SU1216176A1 - Method of treating glycerine water - Google Patents

Description

This invention relates to an improved process for treating glycerin water resulting from the thermal hydrolysis of dietary fats. The result is a technical glycerin used widely in organic synthesis and a fatty acid concentrate used to make soap.

The aim of the invention is to simplify the process technology, reducing the loss of glycerol and fatty acids.

Example 1. Glycerol water from a brewery obtained by hydrolysis of edible fats in the presence of water at 210-225 C, containing 140 g / l glycerol and 50 g / l fatty acids and having a temperature of 80 ° C, is passed through an ESW separator with a capacity 1,400 kg / h You get fatty acids (66 kg / h) and partially defatted glycerin water (1334 kg / h which contains 3 more g / l of fatty acids, and has a pH of 4.5. This glycerin water is pumped under a pressure of 0.3-0, 4 MPa circulate through a section of serially connected tubular ultrafilters with cellulose acetate, fluoroplast and polysulfonamide membranes at 48 ° C and speed

flow of liquid over the membrane 4.4 m / s. At the same time, part of the glycerin water passes through the membrane, and the suspension of fatty acids is retained by it and concentrated to 60 g / l (concentration by volume 20 times (6 wt.% The resulting filtrate (purified from fatty acids glycerin water) in the amount of 90 for ultrafilters with cellulose acetate membrane, 107 for ultrafilters with polysulfone. The membrane membrane and 91 l / m.h for ultrafilters with fluoroplastic membranes does not contain fatty acids, has an ash content of 0.034% and is sent to dehydration by evaporation and to obtain technical glycerol. Fatty acid concentrate in glycerol water obtained from ultrafiltration (5% by volume of the initial glycerol water supplied to the ultrafiltration is mixed with the original glycerol water after hydrolysis of the fats and sent for separation to separate the fatty acids used for making soap or other purposes.

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Example 2. Cleaning method; glycerin water as described in

Example 1, but glycerol water after hydrolysis of fats containing 100 g / l glycerol and 30 g / l fatty acids, and after separation 110 g / l glycerol and 2 g / l fatty acids by pump under pressure 0.3-0.4 MPa circulating through ultrasonic filter sections with cellulose acetate membranes at a speed of 5 m / s. In this case, the filtration performance of the ultrafilters is 90 l / m.h. The filtrate does not contain fatty acids and

15 has an ash content of 0.034%. The concentrate obtained from ultrafiltration contained 31 g / l of fatty acids (3.1% by weight). Its volume is 3.9% of the volume of the original glycerol I

20 water supplied to the ultrafilter. This fatty acid concentrate is mixed with the starting glycerol g with water after hydrolysis of the fats and sent for separation to separate the 25 fatty acids. After separation of this glycerin mixture, water contains 110 g / l of glycerin, 2 g / l of fatty acids, .0.034% ash.

Example 3. Cleaning Method

30 glycerin water as described in

Example 1, but glycerin water after separation, containing 4.6 g / l of fatty acids and 140 g / l of glycerin, is pumped under a pressure of 0.3-0.4 MPa through a section of ultrafilters with polysulfonamide membranes at a speed of 5 m / with. In this case, the filtration performance of the ultrafilters is 107 l / m. The filtrate does not contain fatty acids and has an ash content of 0.034%. The concentrate obtained from ultrafiltration contains 60 g / l of fatty acids (6% by weight). Its volume is 7.2% of the volume of the original glycerin water supplied to the ultrafiltration. This fatty acid concentrate is mixed with the original glycerol water after hydrolysis of the fats and sent for separation to separate the fatty acids.

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Example 4. The method of purification of glycerin water, as described in example 1, but after the separation, glycerin water containing 4.6 g / fatty acids and 140 g / l glycerin is circulated through a pump under pressure of 0.3-0.4 MPa ultrafilter sections with fluoroplastic membranes at a speed of 5 m / s. At the same time, the filtration capacity of the ultrafilters is 91 l / m-h. The filtrate does not contain fatty acids and has an ash content of 0.034%. The concentration obtained from ultrafiltration contains 100 g / l of fatty acids (10% by weight). Its volume is 4.6% of the volume of the true glycerol water fed to the ultrafiltration This fatty acid concentrate is mixed with the original glycerol water after hydrolysis of the fats and sent to the separation process. Example 1, but glycerin water was obtained as a result of the thermal hydrolysis of technical fats produced in glue, processing oils, gelatin, leather, and recycling plants and other plants. It contains 96 g / l glycerol, 30 g / l fatty acids and has an ash content of 1.70%. After separation, this water containing 100 t / l of glycerin, 3 g / l of fatty acids and 1.70% of ash is pumped under a pressure of 0.3-0.4 MPa and circulated through an ultrafilter section with fluoroplastic membranes at a speed of 5 m / s. In this case, the filtration capacity of the ultrafilters is 66 l / m. h. The filtrate does not contain fatty acids, has an ash content of 1.60%. The concentrate obtained by ultrafiltration of the mouth contains 60 t / l of fatty acids. Its volume is 5% of the volume of the original glycerin water supplied to the ultrafiltration / s. This fatty acid concentrate: A lot is mixed with the original glycerol water after hydrolysis and sent for separation to separate the fatty acids. After separation of this mixture of glycerin, the warmer contains 3 g / l of fatty acids, 100 g / l of glycerin and 1.65% ash.

After ultrafiltration, fatty acid concentrates are fed to trim the separator only if the existing capacity cannot cope simultaneously with the original glycerol water and the concentrate formed by ultrafiltration (Example 6).

PRI me R 6. The method of processing glycerin water, as described in

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Example 1, but a concentrate from ultrafiltration, containing 60 g / l of fatty acids, is not mixed with the original glycerol water from hydrolysis of life

5, and sent to a separate separator to separate the fatty acids. The fatty acids thus obtained are mixed with the fatty acids obtained from the separator for the original

10 glycerin water, or used separately for its intended purpose, and the resulting glycerin water containing 2.7 g / l-fatty acids and having an ash content of 0.029% is mixed

15 with glycerol water after separation of the starting glycerin water after hydrolysis of the fats and directed to ultrafiltration.

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Example 7. The original glycerol water, crawling as a result of hydrolysis of edible fats and the presence of water at 225 ° G, containing 140 g / l glycerol and 50 g / l fatty acids and having a temperature,

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passed through an ESW separator. In this case, fatty acids and glycerol water are obtained, containing 4.6 g / l of fatty acids and having a pH of 4.5. This glycerol water is circulated by pump under a pressure of 0.38 MPa through a section of tubular ultrafilters having semi-permeable membranes with a pore size of 45 nm at a flow rate of glycerol water above

35 membranes 5 m / s. At the same time, glycerin water passes through, and suspension of fatty acids and other substances (osmol and other substances in glyceric water after hydrolysis)

40 is concentrated to 3.0% by weight. By y- The treated filtrate (purified from glycerol water suspended in water, degree of purification from fatty acids is 100%) with an ash yield of 92 l / m h

45 0.035% and sent for dehydration by evaporation to obtain technical glycerol. The resulting concentrate. Fatty acids 30 g / l is mixed with the original glycerin

0 with water and served for separation. Obtained by separating the mixture of the initial glycerin water and the concentrate, glycerin water contains 0.44 g / l of fatty acids, it is directed to ultrafiltration. As a result, the separation of the acid is used to prepare juices or for other purposes.

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When the fatty acids are concentrated by ultrafiltration to less than 3%, it becomes necessary to return large amounts of concentrate to the separation (more than 20% by weight of glycerin water, for ultrafiltration), which is not economically feasible.

Example 8. The method of purification of glycerol water, as described in example 7, but the concentration of fatty acids by ultrafiltration lead to 20 wt.%. The degree of purification of glycerol water from fatty acids by ultrafiltration is 100%, the ash content is 0.034%. The specific yield of filtrate is 97 l / m2. h

Example -9. The method of purification of glycerin water, as described in example 7, but the concentration of fatty acids during ultrafiltration is 1 to 6.0% (60 g / pT) The degree of purification of glycerin water from fatty acids is 100%, ash content is 0.035%. Specific filtrate yield is 90 h Returning the fatty acid concentrate to separation in the order of 7% by weight of glycerin water fed to ultrafiltration.

Example 10. The method of purification of glycerol water, as described in example 7, but the concentration of fatty acids by ultrafiltration lead to 20%. The degree of purification of glycerol water from fatty acids is 99.9%, the ash content is 0.035%, the specific yield of the filtrate drops to 20 l / m. h. Return of the fatty acid concentrate to separation in the order of 2.5%.

Example 11. The method of purification of glycerol water, as described in example 7, but the concentration of fatty acids by ultrafiltration lead to 25 wt.%. Glycerin water from

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fatty acids are not cleared, ash content is 0.041%. The specific yield of the filtrate is reduced to 2. The degree of purification of glycerol water and the low yield of the filtrate make it unacceptable for the practical use of ultrafiltration of fatty acids above 20% by weight.

Example 12 (comparative). Glycerin water obtained as a result of technical hydrolysis of edible or technical fats and separation, as in Example 1, is periodically poured into one or another neutralizer. Then, lime milk at the rate of 3.2 kg per 1 m of glycerin water is added to the neutralizer to the glycerin water. The neutralizer content is heated to 80 ° C and stirred for 1.5 hours. Calcium soaps that float to the surface and foam are collected. The neutralizer content is pumped at a pressure of 0.26 MPa to a frame type filter press for filtering. The resulting filtrate 125 does not contain fatty acids, but has an elevated ash content (by 5–30% compared to the ash content of the filtrate from ultrafiltration, depending on the quality of the starting material). After three days, the filter material was manually disassembled and cleaned from the sludge, which was sent to the dump. The loss of glycerol during the said treatment is 1.5-1.6%. In the process there are a lot of manual operations, t hard working conditions at extreme temperatures and stench.

Comparative results for the proposed and known method are given in the table.

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As can be seen from the table, the use of glycerol contamination of ash inoculation of the proposed method is ensured. The process is carried out to completely remove fatty acids from the glycerin high productivity of ultrasound and their utilization of filtrate filters (60-120 prevents loss and additional s l / m-h).

Claims (3)

1. METHOD FOR PROCESSING GLYCERINE WATER, including purification of it from fatty acids by separation and dehydration, characterized in that, in order to simplify * the process technology, reduce losses of glycerin and fatty acids, glycerin water after separation is separated by ultrafiltration into a fatty acid concentrate with mass fraction of the last 3-20%, directed to separation, and glycerin water, which is subjected to dehydration. 2. The method of pop. ^ characterized in that the mass fraction of fatty acids in the concentrate is 5-10%. 3. The method according to p. ^ Characterized in that the fatty acid concentrate is mixed with the source glycerin water supplied for separation. SH5Sh 76 ³ Example 2. The method of purification of glycerin water, as described in example 1, but glycerin water after hydrolysis of fats, containing 100 g / l of glycerol and 30 g / l of fatty acids, and after separation of 110 g / l of glycerol and 2 g / l of fatty acids pump under pressure of 0.3-0.4 MPa circulate through sections of ultrafilters ^ with cellulose acetate membranes at a speed of 5 m / s. Moreover, the performance of ultrafilters by filtrate is 90 l / m ² .h. The filtrate does not contain fatty acids and has an ash content of 0.034%. The concentrate obtained from ultrafiltration contains 31 g / l of fatty acids (3.1 wt.%). Its volume is 3.9% of the volume of the initial glycerin ί 20 water supplied to ultrafiltration. This fatty acid concentrate is mixed with the starting glycerin _; water after hydrolysis of fats and sent for separation to separate 25 fatty acids. After separation of this mixture, glyceric water contains 110 g / l of glycerol, 2 g / l of fatty acids .034% ash. Example 3. The method of purification of 30 glyceric water, as described in example 1, but glycerin water after separation, containing 4.6 g / l of fatty acids and 140 g / l of glycerol, is circulated by a pump under a pressure of 0.3-0.4 MPa through a section of ultrafilters with polysulfonamide membranes * at a speed of 5 m / s. . Moreover, the performance of ultrafilters by filtrate is 107 l / m ² / 40 The filtrate does not contain fatty acids and has an ash content of 0.034%. The concentrate obtained from ultrafiltration contains 60 g / l of fatty acids (6 wt.%). Its volume is 7.2% of the volume of the initial glycerin water supplied to ultrafiltration. This fatty acid concentrate is mixed with the source glycerin water after hydrolysis of the fats and sent to ₅₀ separation to separate the fatty acids. Example 4. The method of purification of glycerin water, as described in example 1, but glycerin water after separation, containing 4.6 r / ii of fatty acids and 140 g / l of glycerol, by a pump under a pressure of 0.3-0.4 MPa < circulate through sections ultra12161