the same extraction

1) Preparation of seeds before crushing

The task of this first series of tests is to confirm the importance of pre-heating the dried seeds before crushing.

To do this, not dried, whole canola seed were delivered from agricultural farms in plastic bags and processed with changing temperature pre-heating in a drying oven at between 25, 35, 50 and 75°C (temperature T) and then the classic stages of flattening and drying (90°C for 12 hours). Finally, flattened and dried seeds enter into contact with anhydrous alcohol, which passes through the seed layer and is collected at the output of the fixed layer, and at more or less rapid percolation depending on initial conditions, pre-treatment of seeds (pre-heating and flattening). During these tests was measured to the number of extracted oil substances, and flow in percolation.

In particular, the work contains the following steps:

(1) preheating the whole not dried rapeseed in a temperature controlled oven at variable T°C (25, 35, 50 and 75°C) for 60 minutes;

(2) flattening preheated whole seeds;

(3) flattened seeds are placed in a temperature-controlled reactor with a porous layer at 25°C;

(4) then ethyl alcohol at 25°C. was added when the mass ratio of alcohol/seeds, equal to 1.9/1;

(5) passing through the layer of seeds ethanol is collected at the output of the fixed layer in the glass vessel. This measures the quantity of extracted oil substances and percolation.

The results of these tests are presented in table 1b.

Table 1b
The effect of preheating temperature on the amount of oil substances extracted from crushed seeds and the rate of percolation.
Preheating temperature, °C25355075
The preheat time, min 60606060
% oily substance extracted after percolation32313130
The flow rate of percolation, m3/h×m2a 12.714,6of 17.516,5

The temperature of the impregnation alcohol: 25°C, 15 minutes (the mass ratio of alcohol/seeds is equal to 1.9/1).

From the results shown in table 1, clearly shows that the best compromise between a flow rate of percolation and the percentage content of oil extracted substances reach at a temperature of pre-heating the seeds to 50°C. Indeed, at 50°C, all other things being equal, ethyl alcohol penetrates into flakes faster with the output of the extraction of oil equivalent with other conditions pre-heating of the seeds. From the point of view of industrial production, this allows to achieve higher processing speeds, as extracted oil substance is quickly transformed into esters in the presence of a catalyst. On the basis of these results by calculating the increase in production is titelliste at this stage compared to seeds without pre-heating (25°C) can be defined as +38%. Pre-heating the seeds to 70°C before flattening is not possible to improve the performance of the method, as almost equivalent to the output of the extraction (about 30%), flow percolation decreased very slightly (unlike pre-heating up to 50°C).

At temperatures over 70°C, the seeds can dry to flatten, with the result that they become more solid, which will lead to the formation of fine particles at the time of flattening.

2) Preparation of the dried, flattened seeds.

Preparation flattened and dried seeds is a very important step of the method in accordance with the present invention. It includes the following operations:

Seeds flat, to facilitate their drying, extraction, and conversion of oil substances in ester,

- Flattened seeds are dried to remove water. Were prepared and analyzed three categories of rape seed:

Seeds prepared according to method 1,

Seeds prepared according to method 2,

Seeds prepared according to method 3.

2.1) Flattened seeds, prepared according to method 1

According to the method 1, the crushing of rapeseed produced in the following conditions:

- by using rolls: or smooth rolls,

any corrugated rolls;any fresh seeds or dried seeds.

If seed is esplosivo fresh, after flattening them dried within 48 hours.

Flattened seeds were characterized by measuring the following parameters:

- the content of the oily substance obtained by extraction with hexane (to conventional Soxhlet extractions)

- THR 105 - the content of residual moisture at 105°C

Ia, an acid number in mg KOH/g (NF T 60-204)

- THR (residual moisture at 105°C. after drying at 80°C

- bulk density, kg/l

- rate of percolation, m3/h/m2

The results of these measurements and test conditions are presented in tables 2A and 2b.

The flow rate of percolation (l/h/m2)4
Table 2A
The influence of drying before and after flattening and conditions flatten
No.The gap between the rollers (mm)Quality seedsType rollsThe number of grooves/cmThe speed of rotation of the rollsThe content of the received
s3oil substances2(%SW)
THR 105 (%)Ia (mg KOH/g)THR after drying at 80°C (%)Bulk density (g/l)
10,05freshcorrugated8525 before
525 rear
43,429,482,862,9241010264,5
1 bis0,05dried1corrugated8525 before
525 rear
38.813,420,86---
20,05freshcorrugated6525 before
525 rear
41,907,711,811,7940121239,7
30,05dried1 corrugated6525 before
525 rear
42,153,761,121,674632495,8 1752,1
40,05freshsmooth-525 before
525 rear
40,08to 7.673,49---
50,05dried1smooth-525 before
525 rear
37,302,930,72---
60,01freshcorrugated10500 to
500 rear
42,267,53 2,101,6842114520,7

Table 2b
The influence of drying before and after flattening and conditions flatten (continued)
No.The gap between the rollers (mm)Quality seedsType rollsThe number of grooves/cmThe speed of rotation of the rollsContaining
the obtained
s3oil matter2(%SW)
THR105 (%)Ia (mg KOH/g)THR after drying at 80°C (%)Bulk density (g/l)The flow rate of percolation (l/h/m2)4
70,1freshcorrugated10530 before an45,487,423.04 from1,764204016,5
80,1freshcorrugated10525 before an43,067,822,181,8842412396,7
90,1dried1corrugated10525 525 before rear41,784,051,031,364731239,7
100,1freshcorrugated8500 before 525 rear42,287,791,821,5441919198,3
110,1dried1corrugated 8525 525 before rear39,323,970,91---
120,1freshcorrugated6525 525 before rear38,65to 7.591,71---
130,1dried1corrugated6525 525 before rear39,20of 3.070,74---
140,1freshsmooth-500 prior 500 rear31,547,512,58- --
150,1dried1smooth-500 prior 500 rear39,623,240,91---

Table 2C
The influence of drying before and after flattening and conditions flatten (continued and end)
No.The gap between the rollers (mm)Quality seedsType rollsThe number of grooves/cmThe speed of rotation of the rollsThe content of the received
th3oil matter2(%SW)
THR
105 (%)
Ia (mg KOH/g)THR after drying at 80°C (%)Bulk density (g/l)The flow rate of percolation (l/h/m2)4
16 0,1dried1smooth-525 before an34,333,330,91---
170,2dried1corrugated10 (65/45)700 rpm35,723,690,92---
180,2dried1smooth-Are can41,193,320,901,985353338,8
190,2dried1smooth-700 rpm 37,023,480,88---
1Dry seeds were dried at a temperature of from 80 to 100°C;
2The total content of oil substances in the seeds of rape; TH=4%SV;
3Direct extraction with hexane for 10 hours (8+2 hrs) (method soxlet);
4Characteristics of the used column; L=295 mm, dint=39,3 mm, Sc=1,21 .10-3m2Size during sintering=No. 0, the Size of crane=4 mm; the Height of the layer is approximately 40 mm; the Characteristics of ethyl alcohol; the Fortress=92,2°, dam b=0,807, dpercolation=28330,6 l/h/m2; Test conditions; hlayer=4 cm, T=ambient, trep s=10 min

Conclusions:

dried seeds are poorly withstand crushing and percolation of ethanol is weaker with these seeds due to the presence of small particles,

- drying of seeds decomposition oily substance. Indeed, the acid number of the oil substance dry seeds is much lower than that of fresh seeds,

- corrugated rolls produce more small particles than gladkevich,

- the gap between the rollers should be 0.1 mm

2.2) rape Seeds, prepared according to method 2

Flattening produced in the following conditions:

- Conditioner : conditioner brand DAMMAN-CROES,

- Rolls : smooth, diameter 14 cm, length 24 cm,

The gap between rolls : 0.1 mm

- Speed: : 60 rpm

The total oil content of the seeds is 50%. Loss during grinding is calculated as follows:

Table 3
Characteristics of rapeseed
Designation1234
The gap between rolls0,050,10,20,3
PackingPlastic bagPlastic bagPlastic bagPlastic bag
Storage time after flattening2 months2 months is CA 2 months2 months
TMV, %6,596,34of 6.73to 6.67
The oily substance is extracted with hexane, %SV49,3749,8248,8746,96
Losses from grinding, %SV1,240,36of 2.215,73
Acidity, mg KOH/g3,332,982,802,30

Conclusions:

Not dried flattened seeds are poorly preserved. The acid number of the oil substance is significantly increased after 6 weeks of storage (from 1 to 3.3 mg KOH/g). The thinner flat seeds, the better decomposes the oil substance. The contents of the extracted (hexane) of the oil substance is not changed by changing the gap between the rollers from 0.05 to 0.01 mm, It is reduced from 0.2 mm, and particularly when the interval of 0.3 mm

Therefore, it is necessary to dry the seeds after flattening. The gap between the rollers can the t range from 0.05 mm to 0.1 mm In addition, it was found that the final meal should be characterized by the content of the oily substance is less than 2%, the thickness of the flattened seed should be less than 0.2 mm

2.3) rape Seeds, prepared by the method of 3

2.3.1) Purpose

The oily substance flattened wet seeds can be degraded by enzymatic hydrolysis during storage time. Its acid number is increased. The aim of the work produced in this part, is determining the appropriate conditions for the preservation flattened rapeseed.

Rape seeds were flattened and processed immediately on the spot.

2.3.2) the test report

2.3.2.1) Flattening

Rapeseed (7-8% water content) were squashed in the following conditions, without pre-heating:

- Conditioner : conditioner mark Henry,

- Power : 2 fiscal horsepower,

- Rolls : smooth, diameter 14 cm, length 24 cm,

The gap between rolls : 0.1 mm

- Rotation speed : 60 rpm,

- The number of seeds that are processed during a single trial: 20 kg

- Consumption of seeds : 25 kg/h

2.3.2.2) Drying

After that flattened seeds were dried in the dryer with supercharged or at 80°C or 90°C to obtain a residual water content of from 1%to 2%. Drying was carried out under the following conditions:

Machine : Dryer with supercharged brand CERCO SEMIP type THOSE 75 T1-04,

- M is mnost : 6.35mm kW,

Drying basket : 4 quarters with a perforated bottom,

The number of flakes : 4×5 kg

The layer height : 30 cm

- Air consumption: : circular circulation of hot air.

Dry seeds are Packed in airtight plastic bags and stored at ambient temperature. Seed quality monitor measurements:

- volatile content (%),

content of the obtained oily matter (%DM), the output - extracting in to conventional Soxhlet extractions with hexane for 10 hours,

acid number of the oil extract (mg KOH/g) - NF T 60-204,

- peroxide number,

- percolation.

2.3.3) Results storage

Table 4
The influence of the duration of seed storage on the quality of the oil substance
DateJJ+1J+3J+7J+10J+14J+21J+28J+35
Not the dried seeds
THR 95,%6,5-6,56,5-----
TMG available, % SV49,0-48,948,9-----
Ia, mg KOH/g0,8-3,5of 17.0-----
Seeds, dried at 80°C
THR 95,%1,842,011,671,741,981,732,102,312,05
TMG - the Content of available oil-based substances, % SV48,547,847,745,846,648,447,544,6to 47.2
Ia, mg KOH/g0,890,910,770,760,770,780,900,730,88
Ip peroxide number, milligram-equivalent to About2/kg1,43-------1,70
Seeds, dried at 90°C
THR 95,%of 1.571,691,481,871,811,761,871,881,94
TMG - the Content of available oil-based substances, % SV48,948,249,646,545,848,648,448,148,8
Ia, mg KOH/g0,940,960,700,910,870,820,850,850,92
Ip milligram-equivalent to About2/kg 0,73-------0,80

During storage the reverse absorption of moisture cereal is very slow. Other quality parameters of oil substances after 35 days of storage are almost unchanged.

The acidity of the oil is not dried flattened seed grows very quickly: so, after one week, the acidity can reach a value of 17 mg KOH/g This acidity corresponds to 10% of free fatty acids hydrolyzed oil. Formed in this way free fatty acid will adversely affect the reaction in a basic environment, they will be subjected to saponification (the consumption of the catalyst NaOH). Therefore, the yield of ester is the smaller, the stronger the hydrolysis. But the seeds after drying immediately after delivery, are stable over time, the acidity of the oil.

We can conclude that flattened and dried canola seed can be stored for at least 35 days in an airtight plastic bag.

Taking into account the conducted tests it is preferable to perform the preparation of the seed in the following order:

- Purification from admixtures,

- Pre-heating for the avicenia plasticity (< 60°C), while it may be useful to add water vapor

- Flattening using smooth rolls in a single pass,

- Drying at a temperature of from 70 to 90°C immediately after flattening.

3) reaction Conditions and processing products

3.1) the Effect of temperature alcohol impregnation squared away seeds

The purpose of this series of tests is to identify the importance of the stage of alcohol impregnation pre-flattened and dried seeds and, in particular, its impact on extracting and reactive ability of ethanol in relation to the oil substance. For this purpose, the temperature of the alcohol impregnation changed between values 25; 50 and 75°C (temperature T).

From the point of view of the experiments work includes the following key steps:

(1) flattening of whole rapeseed with preheating to 50°C for 60 minutes;

(2) impregnation of seeds in a temperature controlled closed reactor equipped with a mechanical stirrer and a cooler, in the presence of anhydrous ethyl alcohol at a temperature T for 15 minutes at a mass ratio of ethanol/flakes, equal to 1.9/1. At this stage measure the content of the extracted oil substances after 15 minutes. This content expresses the extracting ability of alcohol in the test conditions and, therefore, their subsequent reagent is ity in the presence of a catalyst in the reaction of transesterification of extracted oil.

Indeed, in this type of process, "in planta", since the environment consists of a liquid phase and a solid phase, the reaction primarily occurs due to the diffusion of alcohol in the seeds. Alcohol has a double function of the solvent the oily substance and the reagent. Therefore, the higher the yield of extracted oil substances, the higher the output the desired esters. Under the reaction conditions in the presence of a catalyst to oil extracted material is rapidly transformed into esters. In fact, the extraction of oil substances alcohol from seeds is a major factor in the way. The test results presented in table 5.

Table 5
The effect of temperature alcohol impregnation squared away seeds
The temperature of the alcohol impregnation, °C255075
The duration of the impregnation, min151515
% oil extracted substances after 15 minutes334159
Conditions: the ratio of flakes/alcohol impregnation: 1/1,9
Flakes: preheating to 50°C, flattening 0.05 mm, drying 2% humidity

From the results of table 5 it is clear that the higher the temperature the alcohol impregnation, the greater the yield of extraction of oil substances and, therefore, its subsequent transformation into the desired esters.

This stage can be applied in a periodic process to improve the extraction of oil substances and to increase the purity of ester.

However, in a continuous process this step is not desirable, as was observed sediment, appearing in the upper part of the layer, when the catalyst was added after 30 minutes of impregnation, and even after 5 min of treatment. This residue leads to very rapid and sharp decrease in percolation. On an industrial scale at low percolation operation is not possible because there is a risk of clogging of the extractor.

Table 5 bis
The influence of pre-impregnation on the percolation and conversion in continuous mode
Test1 23
The duration of the impregnation, min5300
The flow percolation impregnation, m3/h·m21010-
The duration of reaction, min303030
The flow percolation during the reaction, m3/h·m25113
The output of the extraction, %909285
The purity of ester, % ether100100100
Condition: Flattened seeds with a thickness of 0.35 mm, dried at 80°C. the Temperature of 50°C. the Ratio of NaOH/EtOH/seeds: 1,5%/2/1

Pre-treatment has a positive influence on extraction (90-92%), but adding the catalyst significantly reduces the consumption of percolation. So, spending the falls from 10 to 5 and even up to 1 m 3/h·m2depending on the time of the preliminary impregnation.

The longer pre-treatment, the greater the reduction in consumption. This phenomenon can be explained as follows. Neutral alcohol medium sugar are soluble. The longer the extraction, the greater the amount of dissolved sugar. Sugar lose their solubility in a basic environment due to the aldol condensation. In this case, a precipitate, which is concentrated in the upper layer and disrupts the process of percolation.

In periodic mode, this reaction is also possible, but the resulting precipitate diverges on all seeds, so only slightly affects the filter.

3.2. Reaction with EtONa as catalyst

The purpose of this series of tests is to confirm the way of bringing to the condition flattened and dried seeds prior to the reaction. As the catalyst used EtONa. Seeds were trained in the above-described method 2:

- drying at 60°C,

- flattening with two gaps between the rolls,

- storing in anhydrous alcohol.

We have studied the basic operation method.

Table 6
VL is of the gap between rolls
DesignationETET8
Preliminary impregnation24 h with tneighborhood.24 h with Tneighborhood.
Reaction
T, °C5050
Duration, h22
Ethyl alcohol, g14001400
The water content, ppm450450
Catalyst
EtONa 99%, g23,723,7
Ethyl alcohol, g89,389,3
Flattened rapeseed, g10001000
The gap between the rollers, mm0,050,10
Water %2,122,12
The content of the oily substance1, %SV46,146,1
Ia oily substances, mg KOH/g0,90,9

Method of preparing seedsMethod 2Method 2
Seeds, dried in a cooperative dryer- Conditioner: DAMMAN-CROES- Conditioner: DAMMAN-CROES
at 90-100°C before flattening- Type rolls: smooth- Type rolls: smooth
- Interval: 0.05 mmLength: 0.10 mm
- T 2nd drying: 60°C- T 2nd drying: 60°C
- Drying time: 1 hour- Drying time: 1 hour
Ethyl alcohol/Flakes, m/m1,51,5
Processing after dryingFiltering in nitrogen at 0.5 barFiltering in nitrogen at 0.5 bar
3 extraction of pomace absolute ethanol3 extraction of pomace absolute ethanol
(Ethyl alcohol/Solid phase=1/1)(Ethyl alcohol/Solid phase=1/1)
The oily substance of the cake after4,18,1
reactions, %SV, including
Ethyl esters (EE), %55,325,4
Monoglycerides (MG), %0,330,9
Diglycerides (DG), %to 1.861,9
Triglycerides (TG), %42,0770,8
Processing liquid phaseLipari is the W ethyl alcohol of 80°C, the Max. vacuum of 100 millibar (R5)Evaporation of ethyl alcohol of 80°C, Max. vacuum of 100 millibar (R5)
Assertion (15 min at 80°C)Assertion (15 min at 80°C)
4 washing esters (80°C)4 washing esters (80°C)
Drying (90°C, 20 mbar, 30 min)Drying (90°C, 20 mbar, 30 min)
Raw glycerin, g7468,2
End esters, g424392
Ethyl esters (EE), %98,898,0
Monoglycerides (MG), %0,470,78
Diglycerides (DG), %0,20,31
Triglycerides (TG), %00
1Defined standard V03-908

End esters status which make about 40% of the original seed. They are characterized by very high purity.

The gap between the rollers in 0.05 mm allows you to get more esters than when the gap is 0.1 mm, the Output of the interesterification reaction is higher with a gap of 0.05 mm than with an interval of 0.1 mm

3.3. optimization of the reaction conditions with NaOH as catalyst

Used as a catalyst EtONa is more effective than soda (NaOH). On the other hand, the soda is cheaper than EtONa. Therefore, the aim of this series of tests is to determine the optimal reaction conditions with NaOH as catalyst (less consumption of catalyst and ethyl alcohol) for conversion of triglycerides in a complex ethyl esters.

The main considered parameters are:

- mass ratio of Catalyst/seeds and the effect of pre-soaking,

- mass ratio of "Ethyl alcohol/seeds"

the water content in ethanol,

the thickness of the flakes.

The procedure works:

The reaction was carried out in a reactor with a double casing at ambient temperature with slow stirring. The order of operations is as follows:

the whole ethanol is injected into the reactor at ambient temperature under nitrogen atmosphere,

- the entire catalyst is introduced into the reactor under moderate stirring,

- the temperature of the reactor was raised to 50°is,

after 30 minutes, all flattened seeds are poured into the reactor under moderate stirring, maintaining a temperature of 50°C,

- take 1 sample of the reaction medium and filtered to obtain a liquid phase (L0) and solid phase (S0),

- produce extraction with hexane L0 system (liquid-liquid)obtained oily substance was washed, dried and analyzed with HPLC,

- produce extraction with hexane S0 (10 hours to conventional Soxhlet extractions);depleted cake is dried in the mold under a fume hood; the resulting oily substance was washed, dried and analyzed with HPLC.

3.3.1) the Influence of mass relations "Catalyst/seeds and prior treatment response in periodic mode

Table 7a
The influence of "Catalyst/Seeds and pre-treatment conversion of triglycerides in periodic mode
OptionsF1F2F3F4F5F6
Pre - NoNothe et YesYesYes
impregnation
T, °C505050
Time min303030
Reaction
T, °C505050505050
Time, h2-42-42-42-42-4 2-4
Ethyl alcohol, g150015001500135013501350
The water content,the
parts per million465434361361402402
Catalyst
NaOH 99%, g15of 17.5of 17.5of 17.5of 17.5of 17.5
Ethyl alcohol, g000150150150
Cereals, canola, g100010001000100010001000
The pace. drying °C909060608060
Water %1,781,781,870,960,960,96
The content of the oily substance1,48,948,948,948,948,948,9
%SV
Ia oily substances, mg KOH/g0,90,90,90,90,90,9
Method of preparationMethod 3Method 3Method 3Method 3Method 3Method 3
seedsConditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRY
Type rolls: smoothType rolls: smoothType rolls: smoothType rolls: smoothType rolls: smoothType rolls:smooth
Gap: 0.1 mmPeriod:
0.1 mm
Period: 0.05 mmPeriod: 0.05 mmPeriod: 0.05 mmPeriod:
0.1 mm
T drying: 90°CT drying: 90°CT drying: 60°CT drying: 60°CT drying: 80°C T drying: 90°C
Drying time:
4 h
Drying time: 4 hoursDrying time: 8 h 30 minDrying time: 8 h 30 minDrying time: 5 h 15 minDrying time: 4 hours
The concentration of MV1after the reaction L0, % (m/m)
2 hours-16,220,022,623,023,8
4 h16,519,317,722,723,624,5
Triglycerides L0, (%MV)
2 hours0 0000
4 h0,840,61000
Triglycerides S0, (%MV)
2 hours19,112,596,16or 4.313,38
4 h24,7633,74-1,851,403,26
The triglyceride/Theoretical
ester, %
2 hours2,251,781,35
4 h0,800,621,32
1Defined standard V03-908

Table 7b
The influence of "Catalyst/Seeds and pre-treatment conversion of triglycerides in periodic mode (continued)
OptionsF7F8F9
Preliminary impregnationYesYesYes
T, °C505050
Time min30303
Reaction
T, °C506060
Time, h2-42-42-4
Ethyl alcohol, g135013501350
The water content, parts per440400-450400-450
million
Catalyst
NaOH 99%, gof 17.5of 17.5of 17.5
Ethyl alcohol, g150150150
Cereals, canola, g100010001000
Water %0,910,914,46
The oil content
substances1, %SV48,948,948,9
Ia oily substances mg
KOH/g0,90,90,9
Method of preparing seedsMethod 3Method 3Method 3
Conditioner: HENRYConditioner: HENRYConditioner: STOLZ
Type rolls: smoothType rolls: smoothType rolls: smooth
Period: 0.05 mmPeriod: 0.05 mmGap: 0.1 mm
T drying: 80°CT drying: 80°CT drying: 80°C
Drying time: 5 h 15 minDrying time: 5 h 15 minDrying time: 5 h 15 min
The concentration of MB1after
the reaction L0, % (m/m)
2 hours23,020,719,0
4 h23,923,319,0
Triglycerides L0, (%MV)
2 hours000
4 h000
Triglycerides S0, (%MV)
2 hours 4,636,112,66
4 h3,543,959,54
The triglyceride/Theoretical
ester, %
2 hours2,252,954,6
4 h1,481,653,51
1Defined standard V03-908

In periodic mode, preferably the use of pre-impregnation for good extraction and conversion of oil substances. Time 30 min impregnation can be reduced to improve the performance of the installations. In periodic mode, the ratio of the Catalyst/alcohol/seeds" can be fixed at the level of 17.5 g/1500 g/1000 g. It is noted that the quality of the flattened seeds has a great influence on the extraction of oil substances. Test conditions F4, F5, F6 are the best.

<> 3.3.2) the Influence of mass relations Ethanol/Seeds" in periodic mode

Table 8A
The influence of mass relations Ethanol/Seeds"
OptionsF10F11F12F13
Preliminary impregnationYesYesYesYes
Reaction
T, °C50505050
Time, h2-42-42-42-4
Ethyl alcohol, g1350135013501350
The water content, ppm 441418443451
Catalyst
NaOH 99%, gof 17.5of 17.5of 17.5of 17.5
Ethyl alcohol, g150150150150
Cereals, canola, g1000100010001000
Water %1,771,641,951,23
The content of the oily substance1, %SV48,948,948,948,9
Ia oily substances, mg KOH/g0,90,90,90,9
Method of preparing seeds Method 3Method 3Method 3Method 3
Conditioner:Conditioner:Conditioner:Conditioner:
HENRYHENRYSTOLZHENRY
The type of rollers:The type of rollers:The type of rollers:The type of rollers:
smooth Interval:smooth Interval:smooth Interval:smooth Interval 1
0.1 mm0.15 mm0.05 mmflatten:
T drying: 80°CT drying: 80°CT drying: 80°C0,5 mm
Drying time:Drying time: Drying time:The period of the 2nd flatten:
5 h 15 min5 h 15 min5 h 15 min0.05 mm T drying: 80°C drying Time: 5 h 15 min
Ethyl alcohol/flakes canola1,51,51,51,5
The concentration of MB1after the reaction L0, % (m/m)
2 hours1715,218,4a 21.5
4 h1918,120,425,5
Triglycerides L0, (%MV)
2 hours0000
4 h0,04 0,060,080
Triglycerides S0, (%MV)
2 hours36,1765,1to 33.81,1
4 h25,265,0of 21.90,8
The triglyceride/Theoretical ester, %
2 hours13,530,0514,70,42
4 h6,528,48,180,28
1Defined standard V03-90

Table 8b
The influence of "Catalyst/Seeds" in periodic mode (cont who begins)
OptionsF14F15F16F17F18F19
Preliminary impregnationYesYesYesYesYesYes
Reaction
T, °C505050505050
Time, h2-42-42-42-42-42-4
Ethyl alcohol, g111511151115111511151115
Soda is the water content, parts per million43833973343351736183516
Catalyst
NaOH 99%, gof 17.5of 17.515,215,215,215,2
Ethyl alcohol, g150150150150150150
Cereals, canola, g100010001000100010001000
Water %1,051,171,261,201,171,22
Content
oil substances1, %SV48,948,948,948,948,9
Ia oily substances, mg KOH/g0,90,90,90,90,9
Method of preparing seedsMethod 3b (Two flatten)Method 3b (Two flatten)Method 3b (Two flatten)Method 3b (Two flatten)Method 3b (Two flatten)Method 3b (Two flatten)
Conditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRYConditioner: HENRY
Type rolls: smooth the Type rolls: smoothType rolls: smoothType rolls: smoothType rolls: smoothThe type of rollers:
smooth
Period 1st flatten: 0,5 mmPeriod 1st flatten: 0,5 mmPeriod 1st flatten: 0,5 mmPeriod 1st flatten: 0,5 mmPeriod 1st flatten: 0.4 mmPeriod 1st flatten: 0,5 mm
The period of the 2nd flatten: 0.05 mmThe period of the 2nd flatten: 0.05 mmThe period of the 2nd flatten: 0.05 mmThe period of the 2nd flatten: 0,07-0,09 mmThe period of the 2nd flatten: 0.04 mmThe period of the 2nd flatten: 0.04 mm
T drying: 80°CT drying: 80°CT drying: 80°CT drying: 80°CT drying: 80°CT drying: 80°C
Drying time: 5 h 15 minDrying time: 5 h 15 min Drying time: 5 h 15 minDrying time: 5 C minDrying time: 5 C minDrying time: 5 h 15 min
Ethyl alcohol/flakes canola1,31,3131,31,3
The concentration of MB1after
the reaction L0, % (m/m)
2 hours26,727,427,820,026,526,5
4 h27,327,227,328,527,4
Triglidae the potassium L0, (%MV)
2 hours000,10,040,20,1
4 h000-0,20
Triglycerides S0, (%MV)
2 hours2,01,02,0446,84,924.09 to
4 h0,91,11,22-3,553,31
The triglyceride/Theoretical ester, %
2 hours0,830,370,8521,62,322,00
4 h0,370,460,51-1,391,61
1Defined standard V03-908

The ratio of Ethanol/Seeds" may be about 1.3/1 in the periodic mode, the reaction with stirring. For continuous mode and the fixed layer, this ratio must be corrected.

3.3.3) the Effect of water content in ethanol

Yes
Table 9
The influence of water content in ethanol
OptionsF14F15
Date27/02/0628/02/06
Preliminary impregnationYes
Reaction
Temperature, °C5050
Time, h2-42-4
Ethyl alcohol, g11151115
The water content, ppm4383397
Catalyst
NaOH 99%, gof 17.5of 17.5
Ethyl alcohol, g150150
Cereals, canola, g10001000
Water %1,051,17
The content of the oily substance, % SV48,948,9
Acidity, mg KOH/g0,90,9
Method3B3B
The gap of 0.05 mmThe gap of 0.05 mm
Drying 80°CDrying 80°C
The ratio of Ethyl1,31,3
alcohol/seeds
The concentration of MB in L0, %27,327,2
Triglyceride L000
Triglyceride S00,881,1

For the reaction of the water content in ethanol may be about 3000 parts per million.

3.4) determine the conditions of processing of the products after reaction

3.4.1) Liquid-phase extraction after reaction

The procedure works:

Two tests were carried out under identical reaction conditions:

- Impregnation flattened and dried seeds ethyl alcohol at 50°C for 30 minutes (Ethyl alcohol/Seeds=115/100 - mass),

- Transesterification at 50°C for 1 h under masoomeen "NaOH/Ethanol/flattened and dried seeds=1,5/130/100" (periodic mode - 1 kg flattened and dried seeds),

Filtering the reaction mixture on filter paper with a pore diameter of 11 microns, in an atmosphere of N2under the pressure of 0.5 bar.

Received from the first filter cake was subjected to 4 straight to extraction with ethyl alcohol at different water content.

Table 10
The influence of water content in ethanol for extraction cake
OptionsFET2FET4
Preliminary impregnation T, °C5050
Time min3030
Reaction T, °C5050
Time min11
Ethyl alcohol reaction, g11501150
The water content, h-a-million34643550
The catalyst NaOH 99%, g 15,215,2
Ethyl alcohol, g150150
Cereals, canola, g10001000
The flake size, mm0,040,05
Water %2,111,75
The content of the oily substance1, %SV4848
Ia oily substances, mg KOH/g0,90,9
Method of preparing seedsMethod 3b (Two flatten)Method 2
Conditioner: HENRYConditioner: DAMMAN-CROES
Type rolls: smoothType rolls: smooth
Period 1st flatten: 0.4 mmGap: 0.05mm T drying: 90°C
The period of the 2nd flatten: 0.04 mmDrying time: (16-29 hours)
T drying: 80°C
Drying time: 5 h 15 min
The ratio of Ethanol/seeds"1,31,3
The number of extraction cake44
Mixing time, min3030
T, °C5050
Purity extractive9797
ethanol %
The final cake
TMV, %
60,058,5
Oil substances after the reaction1, %SV5,9the 4.7
Including:
Complex ethyl esters, %0,6494,1
Triglycerides, %98,7 a 4.9
1Defined standard V03-90

The lower the water content in ethanol, the better the extraction of the meal.

Absolute ethyl alcohol is the best solvent for the extraction with flattened seeds.

3.4.2) condition Determination processing liquid phase

The procedure works:

The preparation liquid after interesterification was produced under the following conditions:

Seeds were prepared according to method 3A (two flatten: 1st flattening at 0.4 mm, and the 2nd flattening at 0.04 mm),

- Drying seeds at 80°C for 5 h 15 min at TMV, equal to 1.3%,

- Impregnation flattened and dried seeds ethyl alcohol at 50°C for 30 min (Ethanol/Seeds=115/100 by weight),

- Transesterification at 50°C for 2 h with a mass ratio of NaOH/Ethanol/Flattened and dried seeds=1,5/130/100" (periodic mode 4 kg flattened and dried seeds),

Filtering the reaction mixture on filter paper with a pore diameter of 11 microns in an atmosphere of N2under the pressure of 0.5 bar for receiving the base fluid, called L0.

The liquid phase (L0) was neutralized with sulfuric acid solution with different concentration of ethanol 97%.

Table 11 shows that complex ethyl esters obtained without neutralization, have ensee acid number. At the same time have the least amount of esters. Partial neutralization allows you to get more esters. The liquid phase can be neutralized with 10%sulfuric acid solution.

Table 11a
Conditions for obtaining fluid L0
OptionsFET1
Preliminary impregnation
T, °C50
Time min30
Reaction
T, °C50
Time min2
Ethyl alcohol reaction, g4600
The water content, ppm3345
Catalyst
NaOH 99%, g60,8
Ethyl alcohol, g600
Cereals, canola,g 4000
The flake size, mm0,04
Water %1,35
The content of the oily substance1, %SV48,9
Ia oily substances, mg KOH/g0,9
The ratio of Ethanol/seeds"1,3
1Defined standard V03-90

Table 11b
The effect of the concentration of sulfuric acid to neutralize the liquid L0
OptionsN2N1N2N3N4
Neutralization (50°C, 20 min)RotavapRotavap(1)Rotavap(1)Rotavap(1)Rotavap(1)
L0, g501,5250,0250,0 250,0250,0
pH9,90 (20°C)The sameThe sameThe sameThe same
Oil substances1, %27,627,627,627,627,6
Equivalent basicity, mmol1,231,231,231,231,23
theoretical concentration of H2SO4, %2,502,5510
The actual concentration of H2SO4, %2,502,384,80of 9.55
Equivalent acidity, mmol-
The quantity of acid solution g2,54-1,270,630,32
The initial pH9,43-to 9.93(to 9.32)
The final pHat 9.53-9,639,909,82
EvaporationRotavapRotavapRotavapRotavapRotavap
T, °C8080808080
Pressure, bar20 (1H 30)23 (20 min)28 (30 min)21 (30 min)21 (30 min)
The collected ethyl alcohol, gto 333.3167,7168, 167,9166,1
DefendingThe flaskCentrifugeThe flaskThe flaskThe flask
T, °CEnvironmentEnvironmentEnvironmentEnvironmentEnvironment
Time min55(Ob/min)555
Glycerin, g28,513,311,916,215,9
THR (95°C) glycerin, %4,0420,118,44by 8.22of 3.64
Raw esters, g132,366,166,766,267,6
THR (95°C) raw ethers, %1,561,680,441,502,34
FlushingVialCentrifugeFlask(3)Flask(3)Flask(3)
Weight esters for washing, gof 124.858,060,760,261,6
T, °C90EnvironmentEnvironmentEnvironmentEnvironment
MixingManualManualManualManualManual
Sedimentation, min155(4500 rpm)SlowFastFast
Num is leaching 46664
Demineralized water/rinsing, gpriblapprox. the 11.6approx. 12,2approx. to 12.0approx. 12,3
DryingRotavapRotavapRotavapRotavapRotavap
T, °C8080808080
Pressure, mbar2620272620
Time min302030-403030-40
End esters, gthe level of 121.855,659,3(6)9,5(6) 60,7(6)
Acid number, mg KOH/g0,480,270,480,45(7)0,46
1Defined standard V03-90

4) Analysis of esters on the basis of the European standards

Obtaining a complex of ethyl esters of rapeseed oil was carried out using 20 kg of whole seeds. Conditions of application of the method in periodic mode (closed reactor) are the following:

- preheating temperature before flattening: 50°C

- flattening on the roll conditioner: the gap between the rollers 0.2 mm

- temperature/drying time flattened seeds: 70°C /12 hours

residual humidity flattened seeds after drying: 1,9%

- mass ratio of alcohol/seeds/the catalyst (NaOH): 160/100/1,7%

the temperature and time of reaction phase: 50°C/30 minutes

- washing of the cake with fresh ethyl alcohol: 3 times, 100 g of ethyl alcohol

- Clearing complex ethyl esters:

- distillation of ethyl alcohol under vacuum (20 mbar) at 90°C for 30 minutes

- sedimentation and separation of glycerin

- washing esters distilled water 4 times to 1500 g of distilled water

- drying is one of the ethyl esters under vacuum (20 mbar) at 110°C for 30 minutes.

The mass of collected complex of ethyl esters is 7600 g, i.e. the emergence of complex ethyl esters is 82%.

Has made the analysis of the thus obtained complex ethyl esters, based on the main criteria of the European standards NF EN 14214 applied to complex methyl esters, intended for use in the fuel. The results show that the obtained complex ethyl esters have a high degree of purity (>97%), do not contain impurities and other by-products in amounts exceeding the norm (total glycerin, water, ethyl alcohol, phosphorus, free fatty acids, mono-, di - and triglycerides). In addition, their cetane number far exceeds the specifications of the norm (>51), and all these results confirm that these complex ethyl esters can be used as fuel.

Table 12
Analysis of the composition of esters obtained from rapeseed according to the claimed method
Characteristics of estersUnitMinimumMaxMethodThe obtained esters
The content of estersppm96,5EN 1410397,7
The content of monoglyceridesppm0,80EN 141050,56
The content of diglyceridesppm0,20EN 141050,09
Triglyceridesppm0,20EN 141050,11
Free glycerolppm0,02EN 14105 EN 14106<0,01
Total glycerinppm0,25EN 141050,17
Density at 15°Ckg/m3 860900EN ISO 3675870
EN ISO 12185
Viscosity at 40°Cmm2/s3,505,00EN ISO 31044,73
Index of cetane51,0EN ISO 1037055
Water contentmg/kg-500EN ISO 12937108
Acid numbermg KOH/g0,50EN 141040,21
Indicator of iodineg iodine/100 g120EN 14111110,1
The content of the words is different methyl esters of linolenic acid ppm absoluteto 12.0EN 1410310,2
The ethanol contentppm0,2<0,01
The phosphorus contentmg/kg10,0EN 14107<10

1. The method of obtaining esters of fatty acids, used as biodiesel, from the whole seeds of oilseed plants, comprising the following successive stages:
a) pre-heating popularnych and cleaned the whole seeds;
b) crushing of oilseeds together with their casing;
c) drying the flattened seeds until the water content and volatile matter from 0.5 to 2.5%;
d) transesterification flattened by contact of the seeds with an alcoholic medium in the presence of a catalyst;
e) separating the liquid and solid phases obtained by interesterification;
f) neutralizing the liquid phase obtained in step e); and
g) removing the alcohol and the separation of the glycerol from the fatty acid esters, which are then on imaut.

2. The method according to claim 1, characterized in that the thickness of the flattened seeds is in the range from 10 μm to 1 mm, preferably from 0.1 mm to 0.3 mm, more preferably the thickness of the flattened seeds less than 0.2 mm, and the size of the flattened seeds is in the range from 3 to 5 mm.

3. The method according to claim 1, characterized in that step C) drying carried out immediately after step b) flatten, not later than 24 hours after step (b) flatten, preferably less than 2 h after step b) flattening at a temperature which is from 50 to 100°C., preferably from 70°C to 90°C.

4. The method according to claim 1, wherein the oil seeds are subjected to preliminary heating at a temperature of from 50 to 55°C for 5-60 min before carrying out step b) flatten, if necessary, in the atmosphere of water vapor.

5. The method according to claim 1, characterized in that the crushing of oilseeds produced with the assistance of the rolls, the gap between which is less than 0.2 mm and preferably less than 0.1 mm

6. The method according to claim 1, characterized in that the crushing of oilseeds produced using smooth rolls, preferably in a single pass.

7. The method according to claim 1, characterized in that the alcohol environment on stage d) interesterification contains one or more alcohols selected from alcohols of C1-C6, such as methyl alcohol or ethyl alcohol, if not the bhotekoshi, in a mixture with one or more aliphatic hydrocarbons.

8. The method according to claim 7, characterized in that the alcohol environment is ethyl alcohol containing water in an amount less than 5000 million-1.

9. The method according to claim 1, wherein the catalyst in step (d) interesterification is basically a catalyst selected from the group comprising sodium, potassium, carbonate or bicarbonate of sodium or potassium or sodium carbonate or potassium methylate or ethylate of sodium or potassium.

10. The method according to claim 1, characterized in that the periodic mode, flattened seeds enter into contact with the alcohol environment prior to the implementation of the interesterification catalyst, preferably during the period from 10 to 30 minutes at a temperature of from 40 to 80°C.

11. The method according to claim 1, characterized in that the mass ratio of catalyst/flattened seeds in stage d) interesterification is from 0.5/100 to 2/100, and the mass ratio of alcohol/flattened seeds in stage d) interesterification is from 100/100 to 500/100.

12. The method according to claim 1, characterized in that the periodic mode, the interesterification reaction is carried out at a temperature of from 45 to 55°C. and preferably at a temperature of approximately 50°C, during the time from 10 min to 2 h, preferably from 20 to 40 minutes

13. The method according to claim 1, characterized in that the contact flattened seeds with spirit cf the DOI during stage d) interesterification is carried out with slow stirring or by wetting and percolation.

14. The method according to claim 1, characterized in that it further comprises the following steps:
h) extracting the alcohol of the specified solid phase obtained in step e);
i) collecting the solid phase obtained in this way;
j) filtering and combining the solid phases obtained in the steps (e) and (h).

15. The method according to claim 1, wherein step h) the extraction is carried out by percolation, preferably countercurrent percolation, preferably in a mass ratio of alcohol/flattened seeds that are in the range from 100/100 to 200/100, where the alcohol is preferably selected from alcohols of C1-C6, more preferably the alcohol is ethanol containing water in an amount of less than 5000 parts per million.

16. The method according to claim 1, characterized in that step f) neutralization is carried out with the aid of acid which is selected from the group comprising sulfuric acid, hydrochloric acid, phosphoric acid, citric acid or acetic acid.

17. The method according to item 16, wherein the acid in step f) neutralization is added in an amount which results in a pH of about 10.

18. The method according to item 16 or 17, characterized in that the acid in step f) neutralizing add in the liquid phase obtained in stage e) or i), in the amount of less than 0.04% of the total number of esters of fatty acids present in the specified liquid phases is.

19. The method according to claim 1, wherein step (g) removal of the alcohol is carried out by evaporation at a temperature of from 50 to 100°C. under a pressure of from 200 to 1000 mbar, preferably at a temperature of about 80°C at atmospheric pressure to obtain a residual volume of less than 1%.

20. The method according to claim 1, characterized in that the separation of glycerin from the ester of fatty acids in step (g) is produced by centrifugation at a temperature of from 60 to 80°C.

21. The method according to claim 1, characterized in that after step (g) esters of fatty acids washed with water, preferably at about 80°C, then separated from the wash water, in particular, by sedimentation or centrifugation, preferably at a temperature of 80°C, then dried, preferably by evaporation at a temperature of from 90 to 100°C. under pressure of about 200 mbar to obtain a residual water in quantities of less than 500 ppm relative to the total amount of dry matter.

22. The method according to claim 1, wherein the seeds are selected from rapeseed, peanuts, Orchis, castor, sesame, olive, sunflower, Sapporo, soybean, lupine, flax linen, cotton, rice) bran and preferably chosen from rapeseed, sunflower and Orchid.

23. A method of obtaining a meal intended for use as animal the x feed from the solid phase resulting from step e) or step i) of the method according to any of the preceding paragraphs, comprising the following steps:
1) removing alcohol from the specified solid phase; and
2) adding glycerol obtained in stage g) of the method according to any of the preceding paragraphs.

24. The method according to item 23, wherein the solid phase obtained in step 1)add wash water used for washing in the method according to item 21.

25. The method according to item 23 or 24, characterized in that the removal of alcohol from the specified solid phase is produced mechanically, in particular by pressing or push-UPS, then heat through entrainment with water vapor to obtain a residual amount of water less than 500 ppm relative to the total dry substance.



 

Same patents:

FIELD: food industry.

SUBSTANCE: invention relates to production of a cocoa butter fat substitute for chocolate. The method envisages vegetable fat fractionation, fat material semi-product manufacture by way of mixing the fractionated vegetable fat with stearic acid derivatives and fermentative interesterification of the fat material semi-product. The produced cocoa butter fat substitute contains POP triglyceride in an amount of 10 wt % or less of the total weight of the cocoa butter fat substitute and has POS/SOS triglycerides content ratio equal to 1.0 to 1.5. Additionally, the present invention relates to a chocolate composition involving usage of the said cocoa butter fat substitute.

EFFECT: invention allows to produce a natural cocoa butter fat substitute for chocolate or coatings for pastry with good resistance to heating and a texture and fast melting capability analogous to those of natural cocoa butter.

6 cl, 1 dwg, 14 tbl, 11 ex

FIELD: medicine.

SUBSTANCE: composition contains at least one triglyceride, acyl group consisting of residues of saturated, monounsaturated and polyunsaturated fatty acids with the total contents of palmitoleic acid residues in the composition making approximately 15-55% of the total content of fatty acid residues. At least 13% of the total content of fatty acids in a position of sn-2 carbon skeleton of triglyceride represent palmitoleic acid residues in the composition. What is presented is a method of treating and preventing a condition in a subject suffering or having a severe risk to suffer short bowel syndrome, intestinal inflammatory disease or necrotising enterocolitis, and activation of intestinal development, maturation, adaptation and differentiation involving the introduction of said lipid composition into a subject.

EFFECT: invention enables preventing or avoiding said intestinal disorders in a subject.

37 cl

FIELD: medicine.

SUBSTANCE: what is presented is a method for reduction of re-esterification activity of lipase prepared of Thermomyces sp. and immobilised on a carrier, or a lypase powder mixture which contains a filter excipient and lypase prepared of Thermomyces sp. immobilised on the carrier. The lipase powder mixture is ground to average particle size 1 mcm to 300 mcm. The method is implemented by washing said lypase or lypase powder mixture in triacylglycerol. What is also presented is a method for re-esterification. It involves conducting a re-esterification reaction with the use of said lypase or lypase powder mixture. Then lypase or lypase powder mixture is separated from the reaction system and washed in triacylglycerol for reduction of re-esterification activity. One more re-esterification reaction is conducted with the use of reduced lypase or lypase powder mixture.

EFFECT: method provides effective reduction of low re-esterification activity of lypase or lypase powder mixture to be re-used in the re-esterification reaction.

10 cl, 3 dwg, 1 tbl, 3 ex

FIELD: medicine.

SUBSTANCE: what is presented is a method for reduction of re-esterification activity of lipase prepared of Thermomyces sp. and immobilised on a carrier, or a lypase powder mixture which contains a filter excipient and lypase prepared of Thermomyces sp. immobilised on the carrier. The lipase powder mixture is ground to average particle size 1 mcm to 300 mcm. The method is implemented by washing said lypase or lypase powder mixture in triacylglycerol. What is also presented is a method for re-esterification. It involves conducting a re-esterification reaction with the use of said lypase or lypase powder mixture. Then lypase or lypase powder mixture is separated from the reaction system and washed in triacylglycerol for reduction of re-esterification activity. One more re-esterification reaction is conducted with the use of reduced lypase or lypase powder mixture.

EFFECT: method provides effective reduction of low re-esterification activity of lypase or lypase powder mixture to be re-used in the re-esterification reaction.

10 cl, 3 dwg, 1 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: hydrogenation is carried out on a fixed-bed catalyst which is in form of crystallites of catalytically active palladium, deposited on the surface of carbon material, the carbon material being mesoporous graphite-like material with granule size 0.5-6.0 mm, preferably 3.0-6.0 mm, with specific surface area 100-450 m2/g, mean mesopore size from 40 to 400Ǻ, total pore volume 0.2-0.6 cm3/g and fraction of mesopores in total pore volume not less than 0.6, in which palladium crystallites inside the granules of the carbon material are distributed such that distribution maxima of the active component lie at a distance from the outer surface of the granules which is 1-30% of the radius of the granules, with content of deposited palladium from 0.5 to 2.0 wt %.

EFFECT: high rate of hydrogenating material when producing industrial grades of hydrogenated fats and high stability.

2 cl, 1 dwg, 3 tbl, 16 ex

FIELD: chemistry.

SUBSTANCE: gum is treated with one or more enzymes having PLA activity at temperature of about 40-60°C and pH of about 3-7 for not more than 4 hours, which leads to formation of lysophospholipids and free fatty acids. Gum is treated with one or more enzymes having PLC activity at temperature of about 40-80°C and pH of about 8 or lower for not more than 30 minutes to form diacylglycerols and phosphates.

EFFECT: diacylglycerols and free fatty acids formed from independent reactions are combined in the presence of not less than one of said enzymes to form novel triacylglycerol molecules.

22 cl, 8 dwg, 9 tbl, 16 ex

FIELD: chemistry.

SUBSTANCE: gum is treated with one or more enzymes having PLA activity at temperature of about 40-60°C and pH of about 3-7 for not more than 4 hours, which leads to formation of lysophospholipids and free fatty acids. Gum is treated with one or more enzymes having PLC activity at temperature of about 40-80°C and pH of about 8 or lower for not more than 30 minutes to form diacylglycerols and phosphates.

EFFECT: diacylglycerols and free fatty acids formed from independent reactions are combined in the presence of not less than one of said enzymes to form novel triacylglycerol molecules.

22 cl, 8 dwg, 9 tbl, 16 ex

FIELD: process engineering.

SUBSTANCE: invention relates to hydration of vegetable oils. Proposed method differs from known processes in that hydration id carries out on catalyst made up of crystallites of catalytically active palladium applied on carbon carrier surface with granule size of 1.0-5.0 nm, specific surface of 100-450 m2/g, mean pore size of at least 4 nm and ratio of basal-to-lateral faces of carbon lattice packs varying from 0.7 to 1.4.

EFFECT: reduced content of trans-isomers.

2 cl, 3 tbl, 10 ex

FIELD: chemistry.

SUBSTANCE: invention relates to an improved method for reesterification of at least one compound containing at least one ester functional group with at least one compound containing at least one hydroxyl group, in which red mud, formed during production of aluminium through a Bayer process, is used as a reaction-accelerating compound.

EFFECT: method allows for maximum utilisation of wastes - red mud, both in storage and annually formed.

27 cl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to methods of producing organic carbonates and carbamates. Described is an alcoholysis method, involving: feeding reactants and a trace amount of a soluble organometallic compound, which is soluble in the reactants, into a reactor containing a solid alcoholysis catalyst, wherein the trace amount ranges from about 1 ppm to about 3000 ppm with respect to total mass of the added reactants; where the soluble organometallic compound and the solid alcoholysis catalyst each independently contains a Group II to Group VI element. Described is a method of producing dialkylcarbonates, involving: feeding an alcohol and an alcoholysis reactant, containing at least one compound from urea, organic carbamate and cyclic carbonate, in the presence of the catalyst system described above. Described is a method of producing diarylcarbonate, involving: feeding an aromatic hydroxy compound and dialkylcarbonate in the presence of the catalyst system described above. Described is a method of producing alkylarylcarbonate, involving: feeding an aromatic hydroxy compound and dialkylcarbonate in the presence of the catalyst system described above. Described is a method of producing biodiesel, involving: feeding an alcohol and glycerine in the presence of the catalyst system described above The methods described above involve reaction of a spent solid alcoholysis catalyst, involving: removal of polymer materials deposited on the catalyst; and redeposition of catalytically active metals on the solid catalyst.

EFFECT: longer duration of the cycle of the alcoholysis method.

36 cl, 7 tbl, 18 dwg, 14 ex

FIELD: chemistry.

SUBSTANCE: invention relates to oil refining, particularly to methods of producing ecologically clean diesel fuel. The method involves mixing starting low-sulphur diesel fuel with an ester additive in form of products of esterification of oxalic acid with C4-C8 aliphatic alcohols.

EFFECT: method enables to obtain chemically stable diesel fuel with high lubricating capacity.

2 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: present invention relates to a method of obtaining compositions which contain organic compounds and are suitable as chemical industrial material or a fuel composition using alcohol, for example ethanol, as a raw material. The method comprises a first step for bringing at least one alcohol selected from methanol, ethanol, propanol, butanol, pentanol, hexanol, heptanol and octanol into contact with at least one alcohol conversion catalyst selected from phosphate or clay mineral. The alcohol conversion catalyst simultaneously causes dehydration and dehydrogenation of the alcohol. The method comprises a second step where the product obtained at the first step undergoes hydrogenation to obtain a composition. The obtained composition contains at least one component selected from a group consisting of paraffins and alcohols. The invention also relates to compositions which are obtained using said method and are used as internal combustion engine fuel compositions.

EFFECT: high efficiency of the method.

53 cl, 1 dwg, 17 tbl, 5 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the fish industry and methods of producing biofuel from hydrobiont wastes. The method of obtaining biofuel from fat-containing hydrobiont wastes involves obtaining fish oil with acid number of 2.1-4.6 mg KOH/g. The fish oil is neutralised by adding alkali until attaining acid number of 0.7 mg KOH/g. The neutralised fat, which contains soap and alkali residues, is washed once with 10% salt solution and twice with water at temperature 90-95°C for 90 minutes. The fish oil undergoes reesterification while adding 25% ethanol and 0.75% dry NaOH based on the weight of the fat used.

EFFECT: improved method and high output of biofuel.

1 cl, 1 ex

FIELD: power engineering.

SUBSTANCE: invention relates to a combined packet of lubricant oil and a fuel composition for operation in a diesel engine, where lubricant oil includes basic oil, containing (i) a continuous row of iso-paraffins having n, n+1, n+2, n+3 and n+4 atoms of carbon and/or (ii) continuous row of iso-paraffins having n, n+2 and n+4 atoms of carbon and not having n+1 and n+3 atoms of carbon, and where the value n is between 15 and 40, and where the fuel composition contains a component of paraffin gas oil, having content of paraffins higher than 80 wt % and content of saturated hydrocarbons is higher than 98 wt %. The invention also relates to a device of an engine for generation of kinematic and thermal energy, to a transport vehicle containing the engine device, to the method of power generation with lower emission of exhaust gases, containing nitrogen oxides, and to application of a combined packet of lubricant oil and fuel to reduce content of nitrogen oxides in exhaust gases.

EFFECT: application of a combined packet of lubricant oil and fuel composition resulting in considerable reduction of nitrogen oxide content in exhaust gases.

12 cl, 1 ex, 4 tbl, 1 dwg

FIELD: power industry.

SUBSTANCE: bioethanol obtaining method involves preliminary raw material treatment. Green raw material is collected and crushed, and fluid is obtained. Yeast or special alcohol bacteria are added to the obtained fluid. Fermentation process is performed during 3-5 days. Distillation is performed so that crude alcohol is obtained, and after that, rectification of crude alcohol is performed so that final product - bioethanol is obtained. In addition, as raw material for obtaining bioethanol there used is wild or domestic hogweed containing 17-31% of saccharose of budding phase to flowering phase.

EFFECT: reduction of use of cultures of food purpose as initial components for obtaining bioethanol; restricting the spread and harmfulness of hogweed as aggressive invasive type of plants.

1 cl, 1 dwg, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to ethanol based diesel fuel. The fuel contains 60-80% (vol/vol) absolute ethanol, 2.5-20% (vol/vol) linear dialkyl ether with chain length from 10 to 40, as well as mixtures thereof and 15-30% (vol/vol) combustion booster. The combustion booster is FAME according to DIN EN 14214 (2004) and is rapeseed oil methyl ether, soya oil methyl ether or palm oil methyl ether.

EFFECT: obtained fuel burns without aerosol emissions and is suitable for use in ordinary diesel engines.

6 cl, 3 dwg, 2 tbl, 4 ex

FIELD: organic chemistry.
SUBSTANCE: invention refers to using a flocculating and sequestering agent with the organic solution as an agent to facilitate such purification. A method of purifying an organic solution, comprising contacting a flocculating and sequestering agent with the organic solution, which organic solution comprises fatty acid alkyl esters, wherein the water content of the organic solution is equal or less than 5% by weight, when the pH in the organic solution is 9 to 12, wherein the flocculating and sequestering agent is chosen from polyaluminium coagulants. There is provided a process for purification of an organic solution of fatty acid alkyl esters suitable for use as biodiesel, comprising: adding a flocculating and sequestering agent chosen from polyaluminium coagulants to the organic solution so as to facilitate the purification when the pH in the organic solution is 9 to 12 and removing a portion from the organic solution, which portion comprises the flocculating and sequestering agent, and impurities, wherein the water content of the organic solution is equal or less than 5% by weight.

EFFECT: process will enable less energy input and becomes less time-consuming and less costly, as compared to the known processes using water to purify the organic solution.

10 cl, 3 tbl, 12 ex

FIELD: chemistry.

SUBSTANCE: composition contains biodiesel fuel and an antioxidant effective amount of a mixture of at least one aromatic diamine and at least one sterically hindered phenol. The aromatic diamines are selected from a group consisting of N-(1,4-dimethylbutyl)-N'-phenyl-p-phenylene diamine, N-(1,3-dimethylbutyl)-N'-phenyl-p-phenylene diamine and N,N'-di-fluoro-butyl-p- phenylene diamine. The sterically hindered phenols are selected from a group consisting of 2,4-di-methyl-6-tert-butylphenol, 2-methyl-6-tert-butylphenol, 2,6-di-tert-butyl-4-methylphenol and 1,2,3-trihydroxybenzene. The weight ratio of the aromatic diamine to the sterically hindered phenol is approximately equal to 1:1.

EFFECT: mixture of aromatic diamines and sterically hindered phenols has synergetic antioxidant activity in biodiesel fuel and actively stabilises biodiesel fuel against oxidative degradation and formation of deposits.

17 cl, 3 dwg, 3 ex

FIELD: gas and oil production.

SUBSTANCE: invention refers to procedure for production of high-octane mixtures containing alkyl-tert-alkyl ethers with implementation of at least interaction of tert-pentene in fraction containing mainly hydrocarbons C5 and, possibly, hydrocarbons C6 with alcohol(s) C1-C4 at presence of acidic solid catalyst(s) at 20-100°C rectification. The procedure consists of processing in two stages. At the first stage there is performed synthesis of mainly alkyl-tert-amyl ether with contacting fraction of hydrocarbons C5 and partially C6 with alcohol(s) C1-C4 distillation of distillate. At the second stage alcohol is recuperated from the said distillate, for which purpose distillate is subjected to additional contacting with at least the said catalyst(s) and also with hydrocarbon mixture including isobutene and/or tert-pentene at amount sufficient for transformation of major portion of alcohol into alkyl-tert-alkyl ether(s). In case of their utilisation C4-hydrocarbons are removed from reaction mixture together with admixture of alcohol when limit of its concentration, allowed for benzene ingredients, is exceeded.

EFFECT: reduced power inputs due to improved recuperation of alcohol.

8 cl, 9 ex, 2 tbl, 3 dwg

FIELD: power industry.

SUBSTANCE: hydrocarbon fuel obtaining method involves contacting of glycerides of fatty acids with C1-C5 alcohol in presence of solid double cyanide of metals as catalyst at temperature of within 150-200°C during 2-6 hours, cooling of the above reaction mixture to temperature within 20-35°C, filtration of reaction mixture for separation of catalyst with further removal of unreacted alcohol from the obtained filtrate by vacuum distillation so that hydrocarbon fuel is obtained; at that, one metal of catalyst is Zn2+, and the second one is Fe ion.

EFFECT: high output of hydrocarbon fuels.

11 cl, 9 ex, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method for producing ethylene glycol dimethacrylate, involving transesterification of an ester of methacrylic acid with ethylene glycol, where methacylate is formed by an alcohol containing 1-4 carbon atoms, at temperature ranging from 90°C to 130°C in the presence of lithium chloride in a combination with another chemically active compound as a catalyst and a polymerisation inhibitor and separating alcohol released from the ester of methacrylic acid used, the other chemically active compound used being lithium amide (LiNH2).

EFFECT: method according to the invention enables to obtain ethylene glycol dimethacrylate at a very low cost and having very high purity.

22 cl, 7 ex

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