Advanced treatment device for glyphosate evaporation concentrated solution

By diluting and washing the glyphosate evaporation concentrate, the separation of sodium chloride by membrane technology was solved, and the problems of low sodium pyrophosphate quality and unstable operation of the incinerator were solved, thus improving the coke Sodium phosphate quality and the effect of reducing treatment costs.

CN222274304UActive Publication Date: 2024-12-31HUBEI TAISHENG CHEM
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Patent Information

Application Number
CN202420786986.9
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-04-16
Publication Date
2024-12-31
Estimated Expiration
2034-04-16

AI Technical Summary

Technical Problem

The sodium chloride content in the evaporated concentrate produced during glyphosate mother liquor treatment is too high, resulting in low quality of sodium pyrophosphate products and easy to coke during incineration, affecting the operation of the device and product value.

Method used

By diluting and washing the evaporated concentrate, sodium chloride is separated by membrane technology to reduce its content, improve the quality of sodium pyrophosphate and the working conditions of the incinerator, and extend the operating time of the device.

Benefits of technology

The quality of sodium pyrophosphate and the operating state of the incinerator are improved, the processing cost is reduced, the value of by-products is increased, and the effective operation time of the device is extended.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model provides an advanced treatment device for a glyphosate evaporation concentrated solution. An evaporation concentrated solution ground pool is connected with a dilution water tank through a transfer pump; the dilution water tank is connected with the pH adjusting mixer through the transfer pump; the mixer is connected with the filter, the filter is connected with the heat exchanger, the heat exchanger is connected with the buffer water tank, and the buffer water tank is connected with the high-pressure membrane through the high-pressure pump; the high-pressure membrane is connected with the light salt brine tank; the light salt brine tank is connected with the light salt brine film through a high-pressure pump. The method comprises the following steps: performing salt leaching and membrane treatment on an evaporation concentrated solution with high COD (Chemical Oxygen Demand), high total phosphorus and high sodium chloride content, separating phosphorus and salt components in the evaporation concentrated solution to obtain a phosphorus concentrated solution and a salt concentrated solution, reducing the phosphorus concentrated solution in an evaporation device, incinerating to prepare high-quality sodium pyrophosphate, returning the salt concentrated solution to an MVR (Mechanical Vapor Recompression) and a multi-effect evaporation device, and recovering sodium chloride in the salt concentrated solution; after the glyphosate evaporation concentrated solution is subjected to deep treatment, the operation condition of coking and wall hanging of the sodium pyrophosphate incinerator is solved, the labor intensity of coke cleaning operation of workers is reduced, and stable operation of the device is guaranteed.
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Description

Technical Field

[0001] The utility model belongs to the technical field of wastewater treatment in the chemical industry. The deep treatment device of evaporation concentrate provided by the utility model can separate phosphorus and salt components in wastewater, especially for evaporation concentrate with high COD, high phosphorus and high sodium chloride produced in the treatment of glyphosate mother liquor. Background Art

[0002] Glyphosate is a highly effective, broad-spectrum, low-toxic and safe herbicide. There are two main methods for its industrial production: one is the production method using iminodiacetic acid (IDA) as raw material, and the other is the production method using glycine and alkyl phosphite as raw materials. Our company's glyphosate production adopts the glycine-alkyl ester synthesis process, with triethylamine as catalyst, polyformaldehyde depolymerizes in solvent methanol to generate hemiacetal, which is further reacted with glycine and then esterified with dimethyl phosphite. The synthetic liquid is then mixed with hydrochloric acid, acidolyzed, desolventized, deacidified, crystallized, separated, and dried to obtain solid glyphosate. The glyphosate mother liquor produced after synthesis has the characteristics of high phosphorus, high nitrogen, high COD and high sodium chloride content. After ECO wet catalytic oxidation, various C, N, P-containing organic matter and phosphite in the glyphosate mother liquor are oxidized into CO2, N2, NH3 and orthophosphate. Then, by-products such as phosphate, sodium chloride and ammonia water are obtained through deamination, extraction, refining, evaporation concentration and incineration, so as to achieve the purpose of resource utilization of glyphosate mother liquor.

[0003] In the process of glyphosate mother liquor treatment, the evaporation concentrate produced by the multi-effect and MVR evaporation devices is transferred to the sodium coke incinerator for incineration to produce sodium pyrophosphate. The sodium chloride content in the evaporation concentrate is about 12.0%, and the COD and TP contents are both above 100,000 ppm. Due to the high sodium chloride content, the sodium pyrophosphate produced by the sodium coke incinerator is mostly low-quality products. The main content of low-quality sodium pyrophosphate is only about 50.0%, and the sodium chloride content is about 30.0%. The product value is low, and during the incineration process of the evaporation concentrate, the material is easy to coke and hang on the wall due to the high sodium chloride content, which affects the normal production and operation of the device. Summary of the invention

[0004] The utility model analyzes the contents of components such as COD, TP, and sodium chloride in the evaporation concentrate. Due to the high contents of COD and TP, it is difficult to directly separate sodium chloride from the evaporation concentrate with current process technologies or devices. Through process experiments, it is found that after the evaporation concentrate is diluted and the pH is adjusted, concentrated water with low sodium chloride content can be obtained through membrane treatment, and the produced water is returned to the multi-effect and MVR for further evaporation and concentration to recover sodium chloride. After the concentrated water is incinerated, sodium pyrophosphate of good quality is obtained, the main content of which can reach more than 90.0%, the sodium chloride content can be reduced to less than 5.0%, and it is loose and not easy to coke. Finally, the membrane treatment technology method and device of "dilution + water washing" are determined to deeply treat the glyphosate evaporation concentrate, which can improve the quality of the sodium pyrophosphate obtained by incineration, improve the working conditions of the incinerator, extend the effective operation time of the incinerator, and reduce the treatment cost of the glyphosate mother liquor.

[0005] Purpose of the invention

[0006] The utility model provides a glyphosate evaporation concentrate deep treatment device. Its purpose is to dilute the evaporation concentrate with water, wash it with water, and separate it through a membrane group, so as to reduce the sodium chloride content in the evaporation concentrate, improve the quality of the sodium pyrophosphate obtained by incineration, and improve the working conditions of the incinerator, increase the value of the by-products, reduce the processing cost, and finally achieve the purpose of increasing the resource utilization value of the glyphosate mother liquor and stabilize the development of the green circular economy of glyphosate.

[0007] A device for deep processing of glyphosate evaporation concentrate, wherein the evaporation concentrate pool is connected to a dilution water tank via a transfer pump;

[0008] The dilution water tank is connected to the mixer via transfer pump 2;

[0009] The mixer is connected to the filter, the filter is connected to the heat exchanger, the heat exchanger is connected to the cache water tank,

[0010] The cache water tank is connected to the high-pressure membrane via high-pressure pump three;

[0011] The high-pressure membrane is connected to the salt water tank;

[0012] The salt water tank is connected to the salt water membrane via a high pressure pump 7.

[0013] The high-pressure membrane is connected to the cleaning water tank; the cleaning water tank is connected to the water-washing membrane through a high-pressure pump 6.

[0014] The water-washed membrane is connected to the concentrated water tank, the concentrated water tank is connected to the evaporation device through the transfer pump 8, and the evaporation device is connected to the evaporation condensation water tank;

[0015] The evaporation device is connected to the concentrated liquid ground pool;

[0016] The evaporation condensation water storage tank is connected to the high pressure pump nine, and the high pressure pump nine is connected to the RO membrane, so as to achieve the purpose of transporting the evaporation condensation water to the RO membrane.

[0017] The wash water tank is connected to the dilution water tank via a transfer pump 4; the water tank is connected to the cleaning water tank 9 via a transfer pump 5.

[0018] The salt water membrane is connected to the washing water tank; the RO membrane is connected to the washing water tank.

[0019] The RO membrane is connected to the salt water tank.

[0020] In the utility model, the evaporation concentrated liquid ground pool is connected with a transfer pump, and the transfer pump is connected with a dilution water tank, so that the evaporation concentrated liquid is transferred from the ground pool to the dilution water tank.

[0021] The dilution water tank is connected to the transfer pump 2, the transfer pump 2 is connected to the pH adjusting mixer, the mixer is connected to the filter, the filter 4 is connected to the heat exchanger 5, and the heat exchanger is connected to the cache water tank, so as to achieve the purpose of transporting the diluted evaporated concentrate to the cache water tank after pH adjustment, filtration and temperature control.

[0022] The cache water tank is connected to high-pressure pump three, and high-pressure pump three is connected to the high-pressure membrane, so as to achieve the purpose of transporting the material in the cache water tank to the high-pressure membrane.

[0023] The high-pressure membrane is connected to the cleaning water tank to achieve the purpose of transporting concentrated water to the cleaning water tank.

[0024] The high-pressure membrane is connected to the salt water tank to achieve the purpose of transporting the produced water to the salt water tank.

[0025] The wash water tank is connected to the transfer pump four, and the transfer pump four is connected to the dilution water tank, so as to achieve the purpose of transporting the wash water to the dilution water tank.

[0026] The wash water tank is connected to the transfer pump 5, and the transfer pump 5 is connected to the cleaning water tank, so as to achieve the purpose of transferring the wash water to the cleaning water tank.

[0027] The cleaning water tank is connected to the high-pressure pump six, and the high-pressure pump six is ​​connected to the water-washing membrane, so as to achieve the purpose of transferring the materials in the cleaning water tank to the water-washing membrane.

[0028] The water-washed membrane is connected to the concentrated water pool to achieve the purpose of transferring the concentrated water to the concentrated water ground pool.

[0029] The water-washed membrane is connected to the salt water tank to achieve the purpose of transporting the produced water to the salt water tank.

[0030] The salt water tank is connected to the high pressure pump seven, and the high pressure pump seven is connected to the salt water membrane, so as to achieve the purpose of transferring the materials in the salt water tank to the salt water membrane.

[0031] The salt water membrane is connected to the washing water tank to achieve the purpose of transporting the produced water to the washing water tank.

[0032] The concentrated water pool is connected to the transfer pump 8, and the transfer pump 8 is connected to the evaporation device, so as to achieve the purpose of transferring the concentrated water to the evaporation device.

[0033] The evaporation device is connected to the evaporation condensation water tank to achieve the purpose of transporting the evaporation condensation water to the evaporation condensation water tank.

[0034] The evaporation device is connected to the concentrated liquid pool to achieve the purpose of transferring the concentrated liquid to the concentrated liquid pool.

[0035] The evaporation condensation water storage tank is connected to the high pressure pump nine, and the high pressure pump nine is connected to the RO membrane, so as to achieve the purpose of transporting the evaporation condensation water to the RO membrane.

[0036] The RO membrane is connected to the salt water tank to transfer the concentrated water to the salt water tank.

[0037] The RO membrane is connected to the wash water tank to achieve the purpose of transferring the produced water to the wash water tank.

[0038] The evaporated concentrate and the washing water are diluted in the dilution water tank in proportion, and then the pH is adjusted by the mixer, the impurities are removed by the overpressure filter, and the temperature is controlled by the heat exchanger. The material enters the cache water tank for cache, and then undergoes primary separation through the high-pressure membrane to obtain high-pressure membrane produced water and concentrated water. The high-pressure membrane concentrated water enters the cleaning water tank and is mixed with the washing water in proportion for salt washing. The high-pressure membrane produced water enters the brine water tank; the washing water in the washing water tank enters the dilution water tank through the transfer pump, and the washing water enters the cleaning water tank through the transfer pump. The remaining washing water can be used as other industrial water; after the washing of the washing water tank is completed, the material enters the water washing membrane for secondary separation to obtain water washing membrane produced water and concentrated water. The produced water enters the brine water tank, and the concentrated water from the washing membrane enters the concentrated water pool; the concentrated water in the concentrated water pool is transported to the evaporation device through a transfer pump for reduction, and the concentrated liquid enters the concentrated liquid pool, and the evaporated condensed water enters the evaporative condensed water storage tank; the evaporated condensed water in the evaporative condensed water storage tank enters the RO membrane through a high-pressure pump for membrane separation to obtain RO membrane produced water and concentrated water, the RO membrane produced water enters the washing water tank, and the RO membrane concentrated water enters the brine water tank; the solution in the brine water tank enters the brine membrane through a high-pressure pump for separation to obtain brine membrane produced water and concentrated water, the brine membrane produced water enters the washing water tank, and the brine membrane concentrated water returns to the original MVR and multi-effect evaporation device for evaporation.

[0039] Beneficial Effects

[0040] The utility model innovatively provides a method and device for deep treatment of glyphosate evaporation concentrate, which can effectively separate phosphorus and salt components in the evaporation concentrate. Different dilution ratios, cleaning water volumes, and water production ratios result in different effective separation effects.

[0041] In the innovative process of the utility model, for the evaporation concentrate produced in the treatment of glyphosate mother liquor, the COD content is about 120000ppm, the TP content is about 100000ppm, and the sodium chloride content is about 12.0%. The evaporation concentrate is mixed and diluted with water at a ratio of 1:3, and washed with water at a ratio of 1:2 to finally obtain a phosphorus concentrate with a sodium chloride content of less than 1.0% and a TP content of about 60000ppm. After evaporation and concentration treatment, the amount of phosphorus concentrate is halved, the TP content is increased to about 120000ppm, and the sodium chloride content is within 2.0%. The evaporation concentrate is incinerated, and the quality of the obtained sodium pyrophosphate is greatly improved, the main content reaches about 96.0%, and the sodium chloride content is reduced to about 3.0%, and the evaporation concentrate is not easy to coke and hang on the wall during the incineration process.

[0042] The investigation found that the value of the sodium pyrophosphate product obtained by incinerating the glyphosate evaporated concentrate treated by the device of the utility model increased by nearly RMB 1,700 / ton compared with the original low-value sodium pyrophosphate, the incineration conditions were greatly improved, and the workload of employees in the coke cleaning operation was reduced. BRIEF DESCRIPTION OF THE DRAWINGS

[0043] Figure 1 This is a device structure diagram of the utility model, wherein, evaporation concentrate pool 1, transfer pump one 1-1, dilution water tank 2, transfer pump two 2-1, mixer 3, filter 4, heat exchanger 5, cache water tank 6, high pressure pump three 6-1, high pressure membrane 7, wash water tank 8, transfer pump four 8-1, transfer pump five 8-2, cleaning water tank 9, high pressure pump six 9-1, water washing membrane 10, brine water tank 11, high pressure pump seven 11-1, brine membrane 12, concentrated water pool 13, transfer pump eight 13-1, evaporation device 14, concentrated liquid pool 15, evaporation condensate storage tank 16, high pressure pump nine 16-1, RO membrane 17. DETAILED DESCRIPTION

[0044] A device for deep processing of glyphosate evaporation concentrate, wherein an evaporation concentrate pool 1 is connected to a dilution water tank 2 via a transfer pump 1-1;

[0045] The dilution water tank 2 is connected to the mixer 3 via the transfer pump 2-1;

[0046] The mixer 3 is connected to the filter 4, the filter 4 is connected to the heat exchanger 5, and the heat exchanger 5 is connected to the cache water tank 6.

[0047] The cache water tank 6 is connected to the high pressure membrane 7 via the high pressure pump 3 6-1;

[0048] The high pressure membrane 7 is connected to the salt water tank 11;

[0049] The desalinated water tank 11 is connected to the desalinated water membrane 12 via a high pressure pump 11-1.

[0050] The high-pressure membrane 7 is connected to the cleaning water tank 9; the cleaning water tank 9 is connected to the water-washing membrane 10 via a high-pressure pump 6 9-1.

[0051] The water-washed membrane 10 is connected to the concentrated water pool 13, the concentrated water pool 13 is connected to the evaporation device 14 via the transfer pump 8 13-1, and the evaporation device 14 is connected to the evaporation condensation water tank 16;

[0052] The evaporation device 14 is connected to the concentrated liquid pool 15;

[0053] The evaporation condensation water storage tank 16 is connected to the high pressure pump 16-1, and the high pressure pump 16-1 is connected to the RO membrane 17, so as to achieve the purpose of transporting the evaporation condensation water to the RO membrane.

[0054] The dilution water tank 2 is connected to the washing water tank 8 via the transfer pump 4 8-1; the water tank 8 is connected to the cleaning water tank 9 via the transfer pump 5 8-2.

[0055] The desalinated water membrane 12 is connected to the washing water tank 8 ; the RO membrane 17 is connected to the washing water tank 8 .

[0056] The RO membrane 17 is connected to the salt water tank 11 .

[0057] The method for deep treatment of glyphosate evaporation concentrate using the device of the utility model is as follows:

[0058] During the treatment of glyphosate mother liquor, the MVR and multi-effect evaporation devices produce about 210 tons of concentrated liquid every day, which is cached in the evaporation concentrated liquid pool. The concentrated liquid is transferred to the dilution water tank at a dilution ratio of 1:3, and 630 tons of washing water are added for mixing and dilution. The dilution is then introduced into the mixer for pH adjustment with hydrochloric acid to control the pH in the range of 6.5-7.5, and an ultrafiltration filter is used to remove impurities in the solution. The material temperature is then controlled in the range of 20-35°C by a heat exchanger, and the material is cached in the cache water tank. The material is then passed through a high-pressure membrane for phosphorus and salt separation, to obtain about 504 tons of produced water 1 and about 336 tons of concentrated water 1, with a water production ratio of 1.5:1.0; wherein the produced water 1 enters the light salt water tank for membrane separation treatment, and the concentrated water 1 enters the cleaning water tank for salt washing. 672 tons of cleaning water are added at a ratio of 1:2, and after cleaning and mixing, they enter the water washing membrane for separation, to obtain about 798 tons of produced water 2 and about 210 tons of concentrated water 2. Tons, the water production ratio is 3.8:1.0; among them, water 2 enters the salt water tank and then undergoes membrane separation treatment. The sodium chloride content of concentrated water 2 is within 1.0%. It is evaporated and concentrated to produce about 110 tons of concentrate. The sodium chloride content of the concentrate is within 2.0%, and the TP content is about 120000ppm. The concentrate is incinerated, and the main content of sodium pyrophosphate is 96.1%, and the sodium chloride content is reduced to 3.1%; water 1, water 2 and concentrated water 4 are salt water, which are treated by salt water membrane to obtain water 3 and concentrated water 3, which are 1137 tons and 415 tons respectively. Water 3 is used as dilution water and cleaning water, and concentrated water 3 will continue to evaporate and concentrate in MVR and multi-effect devices; the evaporated condensed water produced by the evaporation device is treated by RO membrane to obtain water 4 and concentrated water 4. Water 4 is used as dilution water and cleaning water. The excess of water 4 and water 3 is used as other industrial water, and can also be directly discharged into the sewage treatment station.

Claims

1. A device for deep treatment of glyphosate evaporation concentrate, characterized in that: The evaporation concentrate pool (1) is connected to the dilution water tank (2) via a transfer pump (1-1); The dilution water tank (2) is connected to the mixer (3) via the transfer pump 2 (2-1); The mixer (3) is connected to the filter (4), the filter (4) is connected to the heat exchanger (5), and the heat exchanger (5) is connected to the cache water tank (6). The buffer water tank (6) is connected to the high-pressure membrane (7) via the high-pressure pump three (6-1); The high-pressure membrane (7) is connected to a salt water tank (11); The salt water tank (11) is connected to the salt water membrane (12) via a high-pressure pump (11-1).

2. The glyphosate evaporation concentrated liquid deep processing device according to claim 1, characterized in that: The high-pressure membrane (7) is connected to a cleaning water tank (9); the cleaning water tank (9) is connected to a water-washing membrane (10) via a high-pressure pump six (9-1).

3. The glyphosate evaporation concentrated liquid deep processing device according to claim 2, characterized in that: The water-washed membrane (10) is connected to a concentrated water tank (13), the concentrated water tank (13) is connected to an evaporation device (14) via a transfer pump eight (13-1), and the evaporation device (14) is connected to an evaporation condensate storage tank (16); The evaporation device (14) is connected to the concentrated liquid pool (15); The evaporated condensed water storage tank (16) is connected to the high-pressure pump nine (16-1), and the high-pressure pump nine (16-1) is connected to the RO membrane (17), so as to achieve the purpose of transporting the evaporated condensed water to the RO membrane.

4. The glyphosate evaporation concentrated liquid deep processing device according to claim 3, characterized in that: The dilution water tank (2) is connected to a washing water tank (8) via a transfer pump 4 (8-1); the washing water tank (8) is connected to a cleaning water tank (9) via a transfer pump 5 (8-2).

5. The glyphosate evaporation concentrated liquid deep processing device according to claim 4, characterized in that: The salt water membrane (12) is connected to the washing water tank (8); and the RO membrane (17) is connected to the washing water tank (8).

6. The glyphosate evaporation concentrated liquid deep processing device according to claim 5, characterized in that: The RO membrane (17) is connected to the salt water tank (11).