Method for purification of fatty acid alkyl esters and use of agents to facilitate such purification

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

 

The technical field to which the invention relates

The present invention relates to the use of certain agents to facilitate purification of organic solutions of alkyl esters of fatty acids. The present invention also relates to a method of purification of alkyl esters of fatty acids suitable for use as biodiesel fuel.

The level of technology

Known use as biodiesel alkyl esters of fatty acids (monoalkyl esters of fatty acids, such as methyl and ethyl esters of fatty acids derived from vegetable oils or animal fats. Known methods for producing such alkyl esters of fatty acids include the transesterification of triglycerides comprising vegetable oils or animal fats, in the presence of alcohol and catalyst. In the art it is well known the use of catalysts, such as acid catalysts, or more frequently used catalysts based on alkali metal, for example sodium hydroxide or potassium, or a metal alkoxide such as sodium methoxide or potassium. In fact, the metal alkoxide is a compound formed by the reaction of an alcohol with an alkali metal. Thus, the interesterification reaction can be described in General as follows:

.

Among vegetable oils and animal fats, which can be used are coconut oil, palm oil, oil from plant seeds, olive oil, sunflower oil, soybean oil, rapeseed oil and tall oil. Suitable alcohols which may be used are alkyl alcohols, such as methanol, ethanol, propanol and butanol. Usually in the production of biodiesel using methanol because of its low cost, polarity and short circuit. Due to its high activity as the main catalyst on an industrial scale usually use potassium hydroxide.

Well-known methods for producing alkyl esters include heating, for example, vegetable oils to a temperature usually in the range from 30°C to 110°C. the Method further includes adding to the heated oil, alcohol and catalyst. The reaction will result in two phases, one comprising the obtained glycerin and another that includes the obtained alkyl ether fatty acids. Additionally, the method includes removing the obtained glycerin phase from the phase of the received alkyl ether fatty acids.

Alkyl esters of fatty acids according to known methods, as described above, typically include a too high concentration of impurities, in order to satisfy regulatory nonmonotonically alkyl esters of fatty acids, for example the European standard EN 14214 for the methyl esters of fatty acids, which are particularly limit the impurities originating from the metals K, Na, Mg and Ca. Thus, there is a need for purification of alkyl esters of fatty acids. Known methods of purification include stage neutralization and washing with water, which washes away impurities, and obtain alkyl ether fatty acids, which meets regulatory standards and, thus, can be used as biodiesel fuel. After each stage of the washing water can be separated from the alkyl esters of fatty acids using any method known in the art, such as the expectation that the mixture will separate into two phases, and subsequent removal of the aqueous phase, or by centrifugation of the mixture. Usually the total amount of water used is in the range from 20 to 100% of the water from the total received amount of alkyl esters of fatty acids. After cleaning is completed, it is necessary to remove traces of water contained in the alkyl esters of fatty acids, for example, by re-heating the alkyl esters of fatty acids. Additionally, the water usually contains impurities, which, in turn, must be removed, for example by filtering water and/or by passing water through ion exchange medium. The water then you can re-use the AMB or to consider it simply as waste water.

A disadvantage of the known procedures for purification of alkyl esters of fatty acids using water is that it is difficult to reduce the amount of metal impurities, impurities such as calcium and magnesium to a concentration that meets regulatory standards relative to the alkyl esters of fatty acids, even when using large quantities of water for cleaning. Another disadvantage of the known procedures for purification of alkyl esters of fatty acids using water is that the production of biodiesel, for example, requires a large amount of energy consumed and becomes intensive and costly because the method requires large amounts of water for cleaning, which, in turn, should be cleared.

usnot inventions

From the viewpoint of the above-mentioned aspects of the known methods, the purpose of the present invention is to provide for the use of certain agents, as well as the method of purification of alkyl esters of fatty acids, which are fully or partially eliminates the disadvantages of the known technological methods, and which allows to obtain esters of fatty acids, which is easy to use and which leads to high-quality alkyl esters of fatty acids suitable for use as biodiesel fuel.

The invention determines the independent claims. Embodiments of the invention are evident from the dependent claims and the following description and examples.

According to the first aspect is provided the use of flocculonodular and chelating agent as an agent that facilitates purification of the organic solution comprising alkyl esters of fatty acids.

Under "flocculation and chelating agent" means a reagent, usually polyelectrolyte added to the suspension to combine small particles with the formation of flakes. Additionally, the term includes an agent that can form multiple ties with a metal ion, such as calcium and magnesium. Additionally, the term also refers to the agent, which forms the aqueous phase in the organic solution, where this phase also attracts ions.

Under "organic solution of alkyl esters of fatty acids" mean phase mainly comprising the above alkyl esters of fatty acids, and small amounts of impurities, such as reagents and products of the method of transesterification of triglycerides, such as soap, and ions and metal salts.

Use flocculonodular and chelating agent to facilitate the removal of impurities, impurities such as calcium, magnesium, potassium and sodium. Additionally, processing flocculation and chelating agent when the correct DOB is tion and the removal does not affect the acid number of the product, for example, measured in the form of free fatty acids in the form of different acidity. Acid number of the methyl esters of fatty acids, for example, according to EN 14214 is limited to 0.5 mg KOH/kg of oil (discussed further below).

In one of the embodiments flocculate and chelating agent selected from the group consisting of semi-aluminum coagulants.

Such semi-aluminum coagulants to significantly improve the way in which the subject to remove impurities, impurities such as calcium, magnesium, potassium and sodium, even from non-polar environment of the organic solution of alkyl esters of fatty acids.

In one of the embodiments flocculate and chelating agent is polylysine hydrochloride.

Polyaluminium hydrochloride to greatly facilitates the removal of impurities from the nonpolar environment of the organic solution of alkyl esters of fatty acids, attracting metal ions such as calcium ions and magnesium. Additionally, polyaluminium hydrochloride forms the aqueous phase in the organic solution, this phase also attracts metal ions such as sodium ions and potassium. Moreover, chlorine ions facilitate the removal of ions such as sodium and potassium.

In one embodiment, the implementation of the organic solution is largely besod the output.

The term "substantially anhydrous" should be understood in this context so that the organic solvent does not contain an effective amount of water. The effective amount is such an amount which is sufficient to achieve a significant reduction of the impurity content according to known methods of cleaning using water to flush impurities without adding flocculonodular and chelating agent. The amount of water known as effective in such ways exceeds 10% by weight, typically from about 10% to 60% (by weight) relative to the organic solution. In its narrow definition, the term means that no free water is not required for cleaning, and thus, it is not added to the organic solution during the cleaning method when using flocculonodular and chelating agent. This means that the only water present at any time during the cleaning method, represents water, remaining from a previous processing, such as the way interesterification, and add a connection in the course of cleaning. Adding flocculonodular and chelating agent increases the water content, and this increase depends on the added amount of the agent. To some extent, a small amount of water, for example less than 1000 ppm by mA is CE, will contribute to the formation of phases in the organic solution phase, which attracts ions such as sodium ions and potassium. However, the use of large quantities of water simultaneously with flocculation and chelating agent may have a negative impact on the organic cleaning solution, for example flocculate and chelating agent will not facilitate the removal of impurities.

However, in the preferred embodiment, the maximum water content in the organic solution may be up to 10% (wt./mass.). In a more preferred embodiment, the maximum water content in the organic solution may be up to 9,5, 9,0, 8,5, 8,0, 7,5, 7,0, 6,5, 6,0, 5,5, 5,0, 4,5, 4,0, 3,5, 3,0, 2,5, 2,0, 1,5, 1,0, 0,5, 0,43 or to 0.10% (wt./mass.). In a more preferred embodiment, the water content is from about 100 to 1000 ppm (wt./mass.) and, even more preferably, about 500 h/million Each of these embodiments will allow the presence of a small amount of water until the total water content remains significantly lower than the effective amount of water, as noted above, and thus that there is no negative impact on the cleanup.

According to the second aspect provides a method for purifying an organic solution of alkyl esters of fatty acids suitable for use is as biodiesel, including:

- add flocculonodular and chelating agent to an organic solution for easier cleaning and

- remove part of the organic solution, a specified part includes flocculate and chelating agent and impurities.

This method of purification of alkyl esters of fatty acids makes it possible to reduce the amount of metal impurities, impurities such as calcium and magnesium, to such a concentration that meets regulatory standards relative to the alkyl esters of fatty acids.

In one of the embodiments of the method of removing part of the organic solution includes a step of centrifugation the organic solution thus to remove flocculate and chelating agent together with the impurities, which are solid, polar and/or have other densities compared to alkyl esters of fatty acids.

This method provides a lower cost of energy and becomes less intensive and less expensive than known methods using water to clean the organic solution. Additionally, the efficiency of the method is its ease of control, and the method does not require great control. Moreover, the method can be carried out in a system with a low water content during the entire method. is the aka method does not require water for cleaning, which, in turn, do not need to clean. Additionally, the method leads to a large number of purified alkyl esters of fatty acids, which are suitable for use as biodiesel fuel. This method will also allow you to obtain alkyl esters of fatty acids without the need for a separate neutralization, for example with acetic solution. In the European standards (see above), there is a need to limit the acid number, which includes both fatty and mineral acids in the biodiesel. The maximum value represents 0,5, expressed as mg KOH/g of biodiesel. There is no requirement to pH biodiesel, but necessary, neutralize originate from the formation of metal salts as a by-product of neutralization. As an example, upon receipt of the methyl esters of fatty acids when using methanol and lye organic solution may contain relatively high concentrations of alkali, which, in turn, causes the pH to about 11. In the known methods for material you add vinegar solution.

In one embodiment, the method centrifugation is carried out at reduced pressure to remove water from the organic solution.

In one embodiment of the method to the organic solution in Ho is th way to remove impurities largely do not add water.

The term "substantially not add water" should be understood in the context of the term "substantially anhydrous"as discussed above, i.e. the method includes that cleaning is performed in the absence of an effective amount of free water.

According to one embodiments, the water content of the organic solution of alkyl esters of fatty acids during the process can be up to 10% (wt./mass.). In a more preferred embodiment, the maximum water content in the organic solution during the process could be up to 9,5, 9,0, 8,5, 8,0, 7,5, 7,0, 6,5, 6,0, 5,5, 5,0, 4,5, 4,0, 3,5, 3,0, 2,5, 2,0, 1,5, 1,0, 0,5, 0,43 or to 0.10% (wt./mass.). In a more preferred embodiment, the water content is from about 100 to 1000 parts per million (mass./mass.) and, even more preferably about 500 parts per million. Each of these options will allow the presence of a small amount of water until the total water content remains significantly lower than the effective amount of water, as noted above, and thus that there is no negative impact on the cleanup.

In one embodiment, the implementation of impurities impurities include glycerin, soap, free fatty acids and/or metal.

The method of purification of alkyl esters of fatty acids making it possible to reduce the number of t is such impurities.

In one embodiment, the implementation of the impurity metals originate from metals, including calcium, magnesium, potassium and/or sodium.

The method of purification of alkyl esters of fatty acids makes it in particular possible to reduce the amounts of such metal impurities and even a reduction in the quantities of metal impurities in the final product, intended for use as biodiesel, thus, to comply with regulatory standards.

In one embodiment, the method flocculate and chelating agent selected from the group including semi-aluminum coagulants.

In one embodiment, the method flocculate and chelating agent is polylysine hydrochloride.

The methods and uses according to various aspects of the invention will now be described in more detail with reference to embodiments of, and examples.

Detailed description of the invention and embodiments

The invention relates to the use of flocculonodular and chelating agent as an agent that facilitates purification of the organic solution comprising alkyl esters of fatty acids, in particular monoalkyl esters of long-chain fatty acids, which are suitable for use as biodiesel fuel. In one aspect invented the e also relates to a method of cleaning an organic solution of alkyl esters of fatty acids. The method is used flocculate and chelating agent to facilitate cleaning and removal of organic solution, a specified part includes flocculate and chelating agent and impurities.

The organic solution of alkyl esters of fatty acids to be treated, is a product of vegetable oils or animal fats. In one embodiment, the implementation used oils or fats are newly refined oils or fats, which means that oils or fats have never been used. In another embodiment, used oils and fats are reusable crude oils or fats, such as oils, which were used as oil for frying. Examples of vegetable oils, recently treated or re-used are coconut oil, palm oil, olive oil, sunflower oil, soybean oil and rapeseed oil.

Organic cleaning solution can be obtained according to methods known in the art. Examples of such methods are methods that include or acid, or basic catalysts. Examples of such catalysts are hydroxides of sodium and potassium alkoxides, potassium and sodium and anhydrous sulfuric acid and acetic acid. When processing alkyl EPE is s fatty acids, such as methyl esters of fatty acids, it is desirable achievement system with low water content during the entire method. Such a system will block the formation process water, to increase the resulting output alkyl esters of fatty acids and reduce the receiving side products, such as soap. The final product is intended for use as biodiesel fuel should preferably contain less than 500 ppm water. Thus, it is desirable to use catalysts that do not result in the receipt of or leading to the very small amount of water in the course of obtaining or add them. One example of a catalyst in this context is a methoxide, sodium or potassium, which, in turn, can be obtained by the reaction of methanol with sodium or potassium. One example of a method of producing methyl esters of fatty acids involves the heating of vegetable oil to a temperature usually in the range from 30 to 110°C, depending on the oil, for example from 80 to 90°C when using waste cooking oil, 50°C when using rapeseed oil and a slightly lower when using largely unsaturated oils. The method further includes adding methanol and potassium methoxide or sodium heated to whom the asle. The amount of added potassium methoxide or sodium and methanol depend on, for example, the amount of free fatty acids present in the oil, and the average molecular weight of the oil, each of these parameters can be considered as known to the person skilled in the art. Methanol is usually added in excess. The reaction will result in two phases, one comprising the obtained glycerin and another that includes the obtained methyl esters of fatty acids. Additionally, the method includes removing the obtained glycerin phase, typically comprising approximately 15 to 20% (wt./mass.) from the two phases, obtained from phase methyl ester, for example, gravity or two-phase centrifugation. Additionally, methanol is removed by evaporation using an additional pressure or temperature above the boiling point of methanol. This method will lead to an organic solution comprising up to 99% (wt./mass.) methyl esters of fatty acids, specified organic solution needs cleaning according to the invention.

Now let's move to one aspect of the invention, in which flocculate and chelating agent is used to facilitate separation of the impurities from the organic solution of alkyl esters of fatty acids. It has been unexpectedly discovered that the use of flocculonodular and chelating agent prigoda what about the almost non-polar environment of the organic solution to attract different kinds of metal ions. Additionally, it was found that flocculate and chelating agent facilitates the separation of impurities other than metal ions from the organic solution, such as free fatty acids, Soaps and glycerin, which are polar in comparison with the organic solution. Examples of such flocculosa and chelating agents are semi-aluminum coagulants. Semi-aluminum coagulants have a polymeric structure, and they are known as soluble in water. The length of the polymerized chain, molecular weight and the number of ion charges are determined by the degree of polymerization. During the hydrolysis process various mono - and polymeric species. These Vysokomolekulyarnye chelating agents include, for example, polyaluminum chloride, aluminum hydrochloride and polyaluminium hydrochloride sold in the market as, for example, Ekoflock 54 and Sweflock 10. The advantages of using semi-aluminum coagulants are, for example, that they are cheap, non-carcinogenic, and they attract sodium ions and potassium chloride solution. Examples of other hypothetical types of chelating agents on the market, represent the ferrous chloride of polyalanine, EDTA and acrylamide.

Flocculate and chelating agent together with impurities may be separated and removed from the organic solution method and, such as centrifugation and filtration, or by allowing the mixture to separate into two phases under the action of gravity, or by using any other mechanical devices known to specialists in this field of technology. In a preferred embodiment, the impurities are separated and removed with at least one stage centrifugation.

In one embodiment, the implementation of polyaluminium hydrochloride used as flocculonodular and chelating agent, which is known as a suitable chelating agent for metal ions, such as calcium and magnesium in the water. It was found that the chelating agent polyaluminium chloride is a suitable non-polar environment of the organic solution of alkyl esters of fatty acids, attracting metal ions such as calcium ions and magnesium. Additionally, polyaluminium hydrochloride forms the aqueous phase in the organic solution, this phase also attracts ions such as sodium ions and potassium. Thus, even if less than 100% of ions such as calcium ions and magnesium, chelated flocculation and chelating agent, a sufficient content of the remaining ions will be able to go to the aqueous phase. It should be noted that the traces of the "water content" increase in organic solution after adding polyaluminium guy is rocksichord, elevating when adding it to 1000 ppm (wt./mass.) water to the organic solution, depending on the number of injected polyaluminium of hydroxychloride.

In one of the embodiments flocculate and chelating agent is added when the pH of the organic solution is from 9 to 12. Preferably the pH is 10-11. Based on this flocculate and chelating agent are added directly after the completion of the process of interesterification and removal of methanol and glycerol, as the pH is high, approximately 10.3 to 10.5, and the specified pH decreases over time.

In a preferred embodiment, the organic solution is a substantially anhydrous at the time of adding flocculonodular and chelating agent, which means that the organic solvent does not contain an effective amount of water. The effective amount is such an amount that is sufficient to achieve a significant reduction of the impurity content according to known methods of cleaning using water to flush impurities without adding flocculonodular and chelating agent. The amount of water known as effective in such ways exceeds 10% by weight, typically from about 10% to 60% (by weight) relative to the organic solution is. In its narrow definition, the term means that no free water is not required for cleaning, and thus, it is not added to the organic solution during the cleaning method when using flocculonodular and chelating agent. This means that the only water present at any time during the cleaning method, represents water, remaining from a previous processing, such as the way interesterification, and add a connection in the course of cleaning. Adding flocculonodular and chelating agent increases the water content, and this increase depends on the added amount of the agent. To some extent, a small amount of water, for example less than 1000 ppm by weight, will contribute to the formation of phases in the organic solution phase, which attracts ions such as sodium ions and potassium. However, the use of large quantities of water simultaneously with flocculation and chelating agent may have a negative impact on the organic cleaning solution, for example flocculate and chelating agent will not facilitate the removal of impurities, as will be illustrated in the comparison examples 7 through 10.

However, in the preferred embodiment, the maximum water content in the organic solution may be up to 10% (wt./mass.). In more preferred is entrusted embodiment, the maximum water content in the organic solution can be up to 9.5, 9,0, 8,5, 8,0, 7,5, 7,0, 6,5, 6,0, 5,5, 5,0, 4,5, 4,0, 3,5, 3,0, 2,5, 2,0, 1,5, 1,0, 0,5, 0,43 or to 0.10% (wt./mass.). In a more preferred embodiment, the water content is from about 100 to 1000 ppm (wt./mass.) and, even more preferably, about 500 h/million Each of these embodiments will allow the presence of a small amount of water until the total water content remains significantly lower than the effective amount of water, as noted above, and thus that there is no negative impact on cleaning. The concentration of water in the final product that will be used as biodiesel, must meet regulatory standards and must be equal to or less than 500 ppm (wt./mass.).

According to one aspect of the invention provides a method of cleaning an organic solution of alkyl esters of fatty acids. The method involves the step of adding flocculonodular and chelating agent to the organic solution thus, to facilitate cleaning. Additionally, the method includes a step of removing part of the organic solution, a specified part includes flocculate and chelating agent and impurities.

In one embodiment, the method stage of removal of organic solution includes a step of centrifugation thus, to reduce the amount of impurities is flocculonodular and chelating agent in an organic solution. One example of a centrifuge is a machine with a locked rotor, for example, the model FM600 from Mann-Hummel, which is driven and operates with a continuous flow of the shared environment. The inlet of the centrifuge can be connected with the tank mixing/ vessel and the pump, and the outlet for the purified solution can be, in turn, connected to the specified tank/vessel.

Notes that can be used any centrifuge, as is well known to specialists in this field. During centrifugation compounds that are solids, polar and/or have a density different from the density of alkyl esters of fatty acids, is separated and removed from the organic solution, such compounds as flocculate and chelating agent and admixture. The total number of impurities may be from about 1 to 5% (wt./mass.) the organic solution. Examples of such compounds are contaminants, such as salts and metals, free fatty acids, glycerine and soap. In one of the variants was carried out using a rotary centrifuge (e.g., model FM600 from Mann-Hummel) part, including free fatty acids, glycerine and soap together with flocculation and chelating agent forms a phase in the rotor, the specified phase is a polar than the s with an organic solution of alkyl esters of fatty acids and drained after centrifugation. Metal ions are also located in this part and, thus, are removed simultaneously. In one of the working embodiments centrifugation carried out using a rotary centrifuge model FM600 (Mann-Hummel), at about 4200 rpm with continuous recirculating flow. In one of the embodiments, the centrifugation is carried out at reduced pressure, for example-0.9 bar. It was shown that the low pressure provides, for example, lowering the water content, where the final water content in the organic solution is less than 500 h/million Number of impurities can be, for example, is reduced from approximately 5 to 1% (wt./mass.) the organic solution. Usually the part that is drained from the centrifuge is approximately 1.1% (wt./mass.) in relation to the initial mass loading. Use flocculonodular and a chelating agent such as polylysine hydrochloride, in combination with separation by centrifugation significantly reduces the amount of impurities in organic solution. The number of added flocculonodular and chelating agent depends on the initial concentration of impurities. You can add saturating concentration, or even an excess, calculated from the initial amount of impurities, such calculation is obvious to experts in the given field of technology. The usual amount of composition which is more than 0,5% (wt./mass.), in particular from 0.5 to 2.5% (wt./mass.) the organic solution is subjected to cleaning.

Purified organic solution must meet regulatory standards, for example the European standard EN-14214. According to this regulation specifies the following limits: 5 mg/kg for potassium plus sodium and 5 mg/kg for calcium and magnesium. Examples of values before cleaning and after cleaning using methods that include both centrifugation and adding polylysine hydrochloride, are as shown in the experimental part, for calcium plus magnesium from 11 to 14 and from 0.3 to 2.2, respectively, and for potassium and sodium from 440 to 100 and from 3.9 to 4.1, respectively.

As discussed above, one embodiment of the method includes, in the way significantly do not add water. As will be clear from the experimental side, the water may even have a negative impact on the cleanup.

In one embodiment, the implementation of adding flocculonodular agent to the organic solution passes to any centrifugation. After you have added should be at least one stage of centrifugation to remove impurities together with flocculation and chelating agent. This method does not require or requires little control by the operator, while cleaning can be carried out in one stage-the Oia impurities.

In another embodiment, the organic solution is subjected to at least one stage of centrifugation before carrying out any additions flocculonodular and chelating agent and subsequent stages remove impurities. The advantage of this method consists in the possibility of removal of impurities, particularly soap and glycerine, in almost pure form, before adding flocculonodular and chelating agent, and the possibility of subsequent stages of centrifugation.

According to an additional aspect of the invention provides a method of obtaining an organic solution comprising alkyl esters of fatty acids, in particular monoalkyl esters of long-chain fatty acids, which are suitable for use as biodiesel fuel. The method includes obtaining organic solution is subjected to purification, as described above, and cleaning of the specified organic solution according to aspects of the invention related to the cleanup.

Examples

Hereinafter the invention will be further illustrated by non-limiting detailed descriptions of the experiments conducted in accordance with them. In these experiments tested aspects of treatment with or without added flocculonodular and a chelating agent and its concentration.

Examples 1 to 6

Test procedures

Each of the experiments in examples 1 to 6 were carried out with the use of the party organic solution of the methyl esters of fatty acids obtained by using one of the options for implementing the above described method interesterification, which was used as the catalyst sodium methoxide or potassium hydroxide and methanol as the alcohol. Add the catalyst for potassium methylate was 0,64% by weight of the organic solution and sodium methylate was to 0.45 mass%. Methanol was added in a stoichiometric amount plus 50% by weight. After completion of the transesterification glycerin phase was decanted and the excess methanol was removed under reduced pressure (- 0.9 bar), leaving the rest of the party organic cleaning solution. The lot size for each experiment was approximately 3000 kg

Experimental conditions for cleaning

In all experiments, the centrifugation was performed using a rotary centrifuge (model FM600 from Mann-Hummel) at 4200 rpm for six hours at 55°C under reduced pressure (- 0.9 bar).

As flocculonodular and chelating agent used polyaluminium hydrochloride (catalog No. 1327-41-9, Eka Nobel). Add the number ranged from 0 to 2.25% by weight of the organic solution.

Poly is lumini hydrochloride was added way after interesterification and after removal of glycerol and excess methanol, while pH remained high, the specified pH was determined as approximately 10.3 to 10.5.

Analysis of metal contents

The levels of Mg, Ca, Na and K were determined using ICP analysis (inductively coupled plasma with argon) using equipment from Spectro GmbH. Analyses were performed based on standard methods described in ASTM D 4951-96, ASTM 5708-95a, ASTM 5185-95, DIN 51390-4, DIN 51391-3 and DIN 51790-6, in accordance with which a spectral line 183801/393366, 285213, 589592 and 766,490 nm was used for determination of the concentration of the contained metals for Ca, Mg, Na and K accordingly, the determination of concentrations is obvious to a person skilled in the technical field.

Analysis of water content

The water content was analyzed volumetric using calcium hydride (CaH2). The hydride reacts with water with the formation of gas pressure, which is measured using specialized for these purposes sensor (sensor-meter in the so-called set Mobil water test No. 429950 produced Signum/ExxonMobil).

Table 1
Results: Examples 1 to 5
Example numberThe origin of the organic solution of the methyl esters of fatty acidsThe initial content of Ca+Mg/Na+K (mg/to the) Polyaluminium hydrochloride (%(wt./mass.))The final content of Ca+Mg/Na+K (mg/kg)
1Rapeseed oil14,3/1220,57,5/8,7
2Used cooking oil1,9/4412,250,3/5,0
3Used cooking oil2,2/44102,2/29,1
4Refined oil for frying0,5/270,641,1/4,1
5Rapeseed oil6 / 25 number0,71,7/8,3

From the data presented in table 1, it is obvious that after obtaining an organic solution comprising alkyl esters of fatty acids prior to any treatment, the quantity of calcium plus magnesium and potassium plus sodium may vary between approximately 20 and 100-450 mg/kg, respectively. After processing the material is and polyaluminium hydrochloride, followed by centrifugation metal content substantially decreased.

In example 3, the results were obtained by the stage of centrifugation, but without adding any flocculonodular and chelating agent. The results show that the metal content is somewhat decreased, but not to the levels obtained using the purification by a combination of centrifugation and add flocculonodular and chelating agent.

For example 5 it should be noted that the results were obtained using somewhat faulty centrifuges.

Results: Example 6

In one of the experiments, analyzed the water content in the organic solution. The water content was highest immediately before centrifugation and was identified as 0,43% (wt./mass.). After centrifugation for two hours the water content amounted to 0.23% (wt./mass.), and after centrifugation was complete, the water content was determined as 0.12% (wt./mass.). It was shown that a relatively high water content after centrifugation was the result of faulty centrifuges. In other experiments, the final water content was determined as lower than 1000 ppm (wt./mass.), and in the final product is less than 500 ppm (data not shown).

The comparison examples 7 to 10

Test procedures

Each of experiment is in examples 7 to 10 were carried out with the use of the party organic solution of the methyl esters of fatty acids, as described above in examples 1 through 6. In each experiment as the source of material used rapeseed oil. The amount of biodiesel used for cleaning in each experiment was 100 g per experiment. Purification of the resulting organic solution was performed in a similar way as described in examples 1 through 6, except that did not phase removing part, including impurities by centrifugation. Instead, the organic solution washed with water. Washing consisted of mixing water with an organic solution, and removing water from the organic solution. Spent three stages of washing, in which was added 20% (wt./mass.) water was removed in each stage. This method is reminiscent of the ways in the art, in which the water is used to wash the organic solution. The only difference in comparison with known methods consisted in the fact that flocculate and chelating agent were mixed with an organic solution before spent any washing water. Stage mixing with flocculation and chelating agent was carried out before stage of leaching. After washing with water, the remaining traces of water were removed, leaving the organic solution in a water bath at 50°C. until the water content became less than 500 h/million

Table 2
Results: Examples 7 to 10
Example No.78910
The added amount of Al(OH)Cl
(% wt./mass.)
00,50,71,0
The number of remaining Na+K (mg/kg)9,914,27,613,2
The number of remaining Ca+Mg (mg/kg)4,23,54,2the 3.8
The number of remaining Cl (mg/kg)<1<1<1<1

From the data shown in table 2, it is obvious that washing with water (3×20 wt. -%/mass.) without centrifugation simultaneously with flocculation and chelating agent will not have a correct action, reducing admixtures of metals, even compared to washing with water without adding any flocculonodular and Heathrow is his agent. Only the values for calcium plus magnesium have approved values. The reason for the relatively high residual metal impurities may be due to the characteristics of low water solubility of the complexes formed flocculation and chelating agent. Moreover, as can be seen from the low residual chloride in the final product, the mechanism for the use of washing water can prevent potassium plus sodium to form chlorides simultaneously with flocculation and chelating agent. Instead of the chloride ions, apparently, preferably migrate into the water and, thus, are washed away without metals and flocculonodular and chelating agent. The concentration of the chloride ions to clean and after adding flocculonodular and chelating agent can be up to 11 mg/kg

These results also show that the addition of water simultaneously with flocculation and chelating agent may have a negative effect on the organic cleaning solution, i.e. flocculate and chelating agent will not facilitate the removal of impurities, even if the cleaning process includes a step of centrifugation.

Examples 11 and 12

Test procedures

Each of the experiments in examples 11 and 12 were carried out with the use of the party organic solution of methyl ester is a fatty acid, purified and analyzed as described above in examples 1 through 6, except that added a different amount of catalyst, and that the lot size was approximately 3000 kg in example 11 and about 16000 kg in example 12. In example 11, the catalyst was a potassium methylate in an amount of about 0,78% by weight of the organic solution. In example 12 catalyst was a sodium methylate in an amount of about 0.51 percent by weight of the organic solution.

Table 3
Results: Examples 11 and 12
Example numberThe origin of the organic solution of the methyl esters of fatty acidsPolyaluminium hydrochloride (%(wt./mass.))The final content of Na+K (mg/kg)The final content of Ca+Mg (mg/kg)
11Rapeseed oil0,61,5<0,5
12Sunflower oil0,54,40,4

From the data shown in table 3 clearly, when processing the organic solution of the methyl esters of fatty acids polyaluminium hydrochloride, followed by centrifugation, the content of metals was significantly reduced, even when the organic solution was obtained from sunflower oil.

1. Application flocculonodular and chelating agent as an agent that facilitates purification of the organic solution comprising alkyl esters of fatty acids, in which the water content of the organic solution is equal to or less than 5% by weight, and where the pH of the organic solution is from 9 to 12, and where flocculate and chelating agent selected from the group consisting of semi-aluminum coagulants.

2. The use according to claim 1, in which flocculate and chelating agent is polylysine hydrochloride.

3. The use according to any one of the preceding paragraphs, in which the water content of the organic solution is equal to or less than 4,5, 4,0, 3,5, 3,0, 2,5, 2,0, 1,5, 1,0, 0,5, 0,43 or to 0.10% (wt./wt.), more preferably from about 100 to 1000 h/mn (wt./wt.) and even more preferably about 500 hours/mn (wt./wt.).

4. The method of purification of the organic solution of alkyl esters of fatty acids suitable for use as biodiesel fuel, including:
- add flocculonodular and chelating agent of choice and the group, consisting of semi-aluminum coagulants, organic solution for easier cleaning when the pH of the organic solution is from 9 to 12, and
- remove part of the organic solution, a specified part includes flocculate and chelating agent and impurity,
where the water content of the organic solution of alkyl esters of fatty acids during the entire method is equal to or less than 5% by mass.

5. The method according to claim 4, in which the removal of part of the organic solution includes a step of centrifugation the organic solution thus to remove flocculate and chelating agent together with the impurities, which are solid, polar and/or have other densities compared to alkyl esters of fatty acids.

6. The method according to claim 5, in which the centrifugation is carried out at reduced pressure to remove water from the organic solution.

7. The method according to any one of claims 4 to 6, in which the water content of the organic solution of alkyl esters of fatty acids during the entire method is equal to or less than 4,5, 4,0, 3,5, 3,0, 2,5, 2,0, 1,5, 1,0, 0,5, 0,43 or to 0.10% (wt./wt.), more preferably from about 100 to 1000 h/mn (wt./wt.) and even more preferably about 500 hours/mn (wt./wt.).

8. The method according to claim 4, in which impurities include glycerin, soap, free fatty acid and/or mixture of metals.

9. The method according to the .8, in which impurities of metals originate from metals, including calcium, magnesium, potassium and/or sodium.

10. The method according to claim 4, in which flocculate and chelating agent is polylysine hydrochloride.



 

Same patents:

FIELD: oil and gas industry.

SUBSTANCE: method involves preparation of raw material, stage-by-stage treatment and obtaining of fuel. Preparation of raw material is performed by means of refining. Treatment is performed at three stages. At the first stage fish oil is mixed with absolute ethanol or methanol in ratio of 1:2-1:5. At the second stage concentrated sulphuric acid in quantity of 2-10% is added to the obtained mixture and ester interchange reaction is performed at temperature of not more than 40°C during 20-60 min. At the third stage the mixture temperature is brought to boiling temperature and kept at this temperature during 60-480 min with separation into glycerin and mixture of ethyl or methyl ethers of fatty acids. Then, mixture is neutralised with alkali liquor, washed with water and settled. After that, impurities are removed by centrifuging so that fuel is obtained, which is then dehydrated and cleaned.

EFFECT: improving physical and chemical properties.

3 cl, 1 tbl, 5 ex

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SUBSTANCE: randomisation is performed at presence of catalyst - potassium hydroxide - at continuous mixing components in reactor of randomisation. Upon completion of mixing produced mixture is pumped over into a settling reservoir where mixture settles for not less, than twenty four hours. Further, settled glycerine is drained from the settling reservoir whereto water is pumped. After not less, than twenty four hours, settled water is drained into a reservoir for water, while residue is dried to finished product. Preferably, vegetable oil should be heated to temperature 66÷68°C before randomisation.

EFFECT: simple and safe procedure for production of lubricating additive to diesel fuel corresponding to mixture of ethyl ethers of fat acids.

2 cl

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: present invention relates to a reesterification catalyst and its preparation method. The invention describes a reesterification catalyst of general formula: Zn3M2(CN)n(ROH)·xZnCl2·yH2O, where R is tertiary butyl and M is a transition metal ion selected from Fe, Co and Cr; x lies between 0 and 0.5, y lies between 3 and 5 and n equals 10 or 12. Described is a method of preparing the catalyst, involving the following steps: a) dissolving ZnCb in a mixture of water and tertiary butanol, b) adding the said solution obtained from step a) to an aqueous solution of K4Fe(CN)6 while stirring, c) adding a ternary block copolymer of poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (EO20-PO70-EO20; molecular weight of approximately 5800), dissolved in a mixture of tert-butanol and water, to the above mentioned mixture obtained at step (b) while stirring and at temperature 25°C-70°C, d) filtering the reaction mixture obtained at step (c) to obtain a solid product ad then washing with distilled water and drying at temperature 20-50°C and e) activating the said dried solid product at temperature 150-200°C to obtain the desired reesterification catalyst.

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12 cl, 2 tbl, 12 ex

FIELD: food industry.

SUBSTANCE: invention relates to compositions of breast milk fat substitutes, methods of their production, compositions of fat bases and methods of their production; baby formula containing specified substitutes. Composition of fat base according to invention includes mixture of triglycerides of vegetable origin, characterised by the fact that less than 50% of remains of fatty acids bound in sn-2 position are saturated; and/or amount of remains of saturated fatty acids bound in sn-2 position of glycerin frame makes less than approximately 43.5% of overall amount of remains of saturated fatty acids, 45-65% parts of unsaturated fatty acids in sn-1 and sn-3 positions make parts of oleic acid and/or 7-15% parts of unsaturated fatty acids in sn-1 and sn-3 positions make parts of linoleic acid. Composition of breast milk fat substitute according to invention includes mixture of at least 25% or at least 30% of specified composition of fat base according to the invention and up to 75% or accordingly up to 70% of at least one vegetable oil, in which specified vegetable oil is randomised. Baby formula according to invention includes composition of fat base or composition of breast milk fat substitute.

EFFECT: compositions of fat base make it possible to optimally imitate breast milk fat and are suitable for use in various baby formulas, and methods of production provide for low consumption of fat bases in process of their production.

28 cl, 17 tbl

FIELD: process engineering.

SUBSTANCE: invention relates to oil-and-fat industry. Method and system for fermentative treatment of initial material containing lipides comprises brining initial material in contact with process admixture, passing initial material at, in fact, constant flow rate through treatment system that includes several reactors with ferments and stationary layer connected in series. Reactors with stationary layer may be serviced individually while initial material flow rate being, in fact, constant in cutting one reactor off for servicing purposes. Process admixture is, in fact, dehydrated silicon dioxide with pore size exceeding 150 angstrom. Said admixture may be placed in one or several reactors above layer of ferment, or be placed in pretreatment system that includes one or several reactors.

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32 cl, 6 dwg, 20 tbl, 6 ex

FIELD: food industry.

SUBSTANCE: composition consists of an interesterified fat prepared by interesterification of a mixture containing 5-95 % of at least one dodecanic fat and 95-5 % of at least one non-dodecanic fat; the composition of non-hydrogenised vegetable fats contains at least 50 wt % and less than 15wt % of solid fat (SFC) at a temperature of 20°C and 35°C accordingly; the composition of non-hydrogenised vegetable fats contains C12+C16 fatty acids in an amount of at least 55wt % of the total weight of the fat composition, the C12/C16 of fatty acids ratio being at least 1. The mixture of at least one dodecanic fat and at least one non-dodecanic fat undergoes a process of chemical and fermentative interesterification. The produced fat is added to the composition of confectionery fat, a confectionery product, coffee whitener or an ice-cream composition.

EFFECT: invention allows to produce a fatty composition suitable for application in confectionary industry; this composition does not undergo hydrogenisation and needs no tempering; it is characterised by a high profile of solid fats content, a property to melt well when in the mouth, a waxy sensation absence, good thermal endurance and rather a high crystallisation rate.

17 cl, 3 tbl, 3 ex

FIELD: chemistry.

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EFFECT: obtainment of mix with high content of high-purity alkyl esters.

46 cl, 8 ex

FIELD: chemistry.

SUBSTANCE: method of producing methyl ether of fatty acid (biodiesel) from oil, containing triglycerides and obtained from plants involves: (i) squeezing out oil from seeds and separation of the residue for use as manure, (ii) neutralisation with an alkali of the excess free fatty acid contained in the oil, and separation of the soap residue, (iii) addition of an antioxidant and blowing the oil with dry air to reduce water content, (iv) treatment of the oil with the respective amount of methanol solution of KOH, dried over anhydrous sodium sulphate, (v) separation of the glycerin layer formed during the reaction, (vi) treating the methyl ether of fatty acid with glycerin in two steps to further reduce content of methanol, catalyst and other impurities in the layer of methyl ether of fatty acid, (vii) separation of glycerin, (viii) washing the layer of methyl ether of fatty acid with water in two steps to minimise content of impurities, (ix) separation of washing water, (x) addition of an additional amount of antioxidant to the methyl ether of fatty acid and with blowing dry air to minimise water content, (xi) combination of the glycerin layers and treatment with SOx or flue gas to convert spent KOH catalyst to K2SO4 or K2CO3 respectively, (xii) setting the pH to approximately 7 and distillation of methanol from the glycerin layer, (xiii) hot centrifuging the remaining mass to separate potassium salts from glycerin, (xiv) washing the salt to remove impurities, (xv) separation of the required amount of crude glycerin for washing the layer of methyl ether of fatty acid in the next portion as well as for other uses where crude glycerin is used, and (xvi) distillation of the remaining crude glycerin with low content of water to obtain pure glycerin.

EFFECT: obtaining biodiesel which meets international standards with high output.

21 cl, 18 ex

Fat compositions // 2374860

FIELD: food industry.

SUBSTANCE: invention refers to fat-and-oil industry. Fat composition (versions) containing triglyceride mixture or containing fat fraction with low melding temperature consisting of triglyceride mixture which consists of fatty acids. The acids consist of rests of palmitic, stearic and arachic acids in quantity 40-70 wt %, rests of oleic, linolic and linolenic acids and C18-trans-unsaturated fatty acids in quantity 25-60 wt % which are rests of C18-trans-unsaturated fatty acids, rests of other fatty acids which make rests of behenic acid where total content of triglycerides S2U-Type makes 35-90% in certain SSU/SUS triglycerides ratio and content S3-triglycerides where S represents saturated fatty acids and U - unsaturated fatty acidsand additionally contains sorbitan tristearate. Method provides a) interchange of base triglycerides mixture based on vegetable oils conteining rests of C18-trans-unsaturated fatty acids and fractioning of interchanged mixture for obtaining of triglycerides mixture and addition of sorbitan tristearate or b) interchange of base mixture based on vegetable oils and fractioning of interchanged mixture is possible after or with following hydrogenation for production of triglycerides mixture and addition of sorbitan tristearate or c) interchange of base triglycerides mixture based on vegetable oils and fractioning of interchanged mixture is possible after or with following addition of fatty componentswith high melting temperature and addition of sorbitan tristearate. Obtained fatty composition is added to the food product for human and other mammals, into confectionary goods, baking products filler, into chocolate and chocolate-like products, into cosmetics, pharmaceutical or parapharmaceutical (over-the-counter) product. It is also used in confectionary goods.

EFFECT: invention allows to produce composition with low trans-fat content with high consolidation speed; composition also consolidates in stabile form without preliminary processing.

27 cl, 2 dwg, 12 tbl, 7 ex

FIELD: food industry.

SUBSTANCE: invention relates to complex processing of gadidae fishes liver. The method envisages milling liver and blending it with oil and water at specific ratios. Then one performs stratification, centrifugation and separation which results in production of lipidic and hydrophilic complexes and a dense fraction.

EFFECT: invention allows to process gadidae fishes liver without heat treatment preserving valuable biologically active substances.

6 cl, 15 ex

FIELD: food industry.

SUBSTANCE: vacuum vessel for continuous or semicontinuous treatment of oils with deodorisation contains spaces (12, 121, 122) wherethrough one performs transmission of oil subject to treatment and a device for oil heating or cooling in the shape of U-pipes. There are perforated pipes (26) in the low part of the said spaces for stripping-gas delivery into the said oil. The vessel has connection to a source (7) of vacuum. The spaces in the vessel are positioned so that the oil (which is subject to treatment in the vessel) flows through it by gravity. The heating or cooling medium moving through the U-shape pipes is pumped through them. The U-shape pipes for the heating and cooling medium are located in the said spaces in such a manner that the oil flow is in a contraflow to the flow of the heating and cooling medium along the whole length of the vessel; several U-shape pipes are composed into groups (13), parallel and arranged in rows one above other in the said spaces. The vacuum vessel is designed for preliminary heating of fixed oils subject to deodorisation by previously deodorised oil and exposing the said deodorised oil to further treatment with stripping-gas.

EFFECT: improved efficiency of heat-exchange between the oil and the heating or cooling medium under conditions of the vacuum vessel size restriction.

11 cl, 5 dwg

FIELD: fat-and-oil industry; methods and devices for purification of the vegetable oils.

SUBSTANCE: the invention is pertaining to the fat-and-oil industry and may be used for purification of the vegetable oils with the subsequent withdrawal of the phospholipids. The method of purification of the vegetable oil provides for commixing of the vegetable oil and the hydratable solution, affecting on the received admixture by the pressure and the ultrasound. The production line for the vegetable oil purification includes the coupled by the pipeline system tanks with the crude oil and the hydratable solution, the mixer, the pump, the sediment trapping device, the cavitational-ultrasonic oscillator made in the form of the body with slits and mounted in it the conical nozzle and the deflector. The mixer is combined with the pump. Between the cavitational-ultrasonic oscillator and the pump there is additionally mounted bypass valve. The surface of the deflector of the cavitational ultrasonic oscillator is made relief and the slits in the body are made tangentially. The invention ensures acceleration and simplification of the process of withdrawal of the phospholipids and improvement in quality of the vegetable oil purification.

EFFECT: the invention ensures acceleration and simplification of the process of the phospholipids withdrawal and the improved quality of the vegetable oil purification.

2 cl, 3 dwg

FIELD: food industry, namely, fat and oil branch.

SUBSTANCE: vacuum evaporator plant for vegetable oils consists of vacuum apparatus, condenser and vacuum pump. Device differs from other because vacuum apparatus is made in form of horizontal vessel, made of continuous pipe in form of several mated similar segments of cylinder with large segment of cylinder, and connected to heat carrier circulation contour. Shafts are positioned along axis of large segment of cylinder with possible rotation in different directions, snake-shaped perforated blades being attached to aforementioned shafts.

EFFECT: decreased oil heating temperature and expanded evaporation surface.

2 dwg

FIELD: fat-and-oil industry.

SUBSTANCE: process comprises providing oil-containing vegetable raw material, extracting oil from oil-containing vegetable raw material by way of pressing it and separating oil cake. Extraction of oil from resulting oil cake on extraction installation (which is a part of the invention), wherein two cake deoiling are combined: mixing of cake with extractant used at weight ratio 1:(1.9-2.2) for 10-15 min and final counter-current deoiling on inclined screw extractor to residual content of fat in the cake not higher than 1%. Oil obtained through pressing and extraction is refined using complex refiner consisting of three constituents. The first constituent is high-molecular weight electrolyte or mixture of high-molecular weight electrolytes; the second one is low-molecular weight electrolyte or mixture of low-molecular weight electrolytes; and the third one are organic and/or inorganic peroxides and/or hydroperoxides, taken at weight ratio 1:(25-250):(0.5-2.0), respectively. Refiner is used in amount of 0.2 to 1.5% of the total weight of oil being refined. Mixing of the oil being refined with complex refiner is effected no longer than 30 min at temperature between 0 and 100°C by way of creating spiral trajectory of movement of resulting mixture in a suitable apparatus (which is a part of the invention), after which mixture is settled.

EFFECT: achieved high-performance vegetable oil production technology owing to reduced losses of oil in extraction and refining processes.

30 cl, 2 deg, 1 tbl, 5 ex

FIELD: food processing industry, in particular production of functional foodstuffs.

SUBSTANCE: claimed oil is obtained by treatment hydrated corn oil in thin (0.1-0.2 mm) film helix-rotating at rate of 20-40 c-1 at 60-80°C followed by neutralizing of treated oil with aqueous sodium silicate with concentration of 200-270 g/l under excess of 5-15 % at 60-80°C, and separation of neutralized oil from soap stock by settling. Neutralized oil is washed with water in amount of 5-15 % based on oil mass at 80-90°C followed by separation of washed neutralized oil from washing water, settling, filtering and deodorization at 160-170°C and residual pressure of 1-3 mm Hg.

EFFECT: vegetable oil useful in normalizing of lipid metabolism, particularly in reducing of lipid levels in blood and liver.

3 tbl, 3 ex

FIELD: food industry; vegetable oil deodorizers.

SUBSTANCE: proposed plant includes reservoir for raw vegetable oil, horizontal deodorizer, scrubber, heating unit, return water system, ready product accumulating reservoir and system of pipelines with shutoff valves and cooler. Reservoir for raw vegetable oil is connected through filter with heat exchanger, vacuum system consisting of mixing condenser of vapor ejector vacuum pump connected with scrubber and connected return water system, and deaerator connected with vacuum system and, through pipeline, with heat exchanger, electric heater and deodorizer. Heating unit is formed by series-connected heat exchanger and electric heater with temperature controls at outlet. Deodorizer is connected through pump to electric heater for oil circulating along circuit, and cooler. Plant contains additionally mixer with citric acid solution. Cooler is connected through mixer containing citric acid solution with ready product reservoir, and scrubber is provided with pipeline to deliver sprinkler oil.

EFFECT: reduced heat and power consumption and working area of plant, and improved quality of ready product.

1 dwg

FIELD: food processing industry.

SUBSTANCE: functional-destination corn oil is produced by treating hydrated corn oil in helically rotating thin (0.1-0.2 mm) film at rotation speed 20 to 40 c-1 and 60-80°C. Thus treated oil is neutralized with 5-15% excess of sodium silicate aqueous solution (200-270 g/L) at 60-80°C and neutralized oil is then separated from soap stock by settling. Neutralized oil is further washed with water in amount 5 to 15% based on the weight of oil at 80-90°C and washed oil is settled to separate water, dried, filtered, and deodorized at 160-170°C and gauge pressure 1-3 mm Hg.

EFFECT: achieved retention of a large amount of tocopherols possessing strong antioxidant properties.

3 tbl, 3 ex

FIELD: food processing industry.

SUBSTANCE: functional-destination corn oil is produced by treating hydrated corn oil in helically rotating thin (0.1-0.2 mm) film at rotation speed 20 to 40 c-1 and 60-80°C. Thus treated oil is neutralized with 5-15% excess of sodium silicate aqueous solution (200-270 g/L) at 60-80°C and neutralized oil is then separated from soap stock by settling. Neutralized oil is further washed with water in amount 5 to 15% based on the weight of oil at 80-90°C and washed oil is settled to separate water, dried, filtered, and deodorized at 160-170°C and gauge pressure 1-3 mm Hg.

EFFECT: achieved production of oil reducing excess content of cholesterol in blood serum and in liver.

3 tbl, 3 ex

FIELD: fat-and-oil industry, in particular, vegetable oil refining processes.

SUBSTANCE: method involves freezing out vegetable oil while adding auxiliary filtering powders; holding vegetable oil at low temperature; separating used filtering powder with wax-containing sediment from refined vegetable oil and regenerating separated used filtering powder; during regeneration process, mixing used filtering powder with additionally introduced fatty product to pasty state; heating while mixing to temperature sufficient for melting of all wax fractions and separating resultant mixture by centrifuging into regenerated dry filtering powder and wax-containing fatty product. Regenerated filtering powder produced may be utilized multiple times in the processes of freezing out of vegetable oil.

EFFECT: increased adsorptive activity with respect to wax globules on surface of filtering powder particles, reduced total consumption of filtering powder, obtaining of concentrated wax-containing fatty products immediately from used sediments, reduced loss of winterized oil due to blocking of inner pores of particles by wax-containing fat product.

FIELD: chemistry.

SUBSTANCE: invention concerns oil and fat industry. The method involves reacting oil with an adsorbent - a natural kaolinite-β-quarts mixture. Oil is passed through an adsorbent which is in form of granules with diametre of 3-5 mm and height of 5-7 mm at room temperature. The granules are obtained by moulding a natural mixture in the presence of sodium silicate solution with density of 1.32-1.43 g/cm3 in mass ratio of solid: liquid = 4:1-5:1 with subsequent cutting and drying to constant mass at 110-120 °C.

EFFECT: invention increases degree of purity of plant oil, excludes energy consuming operations and enables carrying out the process in continuous mode.

2 cl, 1 tbl, 3 ex

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