Method of recycling monochloroacetic acid production wastes (versions)

FIELD: chemistry.

SUBSTANCE: invention relates to chemical engineering and specifically to methods of recycling monochloroacetic acid production wastes, used in production of carboxymethyl cellulose, pharmaceutical preparations, pesticides and ethylene diamine tetraacetic acid. Methods of recycling monochloroacetic acid production wastes involve treating the mother solution obtained from purifying monochloroacetic acid, wherein treatment is carried out by neutralising the mother solution with 30-44% aqueous sodium hydroxide solution at temperature 40-45°C until achieving pH 7-7.5, followed by reaction of the reaction mixture with 25% aqueous ammonia solution in molar ratio of monochloroacetic acid to ammonia equal to 1:1.39-1.46 until achieving pH 8.5-9, with step-wise increase in temperature, first to 50-70°C for 2-3 hours, maintaining pH of the mixture by adding 30% aqueous sodium hydroxide solution, and then to 80-105°C for 1-2 hours, followed by cooling and, if necessary, followed by neutralisation of the reaction mixture with hydrochloric acid at temperature 15-60°C for 0.5-2 hours until pH of the mixture equals 1.

EFFECT: recycling monochloroacetic acid production wastes using a simple, non-waste method to obtain a commercial-grade, mixed reagent for preventing deposits of inorganic salts during oil and gas extraction.

2 cl, 2 tbl, 12 ex

 

The invention relates to chemical technology, and in particular to methods of recycling waste production monochloracetic acid (MHUC), used in the manufacture of carboxymethyl cellulose, pharmaceutical drugs, pesticides, ethylenediaminetetraacetic acid.

Monochloracetic acid, obtained by the chlorination of acetic acid (CA) in the presence of catalysts (acetylchloride, acetic anhydride), contains as impurities convertible acetic acid and the products deeper chlorination (up to 6% of dichloracetic acid (DHOC) and a bit of trichloroacetic).

The removal of impurities can be performed by two main methods: crystallization and hydrogenation. Hydrogenation is a very complex and costly process and is not implemented in our industry.

The allocation method commodity monochloracetic acid crystallization is implemented in an industrial environment [Oshin L.A. Industrial organochlorine products. The Handbook. M.: Chemistry, 1978].

In some industries currently crystallization raw MJUK carried out in the bulk reactor jacketed for cooling. The heat removed by the water flow and the concentration of solid phase in suspension regulate the mixing of the reaction mass obtained after chlorination of acetic acid from mother liquor from stage filter is AI. The temperature of the suspension gradually lowered from 70°C to 20°C. At the stage of allocation of commodity monochloracetic acid at OJSC Khimprom Volgograd when the production at full capacity is formed 625 tons/year unusable mother liquor containing up to 35% MHUC, up to 45% DHUK, 20-25% acetic acid and the rest water. Given such significant amounts of unusable waste production MHUC, it becomes clear environmental and economic relevance of the stages of processing them into marketable products.

Also known is a method of processing waste production MJUK containing dichloracetic acid to obtain methyl ester monochloracetic acid [RF patent 2098404 From 07S52, publ. 10.12.97].

The disadvantage of this method is a multistage process with the use of sophisticated technological equipment and the presence of waste in the form of water, washing soda solution and distillation of the process of rectification.

The closest to the invention is a method of recycling the mother liquor from the separation of MJUK containing 38.2% of MHWC and 47.9% DHUK obtaining glycolic acid. The process is carried out by acid hydrolysis mother liquor when cleaning MJUK.

The disadvantage of this method is also a multi-stage process, the use of sophisticated technological equipment, as well as the presence of pfps is niteljnykh waste from the distillation of acetic acid, organic solvent, sodium chloride. [Application Germany 2810906 From 07 S06, From 07 s16, publ. 27.09.79.]

The technical result of the present invention is the utilization of waste production MJUK simple waste-free way of obtaining on the basis of the commodity mixed reagent to prevent deposits of inorganic salts in the extraction of oil and gas.

The technical result according to the first variante is achieved by neutralizing the mother liquor 30-44%aqueous solution of sodium hydroxide at a temperature of 40-45°C until reaching a pH of 7-7,5 with subsequent interaction of the reaction mixture with 25%aqueous ammonia solution in a molar ratio of monochloracetic acid, ammonia 1:1,39-1,46 until reaching pH 8.5-9 with a stepwise increase in the temperature at 50-70°C for 2-3 hours, maintaining the pH of the mixture by the addition of 30% aqueous solution of sodium hydroxide, then at 80-105°C for 1-2 hours and then cooled and receiving reagent to prevent deposits of inorganic salts in the extraction of oil and gas.

The technical result according to the second variant is achieved by neutralizing the mother liquor 30-44%aqueous solution of sodium hydroxide at a temperature of 40-45°C until reaching a pH of 7-7,5 with subsequent interaction of the reaction mixture with 25%aqueous ammonia solution in Molino the ratio of monochloracetic acid, ammonia 1:1,39-1,46 until reaching pH 8.5-9 with a stepwise increase in the temperature at 50-70°C for 2-3 hours, maintaining the pH of the mixture by the addition of 30% aqueous solution of sodium hydroxide, then at 80-105°C for 1-2 hours, followed by cooling and neutralizing the reaction mixture with hydrochloric acid at a temperature of 15-60°C for 0.5-2 hours to achieve a pH of the mixture 1 and receiving the reagent to prevent deposits of inorganic salts in the extraction of oil and gas. So get a highly effective reagent that can be used to prevent sedimentation of salts in the extraction of oil and gas from wells containing the first option such valuable components, as sodium salt, nitrilotriacetic, acetic, glycolic and oxalic acids, and ammonium chlorides and sodium, and the second option themselves of the acids listed above.

The formation of the sodium salt of nitrilotriacetic acid (NTUC) and ammonium chloride is as follows:

To obtain nitrilotriethanol the reaction mixture after amination neutralized with hydrochloric acid:

DHUK contained in the waste, in the process of synthesis is subjected to a dehydrochlorination with the formation of salts glyoxalases, and then glycolic and oxalic KIS is from:

For obtaining of the acid reaction mixture after amination neutralized with hydrochloric acid.

These components are effective functional additives for inhibiting scale compositions by acid treatment of oil wells. [Ibragimov GS, Sorokin V.A., Khisamutdinov NI Chemical reagents for oil: the working Directory. - M.: Nedra, 1986, P. 150, 168.]

Example 1. In chetyrehpolnye glass reactor equipped with a stirrer, thermometer, dropping funnel and reflux condenser, load 100 g of mother liquor production MJUK containing, % mass: 32 MHUC, 33 DHUK, 20 acetic acid and 15 of the water. The contents of the reactor to neutralize 44%aqueous solution of sodium hydroxide to achieve a pH of 7-7,5. The neutralization process is carried out at a temperature of 40-45°C. Then the reaction mixture from a dropping funnel dosed ammonia water (25% aqueous ammonia solution) in a molar ratio MJUK:NH31:1,39. The reaction mixture is heated to 60°C and maintained at these conditions for 2-3 hours, maintaining the pH of the mixture to 8.5÷9 by the addition of 44%aqueous solution of sodium hydroxide. Then the reaction mass is heated to 90°C and kept at this temperature for 2 hours. At the end of the reaction process with the offer cool and get 260,8 g of the required reagent, containing, % mass: 11,1 sodium salt of nitrilotriacetic acid, 4,8 glycolate, sodium, 6.6 sodium oxalate, 6,9 ammonium chloride and 11,46 sodium chloride, 10,48 sodium acetate.

Example 2. Conducting experience, as described in example 1, using 100 g of the mother liquor production MJUK with composition, % mass: 35 MHUC, 32 DHUK, 24 of acetic acid and 9 water. Get 269,95 g of reagent containing, % mass: 11,8 sodium salt of nitrilotriacetic acid, 4,5 glycolate, sodium, 6.1 sodium oxalate, 7,3 ammonium chloride and 10.7 sodium chloride, 12.1 sodium acetate.

Example 3. Conducting experience, as described in example 1, using 100 g of the mother liquor production MJUK with composition, % mass: 25 MHUC, 44,5 DHUK, 25 acetic acid and 5.5 water. Get to 274.9 g of reagent containing, % mass: 8,2 sodium salt of nitrilotriacetic acid, 6.15 glycolate, sodium, 8.4 sodium oxalate, 5,1 ammonium chloride and 14,65 sodium chloride, 12.4 sodium acetate.

Example 4. Conducting experience, as described in example 1, using 100 g of the mother liquor production MJUK with composition, % mass: 31,5 MHUC, 43,8 DHUK, 20 acetic acid and 4.7 water. Get 285,1 g of reagent containing, % mass: 10 sodium salt of nitrilotriacetic acid, of 5.83 glycolate, sodium, of 7.96 oxalate sodium, 6,25 ammonium chloride and 13.9 sodium chloride, 9.6 sodium acetate.

Example 5. Conducting experience, as described Primera 3, dosing ammonia water (25% aqueous ammonia solution) in a molar ratio MJUK:NH31:1,46. Get 277,66 g of reagent containing, % mass: 8,16 sodium salt of nitrilotriacetic acid, 6.09 glycolate, sodium, 8,32 oxalate sodium, 5,1 ammonium chloride and 14.5 NaCl, 12.3 sodium acetate.

Example 6. Conducting experience, as described in example 4, dosing ammonia water (25% aqueous ammonia solution) in a molar ratio MJUK:NH31:1,46. Get 287 g of reagent containing, % mass: 9,94 sodium salt of nitrilotriacetic acid, 5,8 glycolate, sodium, 7.9 sodium oxalate, 6,2 ammonium chloride and 13.8 sodium chloride, 9.5 sodium acetate.

Example 7. Conducting experience, as described in example 1, using 100 g of the mother liquor production MJUK with composition, % mass: 48 MHUC, 32 DHUK, 12 of acetic acid and 8 of water. At the end of the dosing ammonia reaction mass is heated to 50°C and maintained at these conditions for 3 hours. Then the reaction mass is heated to 80°C and kept at this temperature for 2 hours. Get 303 g of reagent containing, % mass: 14,3 sodium salt of nitrilotriacetic acid, 4.1 glycolate, sodium, 5,48 oxalate sodium 8,96 ammonium chloride and 9.58 sodium chloride, 8.6 sodium acetate.

Example 8. Conducting experience, as described in example 7. At the end of the dosing AMM is achnai water, the reaction mass is heated to 70°C and maintained at these conditions for 2 hours. Then the reaction mass is heated to 105°C and kept at this temperature for 1 hour. Get 285 g of reagent containing, % mass: 13,8 sodium salt of nitrilotriacetic acid, 5,9 glycolate, sodium, 5.8 sodium oxalate, 8,6 ammonium chloride and 10 sodium chloride, 8.6 sodium acetate.

Example 9. Conducting experience, as described in example 3, using for neutralizing the mother liquor production MJUK 30%aqueous solution of sodium hydroxide. Get 375 g of reagent containing, % mass: 6,04 sodium salt of nitrilotriacetic acid, 4,5 glycolate, sodium, 6.16 sodium oxalate, 3,8 ammonium chloride and 10.7 sodium chloride, 9.2 sodium acetate.

Example 10. Conducting experience, as described in example 1. To obtain the acid form to the resulting solution was added hydrochloric acid at a temperature of 40-60°C for 1-2 hours to achieve a pH of reagent 1. Get 403,43 g of reagent containing, % mass: 5,34 nitrilotriacetic acid, 2,4 glycolic acid, 2,8 oxalic acid, 4, 48 of ammonium chloride and 22,7 sodium chloride, 4,9 acetic acid.

Example 11. Conducting experience, as described in example 4. To obtain the acid form to the resulting solution was added hydrochloric acid at a temperature of 15-20°C for 0.5-1 hour to achieve a pH of reagent 1. Get 443,65 g of reagent containing, % mass: 4,77 nitrilotriacetic acid, 2.9 picolinate, 3,4 oxalic acid, 4 ammonium chloride and 24.4 sodium chloride, acetic acid 4,5.

Example 12. Conducting experience, as described in example 5. To obtain the acid form to the resulting solution was added hydrochloric acid at a temperature of 20-40°C for 1 hour to achieve a pH of reagent 1. Get 441,6 g of reagent containing, % mass: 3,81 nitrilotriacetic acid, 3 glycolic acid, 3,5 oxalic acid, 3,4 ammonium chloride and 25 sodium chloride, 5,7 acetic acid.

The resulting reagent for treatment of the well is stable during transportation and storage. He mixes well with formation water or hydrochloric acid for acid treatment of wells in any ratio that provides effective prevention of salt formation due to the complex influence of several active substances included in the composition. The procedures are the best way to allow the reagent required quality. In table 1 the data of the conducted experiments. At the treatment of wells with the use of the reagents are prepared as follows:

In capacity for the preparation of the sequentially loaded in % mass: 14-16, we offer reagents, 69-74 water, 12-15 hydrochloric acid - waste production of organofluorine (freon 21 and 22), the content of hydrogen chloride in which the extending t is up to 15-30% of the mass, and hydrogen fluoride up to 4-6% of the mass. The mixture is stirred for 30 minutes to obtain a uniform solution.

Table No. 2
The results of testing the effectiveness of inhibition of hydrates composition containing the proposed inhibiting reagents.
No. n Component content, % massThe efficiency of inhibition
Hydrochloric acid fluoride organic productionsAminirovanie mother liquor production MJUKWaterscaling, %
12345
The proposed composition
11514rest99,3
2 1516rest100
31216rest99,7
Compositions without inhibiting additives
4150rest23
5120rest22,8

Thus, compared to known methods, the proposed method of disposal of waste production MJUK allows you to:

by simple technological design synthesis, without the formation of additional waste, using cheap and readily available raw materials to produce a product that is used as the inhibiting additives in oil production;

to reduce the environmental burden on the environment through efficient use of current waste production, containing valuable components, functionally acting on the formation rock and protecting Neftepolis the new equipment from scaling;

to reduce the cost of production of the reagent to prevent scaling due to the replacement of expensive and scarce components of the current waste production;

to improve technical and economic performance of primary production MJUK.

1. The method of disposal of waste production monochloracetic acid, including the processing of the mother liquor obtained during the purification of monochloracetic acid, wherein the treatment is carried out by neutralizing the mother liquor 30-44%aqueous solution of sodium hydroxide at a temperature of 40-45°C until reaching a pH of 7-7,5 with subsequent interaction of the reaction mixture with 25%aqueous ammonia solution in a molar ratio of monochloracetic acid: ammonia 1:1,39-1,46 until reaching pH 8.5-9 with a stepwise increase in the temperature at 50-70°C for 2-3 h, while maintaining the pH of the mixture by adding 30% an aqueous solution of sodium hydroxide, then at 80-105°C for 1-2 h and then cooled and receiving the reagent to prevent deposits of inorganic salts in the extraction of oil and gas.

2. The method of disposal of waste production monochloracetic acid, including the processing of the mother liquor obtained during the purification of monochloracetic acid, wherein the treatment is carried out by neutralizing the mother liquor 30-44 th aqueous solution of sodium hydroxide at a temperature of 40-45°C until reaching a pH of 7-7,5 with subsequent interaction of the reaction mixture with 25%aqueous ammonia solution in a molar ratio of monochloracetic acid: ammonia 1:1,39-1,46 until reaching pH 8.5-9 with a stepwise increase in the temperature at 50-70°C for 2-3 h, while maintaining the pH of the mixture by the addition of 30%aqueous sodium hydroxide solution, then at 80-105°C for 1-2 h with subsequent cooling and neutralizing the reaction mixture with hydrochloric acid at a temperature of 15-60°C for 0.5-2 h until the pH of the mixture 1 and receiving the reagent to prevent deposits of inorganic salts in the extraction of oil and gas.



 

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The invention relates to the production of trichloroacetic acid (THUK), which is obtained by the oxidation of mixtures hlorosoderzhashie

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