Method for extraction of carbonyl and (or) acid compounds from complex multicomponent organic mixtures

FIELD: chemical technology.

SUBSTANCE: invention relates to the improved method for extraction of carbonyl and (or) acid compounds from the complex multicomponent organic liquid mixtures. Method involves treatment of organic liquid mixtures with sodium sulfite an aqueous solution at intensity of mechanical stirring providing formation of uniform emulsion. The content of carbonyl compounds and acids in the parent mixture to be treated is determined and treatment is carried out with 4.16-26% aqueous solution of sodium sulfite as measured 1.05-1.1 mole of sodium sulfite per 1 g-equiv. of carbonyl compound, and in exceeding of the content of acids (g-equiv.) in the parent mixture over the content of carbonyl compounds - with 1 mole sodium sulfite per 1 g-equiv. of acids and in the mass ratio of sodium sulfite aqueous solution to organic mixture = (1-2.5):(2-1) at temperature 15-30°C; if the content of acids in the parent mixture (g-equiv.) is less the content of carbonyl compounds (g-equiv.) then under control of pH value change in an aqueous phase method involves additional addition of mineral or organic acid in the amount as a difference in the content of carbonyl compounds (g-equiv.) and the content of acids (g-equiv.) in the parent charge of organic mixture per treatment at such rate that pH value of aqueous would decrease constantly but not less 6.5. This simple method provides removing both carbonyl compounds and acids being without significant limitations for the content of carbonyl compounds and acids in the parent mixture. Invention can be used in different branches of industry for treatment of compositions or for utilization of carbonyl compounds and (or) acids.

EFFECT: improved method for extraction.

5 cl, 3 tbl, 26 ex

 

The invention relates to the technology of extraction of carbonyl and (or) acid compounds from complex multi-component organic liquid mixtures and can be used in various industries for cleaning compositions from carbonyl compounds and simultaneously from acids or for the disposal of carbonyl compounds and / or acids.

A method of obtaining gidrooksilirovania (A.S. USSR №571472), where in order to protect the aldehyde group of citronellal is treated with a solution of sodium sulfite, maintaining pH 7.0 to 8.3 and the constant addition of acid.

The disadvantage of this method is that it involves the interaction with sodium sulfite most of the reaction of the aldehyde carbonyl group, and the neutralization of the liberated alkali start, when a significant portion of the aldehyde manages to turn into hydrosulfite derived.

Closest to the claimed is a method of separation of citral from citratesteriod essential oils or semi-products of its synthesis (A.S. USSR №1774616), under which evolved in the course of processing an aqueous solution of sodium sulfite lye is neutralized with carbon dioxide so that during the process the pH is maintained within the range of 9.0 to 9.5, reducing to 8.0 at the end of the process.

The disadvantage of this method, as given above, is the tsya, as the reagent is taken individual aldehyde, and is present in the mixture in fairly large quantities (48-72% wt.), which reacts with the sodium sulfite is much easier and faster than any of even the most reactive ketone. These two factors determine that the process can be conducted at pH 9.0 to 9.5 and finish with decreasing pH to 8.0 with the release of ˜ 80-90%.

If this method be extended to the initial content of aldehyde to 10 wt.%, the degree of extraction will be much lower than 50%, and when replacing the aldehyde in acetone, for example, will be reduced to 10% and below (Iaianou, Ossobranie, Vmimages, Amiano. Some ways of increasing the degree and rate of conversion of sulfite sodium bisulfite derivatives by direct interaction with carbonyl compounds. // Proceedings of the Kursk state technical. Univ. Kursk, 2003, Pp.52-57).

On the other hand, proposed in the cited method, the process is slow (for example 1 is 2.5 hours plus 0.5 hour to reduce the pH to 8.0 and 8.1).

Moreover, carbonic acid (water solution of carbon dioxide) is weak and will react mainly with sodium hydroxide, but not with sodium sulfite. As a result, the latest move in hydrosulfite will be slowed down. So easy and quick interaction with carbonyl compounds, and consequently, Uwe is icene the degree of conversion of the latter to 95% and above, regardless of the initial concentration of carbonyl compounds in the composition will not occur.

And since the dissolution of CO2in water, the process is quite slow, his breakthrough is inevitable, especially at low pH values, resulting in higher costs of this reagent and will make it impossible to monitor progress by measuring the number filed in the system carbon dioxide.

The objective of the proposed solutions is to reduce the dependence of characteristics of the process from the nature of the carbonyl compound and its content in the composition, parallel with carbonyl compounds removal present in the original composition of carbon and impurities of mineral acids and excluding the dependence of the final result on the molar ratio of carbonyl compounds and acids in processed blended composition.

The problem is solved in that define the content of carbonyl compounds and acids in the original mixture, processing lead 4,16-26%aqueous solution of sodium sulfite from the calculation of 1.05-1.1 mol of sodium sulfite in 1 g-EQ carbonyl compounds, while exceeding in the original mixture of acids (g-EQ) over the content of carbonyl compounds 1 mol of sodium sulfite in 1 g-EQ of acid, and the mass ratio of the aqueous solution of sodium sulfite and organic compounds 1-2,5:2-1, at a temperature of 15-30°and if the content of the sour is in the initial mixture (g-EQ) less than the content of carbonyl compounds (g-EQ), while monitoring the change of the pH value of the aqueous phase enters the additional mineral or organic acid in a quantity equal to the difference of content of carbonyl compounds (g-EQ) and acids (g-EQ) in the initial download of the organic mixture to be processed, with such speed, that the pH of the aqueous phase is continuously decreased, but not below 6.5.

While the introduction of the additional acid start after 1.5-10 min, during which time almost completely consume all able to respond in these circumstances the acid. And the process in the case where the acid content (g-EQ) exceeds the content of carbonyl compounds (g-EQ), or equal to, conduct without entering additional mineral or carboxylic acids within 4-10 minutes

As additionally added acid using hydrochloric, Hydrobromic, nitric, sodium hydrosulphate, sulfuric, acetic, Chloroacetic, trichloroacetic, oxalic, malonic, benzoic. This added acid is administered in the form of water or alcohol (for poorly water-soluble acid) solution with a concentration 1-11 g-EQ/liter

Characteristics of the raw materials used

Sodium sulfite according to GOST 195-77.

Organic composition:

Solutions oxidative vegetable oils and fats in white-spirit.

Off-grade vegetable oil and fish oil with the original HT>8 mg To The H/g and high water content are oxidized by air in the mode of bubbling at a temperature of 100-120° To obtain oxidation in the specified viscosity range. Such oxidati contained 0.3 mol/kg carbonyl compounds and had an acid number of up to 25 mg KOH/g Without removal of carbonyl compounds and reduce the acid number for the use they were unsuitable.

Acid oil.

It is collected and separated from the aqueous phase entrapped volatile products and drip ash in the air oxidation in the temperature range 125-165°predominantly sunflower oil in the basics of film-forming agents for drying oils of the type "oksol". Contain up to 5.0 mol/kg carbonyl compounds and up to 3.0 g-EQ/kg of acid in their varying proportions. Targeted use of do not have. Have a sharp odor. Recycling of the components are not developed. Often be incinerated afterburners.

Butter UNDER THE 113-03-476-82.

Oil (a mixture of high-boiling oxidation products of cyclohexane, dehydrogenation of cyclohexanol, polycondensation cyclohexanone); widely used in leather and other industries.

White spirit according to GOST 3134-78.

Acid:

Salt according to GOST 3118-77

Hydrobromic according to GOST 2062-77

Nitrogen according to GOST 4461-77

The sodium hydrosulphate according to GOST 6053-77

Sulfur according to GOST 4204-77

Acetic according to GOST 61-75

Chloroacetic according to GOST 5836-77

Trichloroacetic on THE 6-09-1926-77

Savelev what I GOST 22180-76

Malonic on MRTU 6-09-397-77

Benzoic according to GOST 10521-78

Carrying out the claimed process of extraction of carbonyl compounds and / or acids of complex organic mixtures is as follows. Selected organic composition is subjected to analysis for the concentration of carbonyl compounds and acids. Based on the results of this analysis and, knowing the value of the optimal load in the working machine, is determined by calculation with respect to the allowable range of the ratios of the masses of the aqueous and organic phases and mass loading of these phases, the amount required for the interaction of sodium sulfite, the concentration of sodium sulfite in the aqueous phase and the mass of this reagent. At the same time counting the number requiring additional input acids, choose the latter and is determined by the concentration of this acid in aqueous solution.

After such a calculation are loaded into the reactor organic compositions and aqueous solution of sodium sulfite (or water and solid sodium sulfite), include mechanical mixing and achieve the state that the system was represented fairly evenly by volume of emulsion, and solid phase source of sodium sulfite completely disappeared. 1.5-10 minutes stirring in the specified mode control the pH of the aqueous phase and the residual content of acid in the organic phase. If the settlement is ednie tends to zero, start enter the calculated number of additional acid. The last exercise so that all input was completed within 40 min, and the last 10-15% would be entered in approximately 20-40% of the time. Make control measurements of pH during the process and after entering the estimated amount of additional acid. When you start working with an unknown organic composition in model conditions remove the whole curve changes the pH on the acid number of entered. This gives you the opportunity to compare the results of sampling from this curve.

Upon completion of the process of extraction of carbonyl compounds in organic and aqueous phases are separated, the organic phase is washed with distilled water, after separation which make analyses on the residual content of carbonyl compounds and acids. Usually they are close to zero. But there are also options when some of those present in the composition of carbonyl compounds and acids do not react with sodium sulfite in the selected conditions. These are moreaccessible connection, as acetophenone, C18or more carboxylic acids, etc.

The resulting organic and aqueous phases are processed in accordance with the objectives. Wash water can be used later for cooking is of astora sodium sulfite.

Example 1

The original organic composition is acidic oils with carbonyl compounds 4.4 g-EQ/kg acid and 2.9 g-EQ/kg

The estimated mass loading of organic composition 80 g, which contains 0,352 g-EQ carbonyl compounds and 0,232 g-EQ acids. The required amount of added acid 0.12 g-EQ. The calculated quantity of sodium sulfite and 0.37 moles; correlation with carbonyl compounds 1,051. The concentration of the aqueous solution of Na2SO325,9%, the amount of this solution of 180 g; the ratio of organic and aqueous phase 1:2,25.

In a reactor of the type autoclave made of stainless steel with a diameter of 80 mm and a height of 200 mm, equipped with a paddle stirrer with 1440 rpm and cover with the respective nozzles, load 80 g acid oils and 180 g of an aqueous solution of sodium sulfite. Include mechanical mixing and after 2.5 min start input 20 ml of 6 n HCl solution (0.12 mol HCl). Measurement of pH at the beginning of this entry showed the value 12,20. Program input HCl was as follows (number of introduced acid in ml/time from the beginning of the process): 5/4; 10/7; 15/10; 19/15; 20/25. Input hold from dispenser type burette through a special hole in the lid of the reactor without any stops stirring the reaction mass. During the process the temperature rose from 26 to 30°and the pH dropped to 6.5.

After completion of payment kolichestvennoi acid stop stirring, the reaction mass is poured into a sump-type separating funnel, the organic phase is separated, washed with distilled water, again separated and determine the residual content of carbonyl compounds and acids. In the aqueous phase control the final pH value. The residual content of acids and carbonyl compounds in separated after washing with distilled water the organic phase was less than 0.002 g-EQ/kg each.

Examples No. 2-13

The nature of the processed organic composition, the content of carbonyl compounds and acids, the concentration of the aqueous solution of sodium sulfite, mass loaded organic and aqueous phase and their ratio, the stoichiometric excess of sodium sulfite, the characteristics of the reactor and stirrer, and the sequence of operations similar to that described in example 1. Different nature additionally injected acid concentration of the aqueous solution and the volume entry software acid, the duration of the period until the input of the acid and of the whole process, the initial and final temperature. The results obtained are given in table. 1. Denote GOS-sodium hydrosulphate, MC, HOOK, THUC - acetic, Chloroacetic, and trichloroacetic acid, SK, MK, BK - oxalic acid, malonic acid and benzoic (*-solution in isopropyl alcohol) acid.

Table 1

td align="center"> 0,003
Load characteristics and processExample No.
2345678910111213
Nature additionally injected acidHClHClHBrGOSHNO3H2SO4MCHOOKTHUCSKMKBq*
The concentration of the aqueous solution, which introduces an additional acid, g-EQ/l11,003,003,258,003,7010,005,354,134,732,003,001,73
The amount of added acid, ml10,9140,0036,9215,0032,4312,0022,43depreciation is 29.0625,4060,0040,0069,40
The duration of the process prior to the commissioning of additional acid, min42321,5 1,5342433
Program input additional acid: the amount (ml)/time from the beginning of the process (min)4/6; 8/8; 10/11; 10,8/15; 10,91/1910/5; 20/8; 30/11; 38/15; 40/2610/6; 20/9; 30/13; 35/18; 36,92/245/5; 10/8; 14/15; 15/2010/4; 20/7; 30/11; 32,43/206/5; 11/11; 12/2110/7; 20/15;22,43258/8; 16/12; 25/20;depreciation is 29.063210/6; 20/10; 25/18;25,42820/8; 40/12; 58/20; 60/3015/6 30/9; 39/15; 40/2220/6; 40/9; 60/14; 65/20; 69,4/35
The temperature in the beginning of the process, °152217191620232419181716
The temperature at the end of the process, °182721221923262722212119
PH
- IOM is NT the beginning of the commissioning of additional acid 12,1012,2012,1012,1512,2312,1412,1812,1312,1112,1712,1812,20
- when finished entering additional acid6,63of 6.716,636,74of 6.686,756,52to 6.586,54of 6.71of 6.686,72
The process duration, min192624202021253228302235
The residual content in the composition (g-EQ/kg)
- carbonyl compounds0,0030,0030,0030,0040,0030,0050,0030,0040,0040,0030,0030,002
acids0,0030,0030,0030,0030,0030,0030,0020,0040,0040,0030,002

Examples No. 14-20

The nature of the processed organic composition, reactor, boot order, to treatment and control process similar to that described in example 1. Different values of the concentrations of carbonyl compounds and acids in different batches of acid oils, the ratio of the concentrations of carbonyl compounds and acids, an excess of sodium sulfite and its calculation, the concentration of an aqueous solution of sodium sulfite, nature and amount of additional acid, time, temperature and pH-metric characteristics. The results obtained are given in table. 2

Table 2
Load characteristics and processExample No.
14151617181920
Sour oil
[>C=O], g-EQ/kg0,600,601,05of 1.57of 1.57 2,112,84
[>C(O)HE], g-EQ/kg0,710,711,051,251,251,542,11
Load characteristics:
The mass of acidic oils in loading, g200200180150100120100
The amount of carbonyl compounds in loading, g-EQ0,1200,1200,1890,236of) 0.1570,2530,284
The amount of acid loading, g-EQ0,1420,1420,1890,1880,1250,1850,211
The amount of sodium sulfite, mol0,1420,1260,2040,2590,1730,2730,304
The amount of water, g82,184,198,6117,4178,2145,6of 161.7
The concentration of the aqueous solution of Na2SO3, %17,8915,88 21,4221,7610,8819,1119,15
The mass ratio of the aqueous and organic phases in the beginning of the process1:21:21:1,51:12:1the 1.5:12:1
The required amount of additional acid, g-EQ0,00,00,00,048to 0.0320,0680,073
Nature additionally injected acid---H2SO4HClH2SO4HCl
The concentration of the aqueous solution, which introduces an additional acid, g-EQ/l---2,31,84,5the 5.7
The amount of added acid, ml---20,917,815,212,91
The duration of the process prior to the commissioning of additional acid, min--3333

Continuation of table. 2
Load characteristics and processExample No.
14151617181920
Program input additional acid: the amount (ml)/time from the beginning of the process (min)---10/5;

20/7;

20,9< / br>
15
10/5;

17/9;

17,8< / br>
9
5/5;

10/7;

15/10;15,215
5/5;

10/7;

12/13;

12,91

22
The temperature in the beginning of the process, °15172130272214
The temperature at the end of the process, °15172130272214
PH
in the beginning of the commissioning of additional acid---12,0511,9812,0212,06
in the end of process6,956,4 6,74of 6.686,566,64of 6.71
The process duration, min54515191522
The residual content in the organic phase (g-EQ/kg)
- carbonyl compoundstracestraces˜0,001tracestracestracestraces
acidstraces˜0,08˜0,001tracestracestracestraces

Examples No. 21-26

The reactor, the boot order, the sequence of processing operations and control process similar to that described in example 1. Different nature of the organic composition, the qualitative and quantitative compositions of carbonyl compounds and acids in them, the concentration of an aqueous solution of sodium sulfite, an excess of this reagent and the approach to its calculation, the nature and concentration of the additional input of acid, time, temperature and pH-metric characteristics. Received financial p the tats are given in table. 3. Designation: UNDER - oil; OPM - oxidat sunflower oil with a viscosity of 77 seconds on the viscometer VZ-4 (20°); OK - 55%solution of oxidate sunflower oil white spirit with a viscosity 26-28 seconds by the viscometer VZ-4 (20°).

Table 3
Load characteristics and processExample No.
212223242526
The nature of the organic compositionUNDER1UNDER2OPMOK1OK2OK3
[>C=O], g-EQ/kg2,02,40,170,140,130,12
[>C(OH)IT], g-EQ/kg0,280,720,130,080,140,28
Load characteristics:
Weight organic compounds, g150120200250250250
The number of carbonyl joint is, g-EQ0,300in 0.2880,0340,035to 0.0320,030
The number of downloaded acid, g-EQ0,0420,0860,0260,0200,0350,070
The amount of sodium sulfite, mol0,3300,316being 0.0360,0380,0350,033
The amount of water, g118,4140,295,5for 95.295,695,8
The concentration of the aqueous solution of Na2SO3, %26,0022,184,544,79to 4.414,16
The mass ratio of the aqueous and organic phases in the beginning of the process1,07:1the 1.5:11:21:2,51:2,51:2,5
The required amount of additional acid, g-EQ0,2580,2020,0080,0150,0000,000
Nature additionally injected acidHClH2SO4HBrHBr--
The concentration of the aqueous solution, in the de which introduces an additional acid, g-EQ/l109,41,02,0--
The amount of added acid, ml25,8021,498,007,50--
The duration of the process prior to the commissioning of additional acid, min71054--
Program input additional acid: the amount (ml)/time from the beginning of the process (min)5/10; 10/13; 15/16; 25/25;25,8; 4010/15; 20/22;21,49;334/7; 7/11; 8/203/6; 6/8; 7/11;7,5;< / br>
18
The temperature in the beginning of the process, °201824192316
The temperature at the end of the process, °242126212317
PH
in the beginning of the commissioning of additional acid9,709,8311,5311,72--
in the end of process6,61to 6.576,61to 6.586,63to 6.58

Continuation of table. 3
Load characteristics and processExample No.
212223242526
The process duration, min40332018810
The residual content in the organic phase (g-EQ/kg)
- carbonyl compounds0,0010,005tracestracestracestraces
acidstraces0,006tracestracestraces˜0,15

The positive effect of the proposed solution consists in the following:

1. Using a single reagent (sodium sulfite) of complex organic composition can be removed and carbonyl compounds, acids, and present in the SByte functional group can be removed, and partly to leave. All this makes the proposed solution is more maneuverable.

2. The method is simple to perform, requires no special equipment, no need to supply external heat flows quickly and is pretty reliable.

3. With this method it is possible to delete not only almost all the aldehydes, but many are much less reactive in comparison with aldehydes ketones.

4. This method does not have any substantial restrictions on the content of carbonyl compounds in the original composition. It is effective in the case of large concentrations of carbonyl compounds, and are quite small.

5. At simultaneous presence in the organic composition of aldehydes and ketones with quite large differences in reactivity of the proposed solution allows for the possibility of fractionation remove carbonyl compounds and(or) carboxylic acids. To do this, a series of treatments with the Department of waste aqueous phase with dissolved hydrosulfite derivatives and salts of the acid and its replacement by a new portion of an aqueous solution of sodium sulfite.

1. The method of extraction of carbonyl and (or)acid compounds from complex multi-component organic liquid mixtures by treating them with an aqueous solution of the su is theta sodium intensity mechanical mixing, ensuring the formation of a uniform emulsion, characterized in that define the content of carbonyl compounds and acids in the original mixture, processing lead 4,16-26%aqueous solution of sodium sulfite from the calculation of 1.05-1.1 mol of sodium sulfite in 1 g-EQ carbonyl compounds, while exceeding in the original mixture of acids (g-EQ) over the content of carbonyl compounds 1 mol of sodium sulfite in 1 g-EQ of acid, and the mass ratio of the aqueous solution of sodium sulfite and organic compounds 1-2,5:2-1, at a temperature of 15-30°And, if the acid content in the initial mixture (g-EQ) less than the content of carbonyl compounds (g-EQ), while monitoring the change of the pH value of the aqueous phase enters the additional mineral or organic acid in a quantity equal to the difference of content of carbonyl compounds (g-EQ) and acids (g-EQ) in the initial download of the organic mixture to be processed, with such speed, that the pH of the aqueous phase is continuously decreased, but not below 6.5.

2. The method according to claim 1, characterized in that the input of additional acid start after 1.5-10 min, during which time almost completely consume all able to respond in these circumstances the acid.

3. The method according to claim 1, characterized in that the process without entering additional acid in the case when the holding acids (g-EQ) exceeds the content of carbonyl compounds (g-EQ), or equal to, spend within 4-10 minutes

4. The method according to claim 1, characterized in that the additional added acid using hydrochloric, Hydrobromic, nitric, sodium hydrosulphate, sulfuric, acetic, Chloroacetic, trichloroacetic, oxalic, malonic, benzoic.

5. The method according to claim 1, wherein the added acid is administered in the form of an aqueous or alcohol solution with a concentration 1-11 g-EQ/liter



 

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EFFECT: improved method for treatment.

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1 tbl, 4 ex

FIELD: chemical technology.

SUBSTANCE: invention relates to a method for removing higher organic iodides from organic media. Method for removing organic iodides containing 10-16 carbon atoms from non-aqueous organic media containing organic iodides with 10-16 carbon atoms is carried out by contacting indicated organic media with silver- or mercury-exchange cationic, ion-exchange substrate at temperature from 50°C to 150°C. Invention proposes a method for removing iodides having 10-16 carbon atoms from acetic acid or acetic anhydride by providing flow of acetic acid or acetic anhydride containing organic iodide having 10-16 carbon atoms. Indicated flow is contacted with macroporous strong acid ion-exchange resin wherein at least 1% of active sites acquire form of silver or mercury at temperature in the range 50°C - 150°C. Indicated silver- or mercury-exchange ion-exchange resin removes effectively at least 90 wt.-% of indicated organic iodides from indicated flow of ready acetic acid or acetic anhydride. Also, invention proposes a method for removing organic iodides containing 10-16 carbon atoms from acetic acid or acetic anhydride involving contact of acetic acid or acetic anhydride comprising dodecyl iodide with silver- or mercury-exchange cationic ion-exchange substrate at temperature in the range 50°C - 150°C. Method provides the complete removing higher organic iodides from flow of acetic acid and/or acetic anhydride.

EFFECT: improved method for removing.

29 cl, 5 dwg, 13 ex

The invention relates to an improved method of allocation of ketones and/or acids from hydrocarbon mixtures such as crude oils, petroleum products, dispersed organic matter of rocks, etc
The invention relates to a new process for the preparation of fluorinated acids emulsifiers of waste water for the purpose of regeneration, namely, that first from waste water of polymerization of fluorinated monomers remove interfering components selected from finely dispersed solids and transferred to the solid component, and then connect the fluorinated acid emulsifiers on anion exchange resin and elute from it these fluorinated acid emulsifiers

The invention relates to an improved method for producing crystals of adipic acid used in the production of polymers, for example, to obtain a polyamide or polyurethanes
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