CN220405585U - Chloroacetic acid heavy component recycling device - Google Patents

Chloroacetic acid heavy component recycling device Download PDF

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Publication number
CN220405585U
CN220405585U CN202321807929.6U CN202321807929U CN220405585U CN 220405585 U CN220405585 U CN 220405585U CN 202321807929 U CN202321807929 U CN 202321807929U CN 220405585 U CN220405585 U CN 220405585U
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heavy component
reaction kettle
chloroacetic acid
jacket
cooling water
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罗汉金
周仕鹏
王凤凤
张猛
孙顺平
张佳宇
周晓倩
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Shandong Minji New Material Technology Co ltd
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Shandong Minji New Material Technology Co ltd
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Abstract

The utility model belongs to the technical field of chemical raw material production, and particularly relates to a chloroacetic acid heavy component recycling device which comprises a heavy component buffer tank, a chlorination reaction kettle, a hydrolysis reaction kettle and a crystallization kettle which are sequentially connected with a centrifuge, wherein the chlorination reaction kettle is connected with a condenser, and the hydrolysis reaction kettle is connected with an alkali liquor overhead tank. The utility model has the advantages of convenient operation and simple structure, reduces the treatment cost of heavy components and improves the economic and environmental benefits.

Description

Chloroacetic acid heavy component recycling device
Technical Field
The utility model belongs to the technical field of chemical raw material production, and particularly relates to a chloroacetic acid heavy component recycling device.
Background
Chloroacetic acid is an important chemical raw material, is mainly used for producing glycine, carboxymethyl cellulose and the like, and is also widely applied to the fields of medicine, papermaking, dye, plastic processing, pesticide and the like. The chloroacetic acid production process is divided into a batch process and a continuous process, the batch process is eliminated, and a safe and environment-friendly continuous process is mainly adopted at present. The continuous production process uses acetic acid liquid chlorine as raw material, and the product is obtained after reaction and rectification treatment.
The heavy component removed in the rectification refining process is a poisonous and corrosive liquid, the heavy component is mixed into a waste water area for treatment in industry, alkali liquor is used for neutralizing waste liquid to be nearly neutral, then water is added for dilution, so that the concentration of the solution is reduced and then the solution is sent into biochemical waste water for treatment; there are also attempts to incinerate heavy components, but the original components are highly corrosive and contain chlorine, so that the chlorine incineration process is converted into HCl, the high corrosiveness makes severe demands on an incineration system, and in addition, the incineration tail gas has complex components and needs further harmless treatment.
Along with the expansion of chloroacetic acid productivity, a safe and environment-friendly heavy component treatment device needs to be developed, so that the treatment cost of the heavy component is reduced.
Chinese patent CN 217287203U discloses a mother liquor recycling device for chloroacetic acid production, including distillation tank, crystallization tank one, crystallization tank two, collecting box, be equipped with the mother liquor feed liquor pipe on the lateral wall of distillation tank, the top of distillation tank is equipped with outlet duct one, outlet duct one runs through condensing equipment and is connected with the collecting box, the bottom of distillation tank is equipped with drain pipe one, drain pipe one is connected with the pump body one, the pump body one is connected with crystallization tank one through feed liquor pipe two, the inside of crystallization tank one is equipped with the crystal collection box, the drainage hole has all been seted up to the lateral wall and the bottom of crystal collection box, the bottom of crystallization tank one is equipped with drain pipe two, drain pipe two passes through the pump body two and is connected with crystallization tank two, the inside of crystallization tank two is equipped with the crystal collection box. Because the chloroacetic acid has complex heavy components, the hydrolysis products of the chloroacetic acid are sodium glycolate, sodium oxalate and the like when the chloroacetic acid is directly added with alkali liquor for hydrolysis, and the sodium glycolate is dissolved in the solution in the patent, and is difficult to separate in the final product. If the sodium glycolate needs to be recovered, the sodium glycolate is difficult to separate from other impurities, because the sodium glycolate has high solubility in water, and the sodium glycolate is easy to react and denature when heated and evaporated, and the process is more complicated if other measures such as extraction are adopted.
Disclosure of Invention
According to the defects in the prior art, the technical problems to be solved by the utility model are as follows: the chloroacetic acid heavy component recycling device is convenient to operate, simple in structure and capable of fully recycling chloroacetic acid heavy components.
The technical scheme adopted for solving the technical problems is as follows:
the utility model relates to a chloroacetic acid heavy component recycling device which comprises a heavy component buffer tank, a chlorination reaction kettle, a hydrolysis reaction kettle and a crystallization kettle which are sequentially connected with a centrifuge, wherein the chlorination reaction kettle is connected with a condenser, and the hydrolysis reaction kettle is connected with an alkali liquor high-level tank.
The heavy component buffer tank top be provided with heavy component feed line, the inside first agitator that is provided with of heavy component buffer tank, the cladding of heavy component buffer tank outside has first clamp cover, first clamp cover links to each other with air inlet pipeline, play liquid pipeline respectively.
And a heavy component pump is arranged between the heavy component buffer tank and the chlorination reaction kettle.
The top of the chlorination reaction kettle is provided with a chlorine feeding pipeline, a second stirrer is arranged in the chlorination reaction kettle, a second jacket is coated on the outer side of the chlorination reaction kettle, and the second jacket is respectively connected with the first cooling water inlet pipeline and the first cooling water outlet pipeline.
A chloride pump is arranged between the chlorination reaction kettle and the hydrolysis reaction kettle.
The hydrolysis reaction kettle is internally provided with a third stirrer, the outside of the hydrolysis reaction kettle is coated with a third jacket, the third jacket is respectively connected with a second cooling water inlet pipeline and a second cooling water outlet pipeline, and a hydrolysis liquid pump is arranged between the hydrolysis reaction kettle and the crystallization kettle.
The crystallization kettle is internally provided with a fourth stirrer, the outer side of the crystallization kettle is coated with a fourth jacket, the fourth jacket is respectively connected with a third cooling water inlet pipeline and a third cooling water outlet pipeline, and a slurry pump is arranged between the crystallization kettle and the centrifugal machine.
The top of the centrifugal machine is provided with a washing water inlet pipeline.
The condenser is respectively connected with the fourth cooling water inlet pipeline and the fourth cooling water outlet pipeline.
The top of the alkali liquor high-level tank is provided with an alkali liquor feeding pipeline.
Working principle and process:
the utility model is to obtain sodium oxalate product by chloridizing, hydrolyzing, crystallizing and separating chloroacetic acid heavy component.
The chloroacetic acid heavy component contains monochloroacetic acid, dichloroacetic acid, acetic acid and the like, chlorine is introduced into the chloroacetic acid heavy component for reaction, and acetic acid, monochloroacetic acid and dichloroacetic acid are deeply chlorinated to generate trichloroacetic acid; after the chloroacetic acid heavy component is deeply chlorinated, alkali liquor is added for reaction, the product is sodium oxalate relatively singly, and the solubility of the sodium oxalate in aqueous solution is very small and is very easy to separate. This allows for the adequate recovery of the organic components, typically monochloroacetic acid and dichloroacetic acid, from the heavy components without the need for disposal to a sewage treatment system.
The chloroacetic acid heavy component enters a heavy component buffer tank through a heavy component feeding pipeline, a first stirrer is started, steam enters a first jacket through an air inlet pipeline, the steam exchanges heat with the chloroacetic acid heavy component through the first jacket and becomes steam condensate, the steam condensate is discharged from a liquid outlet pipeline, the preheated chloroacetic acid heavy component is pumped into a chlorination reaction kettle through a heavy component pump, a second stirrer is started, chlorine enters the chlorination reaction kettle through a chlorine feeding pipeline for chlorination reaction, the reaction temperature is 160-170 ℃, the reaction pressure is 3-5bar, the reaction time is 60-80h, acetic anhydride is added as a catalyst in the reaction process, so that a chlorinated solution and a gaseous phase containing hydrogen chloride are obtained, the gaseous phase containing the hydrogen chloride is deeply chlorinated through acetic acid, monochloroacetic acid and dichloroacetic acid contained in the chloroacetic acid heavy component and enters a condenser for condensation, the condensate is returned to the chlorination reaction kettle, and the noncondensable gas enters a subsequent tail gas treatment unit for treatment. Since the chlorination reaction is a strong exothermic reaction, the temperature in the kettle needs to be kept constant by cooling through a second jacket.
The method comprises the steps of pumping chloridizing solution into a hydrolysis reaction kettle through a chloridizing solution pump, feeding 15-25% alkali solution into an alkali solution high-level tank through an alkali solution feeding pipeline, discharging alkali solution from the alkali solution high-level tank into the hydrolysis reaction kettle, starting a third stirrer, cooling to 60-85 ℃ through a third jacket to react, reacting trichloroacetic acid with sodium hydroxide to generate sodium oxalate, pumping the obtained hydrolysate into a crystallization kettle through the chloridizing solution pump after the reaction is finished, starting a fourth stirrer, cooling the hydrolysate to 20 ℃ through the fourth jacket, crystallizing and separating sodium oxalate, pumping the obtained slurry into a centrifuge through a slurry pump, performing centrifugal separation, feeding the separated solution into a subsequent sewage treatment unit, treating, feeding washing water into the centrifuge through a washing water inlet pipeline, performing centrifugal washing on the crystals, and discharging washing water after washing is finished to obtain sodium oxalate products.
The utility model has the beneficial effects that: the operation is convenient, the structure is simple, the treatment cost of heavy components is reduced, and the economic and environmental benefits are improved; the heavy component waste liquid which is difficult to treat in the chloroacetic acid production process can be converted into sodium oxalate products, and the components such as acetic acid, monochloroacetic acid, dichloroacetic acid and the like in the heavy components can be recycled; because the solubility of sodium oxalate in aqueous solution is small, the sodium oxalate can be separated and purified from other residual impurities by crystallization with high efficiency.
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
in the figure: 1. a heavy component buffer tank; 2. a chlorination reaction kettle; 3. a hydrolysis reaction kettle; 4. a crystallization kettle; 5. a centrifuge; 6. a condenser; 7. an alkali liquor overhead tank; 8. a heavy component feed line; 9. a first agitator; 10. a first jacket; 11. an air intake line; 12. a liquid outlet pipeline; 13. a heavy component pump; 14. a chlorine gas feed line; 15. a second stirrer; 16. a second jacket; 17. a first cooling water inlet pipe; 18. a first cooling water outlet pipeline; 19. a chloride pump; 20. a third agitator; 21. a third jacket; 22. a second cooling water inlet pipeline; 23. a second cooling water outlet pipeline; 24. a hydrolysis liquid pump; 25. a fourth agitator; 26. a fourth jacket; 27. a third cooling water inlet pipeline; 28. a third cooling water outlet pipeline; 29. a slurry pump; 30. a washing water inlet pipeline; 31. a fourth cooling water inlet pipeline; 32. a fourth cooling water outlet pipeline; 33. an alkali liquor feeding pipeline.
Detailed Description
Embodiments of the utility model are further described below with reference to the accompanying drawings:
as shown in figure 1, the utility model comprises a heavy component buffer tank 1, a chlorination reaction kettle 2, a hydrolysis reaction kettle 3 and a crystallization kettle 4 which are sequentially connected with a centrifuge 5, wherein the chlorination reaction kettle 2 is connected with a condenser 6, and the hydrolysis reaction kettle 3 is connected with an alkali liquor high-level tank 7.
The top of the heavy component buffer tank 1 is provided with a heavy component feeding pipeline 8, a first stirrer 9 is arranged in the heavy component buffer tank 1, a first jacket 10 is coated on the outer side of the heavy component buffer tank 1, and the first jacket 10 is respectively connected with an air inlet pipeline 11 and a liquid outlet pipeline 12.
A heavy component pump 13 is arranged between the heavy component buffer tank 1 and the chlorination reaction kettle 2.
The top of the chlorination reaction kettle 2 is provided with a chlorine feeding pipeline 14, a second stirrer 15 is arranged in the chlorination reaction kettle 2, a second jacket 16 is coated on the outer side of the chlorination reaction kettle 2, and the second jacket 16 is respectively connected with a first cooling water inlet pipeline 17 and a first cooling water outlet pipeline 18.
A chloride pump 19 is arranged between the chlorination reaction kettle 2 and the hydrolysis reaction kettle 3.
The hydrolysis reaction kettle 3 is internally provided with a third stirrer 20, the outside of the hydrolysis reaction kettle 3 is coated with a third jacket 21, the third jacket 21 is respectively connected with a second cooling water inlet pipeline 22 and a second cooling water outlet pipeline 23, and a hydrolysis liquid pump 24 is arranged between the hydrolysis reaction kettle 3 and the crystallization kettle 4.
The crystallization kettle 4 is internally provided with a fourth stirrer 25, the outside of the crystallization kettle 4 is coated with a fourth jacket 26, the fourth jacket 26 is respectively connected with a third cooling water inlet pipeline 27 and a third cooling water outlet pipeline 28, and a slurry pump 29 is arranged between the crystallization kettle 4 and the centrifugal machine 5.
The top of the centrifuge 5 is provided with a wash water inlet pipe 30.
The condenser 6 is connected to a fourth cooling water inlet pipe 31 and a fourth cooling water outlet pipe 32, respectively.
An alkali liquor feeding pipeline 33 is arranged at the top of the alkali liquor overhead tank 7.
The chloroacetic acid heavy component enters the heavy component buffer tank 1 through the heavy component feeding pipeline 8, the first stirrer 9 is started, steam enters the first jacket 10 through the air inlet pipeline 11, the steam exchanges heat with the chloroacetic acid heavy component through the first jacket 10 and becomes steam condensate, the steam condensate is discharged from the liquid outlet pipeline 12, the preheated chloroacetic acid heavy component is pumped into the chlorination reaction kettle 2 through the heavy component pump 13, the second stirrer 15 is started, the chlorine enters the chlorination reaction kettle 2 through the chlorine feeding pipeline 14 for chlorination reaction, the reaction temperature is 160-170 ℃, the reaction pressure is 3-5bar, the reaction time is 60h, acetic anhydride is added as a catalyst in the reaction process, so that a chlorinated solution and a gaseous phase containing hydrogen chloride are obtained, the acetic acid, monochloroacetic acid and dichloroacetic acid which are contained in the chloroacetic acid heavy component are deeply chlorinated through the chlorination reaction, the gaseous phase containing hydrogen chloride enters the condenser 6 for condensation, the condensate is returned to the chlorination reaction kettle 2, and the noncondensable gas enters the subsequent tail gas treatment unit for treatment. Since the chlorination reaction is a strongly exothermic reaction, it is necessary to maintain the temperature in the kettle constant by cooling the second jacket 16.
The chloridizing solution is pumped into the hydrolysis reaction kettle 3 through a chloridizing solution pump 19, 20% alkali solution enters the alkali solution high-level tank 7 through an alkali solution feeding pipeline 33, the alkali solution is discharged from the alkali solution high-level tank 7 and enters the hydrolysis reaction kettle 3, a third stirrer 20 is started, the temperature of the alkali solution is reduced to 60-85 ℃ through a third jacket 21 for reaction, trichloroacetic acid reacts with sodium hydroxide to generate sodium oxalate, the obtained hydrolysate after the reaction is pumped into the crystallization kettle 4 through a hydrolytic solution pump 24, the temperature of the hydrolysate is reduced to 20 ℃ through a fourth jacket 26, sodium oxalate is crystallized and separated out, the obtained slurry is pumped into a centrifuge 5 through a slurry pump 29 for centrifugal separation, the separated solution enters a subsequent sewage treatment unit for treatment, washing water enters the centrifuge 5 through a washing water inlet pipeline 30 for centrifugal washing of the crystal, and the washing water is discharged after the washing is finished to obtain sodium oxalate products.

Claims (10)

1. The utility model provides a chloroacetic acid heavy ends recycle device, includes heavy ends buffer tank (1), its characterized in that heavy ends buffer tank (1), chlorination reaction kettle (2), hydrolysis reaction kettle (3), crystallization kettle (4) link to each other with centrifuge (5) in proper order, and chlorination reaction kettle (2) link to each other with condenser (6), and hydrolysis reaction kettle (3) link to each other with alkali lye elevated tank (7).
2. The chloroacetic acid heavy component recycling device according to claim 1, wherein a heavy component feeding pipeline (8) is arranged at the top of the heavy component buffer tank (1), a first stirrer (9) is arranged in the heavy component buffer tank (1), a first jacket (10) is coated on the outer side of the heavy component buffer tank (1), and the first jacket (10) is respectively connected with an air inlet pipeline (11) and a liquid outlet pipeline (12).
3. The chloroacetic acid heavy component recycling device according to claim 1, wherein a heavy component pump (13) is arranged between the heavy component buffer tank (1) and the chlorination reaction kettle (2).
4. The chloroacetic acid heavy component recycling device according to claim 1, wherein a chlorine feeding pipeline (14) is arranged at the top of the chlorination reaction kettle (2), a second stirrer (15) is arranged in the chlorination reaction kettle (2), a second jacket (16) is coated on the outer side of the chlorination reaction kettle (2), and the second jacket (16) is respectively connected with a first cooling water inlet pipeline (17) and a first cooling water outlet pipeline (18).
5. The chloroacetic acid heavy component recycling device according to claim 1, wherein a chloride pump (19) is arranged between the chlorination reaction kettle (2) and the hydrolysis reaction kettle (3).
6. The chloroacetic acid heavy component recycling device according to claim 1, wherein a third stirrer (20) is arranged in the hydrolysis reaction kettle (3), a third jacket (21) is coated on the outer side of the hydrolysis reaction kettle (3), the third jacket (21) is respectively connected with a second cooling water inlet pipeline (22) and a second cooling water outlet pipeline (23), and a hydrolysis liquid pump (24) is arranged between the hydrolysis reaction kettle (3) and the crystallization kettle (4).
7. The chloroacetic acid heavy component recycling device according to claim 1, wherein a fourth stirrer (25) is arranged in the crystallization kettle (4), a fourth jacket (26) is coated on the outer side of the crystallization kettle (4), the fourth jacket (26) is respectively connected with a third cooling water inlet pipeline (27) and a third cooling water outlet pipeline (28), and a slurry pump (29) is arranged between the crystallization kettle (4) and the centrifugal machine (5).
8. The chloroacetic acid heavy component recycling device according to claim 1, wherein a washing water inlet pipeline (30) is arranged at the top of the centrifugal machine (5).
9. The chloroacetic acid heavy component recycling device according to claim 1, wherein the condenser (6) is connected with a fourth cooling water inlet pipeline (31) and a fourth cooling water outlet pipeline (32) respectively.
10. The chloroacetic acid heavy component recycling device according to claim 1, wherein an alkali liquor feeding pipeline (33) is arranged at the top of the alkali liquor high-level tank (7).
CN202321807929.6U 2023-07-11 2023-07-11 Chloroacetic acid heavy component recycling device Active CN220405585U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202321807929.6U CN220405585U (en) 2023-07-11 2023-07-11 Chloroacetic acid heavy component recycling device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202321807929.6U CN220405585U (en) 2023-07-11 2023-07-11 Chloroacetic acid heavy component recycling device

Publications (1)

Publication Number Publication Date
CN220405585U true CN220405585U (en) 2024-01-30

Family

ID=89658009

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202321807929.6U Active CN220405585U (en) 2023-07-11 2023-07-11 Chloroacetic acid heavy component recycling device

Country Status (1)

Country Link
CN (1) CN220405585U (en)

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