CN218944414U - Adsorbent regenerating device for recycling organic matters in glyphosate mother liquor - Google Patents
Adsorbent regenerating device for recycling organic matters in glyphosate mother liquor Download PDFInfo
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- CN218944414U CN218944414U CN202222982657.5U CN202222982657U CN218944414U CN 218944414 U CN218944414 U CN 218944414U CN 202222982657 U CN202222982657 U CN 202222982657U CN 218944414 U CN218944414 U CN 218944414U
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Abstract
The utility model provides an adsorbent regeneration device for recovering organic matters from glyphosate mother liquor, wherein the bottom of an adsorption tower is connected with a liquefied liquid collecting tank through a pipeline, the liquefied liquid collecting tank is connected with a rectifying tower, the rectifying tower is connected with a layering tank, the layering tank is connected with a middle tank, and the middle tank is connected with a spray granulation tower. The top of the rectifying tower is connected with a rectifying tower condenser, the rectifying tower condenser is connected with a rectifying tower fraction condensate storage tank, and the rectifying tower fraction condensate storage tank is connected with the adsorption tower. The device can be operated continuously, is suitable for batch processing, and has low running cost and long running period.
Description
Technical Field
The utility model belongs to the technical field of glycine method glyphosate, and particularly relates to a regeneration device for an adsorbent for recycling organic matters in glyphosate mother liquor.
Technical Field
The conventional process for producing glyphosate by the glycine method is as follows: in the synthesis process, formaldehyde, glycine and dimethyl phosphite are used as raw materials, methanol is used as a solvent, triethylamine is used as a catalyst to prepare a synthetic solution, hydrochloric acid is added to carry out acidolysis and hydrolysis reaction, the temperature is raised to remove the solvent, a slurry containing glyphosate is obtained, glyphosate crystals are separated out in the crystallization process through stirring, cooling, crystallization and pH value adjustment by adding alkali, then solid-liquid separation is carried out in the solid-liquid separation process to obtain glyphosate wet powder and glyphosate acid mother liquor, and the glyphosate wet powder is dried to obtain a raw medicine product.
The acid mother liquor contains a large amount of triethylamine hydrochloride and also contains a small amount of alcohols, aldehydes and other organic matters. The common treatment method is to add liquid alkali to the glyphosate acid mother liquor, firstly, layering and recovering triethylamine, wherein the rest mother liquor is mainly composed of water and sodium chloride, and also contains phosphorus-containing substances (glyphosate, gan Lin, phosphorous acid, hydroxymethyl phosphoric acid, methyl glyphosate, phosphate, polyphosphate and the like), glycine and derivatives thereof, sodium hydroxide, other salts and other high-boiling substances and a small amount of ammonia, triethylamine, methanol and other low-boiling substances. Usually, low boiling substances such as triethylamine, ammonia and alcohol are further separated and recovered from the alkaline mother liquor by a distillation (rectification) method.
And the alkali mother liquor is distilled by a rectifying tower and then separated to obtain three parts of tower bottom mother liquor, tower top fraction and noncondensable gas, wherein the tower bottom mother liquor is sent to a later process to further recover salt, phosphorus and nitrogen resources, and the noncondensable gas is subjected to cryogenic cooling or absorption recovery to obtain ammonia water. In the process, the main components of the distilled water led out from the top of the triethylamine rectifying tower are water and triethylamine, and the distilled water also contains free ammonia, methanol and other organic matters.
According to the literature and the disclosure, overhead fraction water is generally applied to a crystallization process of glyphosate production, and is used as industrial water to enter mother liquor again for recycling triethylamine. In the other method, standing and layering the overhead fraction water, dehydrating the separated upper amine water mixed solution to obtain a triethylamine product, and recycling the triethylamine product to be synthesized with glyphosate; the lower amine water mixed solution is combined into an alkali mother solution for redistillation or is applied to a crystallization process of glyphosate production. In the method, in the early production operation of the system, the content of various impurities is lower, but as the production time continues, methanol, free ammonia and other impurities in the distilled water are continuously accumulated and enriched until the quality of triethylamine is seriously influenced and the energy efficiency and conversion rate of the whole glyphosate production system are further influenced due to no discharge condition. The main problem is that the concentration of impurities reduces the conversion rate of glyphosate; the distilled water is repeatedly and circularly distilled, so that a large amount of steam is consumed in the repeated distillation process, and the steam consumption of the triethylamine rectifying tower is high; the gasification amount of the rectifying tower is large, so that the pressure of the rectifying tower is unstable, and even potential safety hazards are formed.
Patent document CN113827992a discloses a method for recycling distilled water at the top of an alkali mother liquor rectifying tower in the glyphosate production process, wherein a recovered liquid obtained by condensing a distilled fraction obtained by rectifying the glyphosate alkali mother liquor is added into a hydrolysis kettle in the process of producing glyphosate by a glycine method to be used as industrial water, and methanol is distilled out for recycling in the heating process of the hydrolysis process; the rest triethylamine hydrochloride enters the acid mother solution again for circulation treatment after completing the subsequent processes of glyphosate production crystallization and solid-liquid separation along with the mother solution. The recovered ammonia water is used for preparing ammonium glyphosate aqua. The patent realizes the recovery of amine, ammonia and alcohol in the alkali mother liquor, realizes the separation of alcohol in the distillation overhead fraction of the alkali mother liquor from a mother liquor system, and has a certain effect on avoiding the enrichment of methanol in the system. Therefore, the method achieves a certain effect, but has a plurality of problems which are not solved. Firstly, in the method of the patent, the removal of ammonia is not thorough, the dissolved ammonia in the overhead fraction returns to the mother liquor along with the water jacket of the fraction to be used in the hydrolysis process, and the negative problems of influencing the pressure stability of the rectifying tower and the like caused by the enrichment of ammonia are not eliminated fundamentally. In the method of the patent, the recovery liquid obtained by condensing the overhead fraction is applied to the hydrolysis process to recover methanol, ammonia and triethylamine in the condensate are alkaline substances, a large amount of hydrochloric acid is consumed to form hydrochloride, and in the subsequent neutralization process of the acid mother liquor, a large amount of liquid alkali is consumed by the hydrochloride to convert the hydrochloride into ammonia, triethylamine and sodium chloride, so that the process needs to consume acid and alkali and increase the sodium chloride amount, and the economical disadvantage exists. Thirdly, aldehyde resources are not recovered, and the hetero amine is not effectively removed.
Disclosure of Invention
Aiming at the defects of the prior art, the device for regenerating the adsorbent for recycling the organic matters in the glyphosate mother liquor is provided.
The bottom of the auxiliary tower is connected with a liquefied liquid collecting tank through a pipeline, the liquefied liquid collecting tank is connected with a rectifying tower, the rectifying tower is connected with a layering tank, the layering tank is connected with a middle tank, and the middle tank is connected with a spray granulation tower.
The top of the rectifying tower is connected with a rectifying tower condenser, the rectifying tower condenser is connected with a rectifying tower fraction condensate storage tank, and the rectifying tower fraction condensate storage tank is connected with the adsorption tower.
The layering tank is connected to a condensate collecting tank after the triethylamine is separated from the glyphosate mother solution; the lower part of the layering groove is also provided with a slurry discharging pipeline.
The lower part of the spray granulation tower is connected to the regenerated adsorbent packaging port.
The utility model has the beneficial effects that: the utility model can separate and recycle triethylamine from the glyphosate alkali mother liquor and recycle organic matters such as methanol, methylal and the like, on one hand, the quality of recycling the triethylamine is improved, and on the other hand, the organic matters such as methanol and the like are recycled. The device can be operated continuously, is suitable for batch processing, and has low running cost and long running period.
Drawings
The device is shown in the figure 1, wherein the device is used for regenerating an organic matter recovered from glyphosate mother liquor, the device is composed of an adsorption tower, a liquefied liquid collecting tank, a rectifying tower condenser, a rectifying tower distillate condensate storage tank, a layering tank, a middle tank, a spray granulation tower and a slurry discharging pipeline.
Detailed Description
Example 1
The utility model relates to a device used in a method for separating and recycling organic matters from glyphosate alkali mother liquor, in particular to a device for recycling organic matters adsorbent regeneration, which comprises an adsorption tower, a liquefied liquid collecting tank, a rectifying tower condenser, a rectifying tower distillate condensate storage tank, a layering tank, a middle tank and a spray granulation tower;
on the basis of the embodiment 1, an adsorbent regeneration device for recycling organic matters in glyphosate mother liquor is provided, the bottom of an adsorption tower 1 is connected with a liquefied liquid collecting tank 2 through a pipeline, the liquefied liquid collecting tank 2 is connected with a rectifying tower 3, the rectifying tower 3 is connected with a layering tank 6, the layering tank 6 is connected with an intermediate tank 7, and the intermediate tank 7 is connected with a spray granulation tower 8.
The top of the rectifying tower 3 is connected with a rectifying tower condenser 4, the rectifying tower condenser 4 is connected with a rectifying tower fraction condensate storage tank 5, and the rectifying tower fraction condensate storage tank 5 is connected with the adsorption tower 1.
The layering tank 6 is connected to a condensate collecting tank after the triethylamine is separated from the glyphosate mother solution; the lower part of the layering tank 6 is also provided with a slurry discharge pipeline 9.
Example 2
Mixing an acid mother solution and 35% liquid alkali in the process of producing glyphosate by a glycine method in a neutralization mixer, carrying out neutralization and replacement reaction to obtain triethylamine, standing for layering, layering to obtain triethylamine (an upper layer) and an alkali mother solution (a lower layer), dehydrating the triethylamine, and recovering to obtain triethylamine with a main content of 99.2% and a water content of 0.19%; the alkali mother liquor is delivered into a triethylamine rectifying tower for rectification, the temperature of the top of the rectifying tower is controlled to be 88-108 ℃, the temperature of the bottom of the rectifying tower is controlled to be 120-125 ℃, and the distillate at the top of the rectifying tower is condensed to obtain condensate; absorbing the noncondensable gas by a tail gas removal tower to obtain ammonia water; and (3) oxidizing, crystallizing and distilling the distilled alkali mother liquor to extract salt to recover phosphorus and salt resources.
Collecting condensate liquid into a collecting tank, standing and layering to obtain an upper organic phase, and analyzing: ammonia (mass content 2.8%), triethylamine (mass content 75%), methanol (mass content 1.9%), formaldehyde (mass content 1.7%), methylal (0.2%). The upper organic phase is conveyed to a dehydration kettle, 98% caustic soda flakes are added for stirring and dehydration, the kettle bottom water phase 2 is separated, the water phase 2 is concentrated alkali liquor, the content of sodium hydroxide is measured to be 42%, and the mixture is collected for standby. And obtaining a triethylamine crude product after dehydration, wherein the main content is 97.8% and the water content is 0.21%.
Pumping the triethylamine crude product into the bottom of an adsorption tower at normal temperature (20-30 ℃). The adsorbent is prepared from 80% of calcium chloride and 20% of active carbon particles, and is paved uniformly. The triethylamine crude product passes through an adsorbent filling layer from bottom to top, impurities are removed by adsorption, refined triethylamine with the main content of 99.2% and the water content of 0.18% is obtained by extraction from the upper part of an adsorption tower, and is collected by a triethylamine storage tank and used for synthesizing glyphosate.
Example 3
After 320 batches of oil phase materials are adsorbed and treated by the adsorption tower according to the method described in the embodiment 2, the device described in the embodiment 1 is used for regenerating the adsorbent, a fan is used for pumping gas in the adsorption tower away from the adsorption tower, then an oil phase inlet and an oil phase outlet are closed, a methanol feed port at the upper part of the adsorption tower is opened for adding methanol, a liquid outlet at the lower part of the adsorption tower is opened, hot water is introduced into the adsorption tower for heating the adsorbent in a partition wall mode, the temperature is controlled to 40-80 ℃, and the adsorbent is liquefied and is discharged from the liquid outlet at the lower part of the adsorption tower.
The liquefied adsorbent mainly contains mixed solution of methanol and calcium chloride and also contains a small amount of triethylamine. And discharging the liquefied adsorbent liquid into a liquefied liquid collecting tank, pumping into a rectifying tower for rectification, condensing methanol vapor at the top of the tower to obtain methanol, and collecting for later use. The mixed solution of concentrated calcium chloride, methanol and water is obtained at the tower bottom and is collected into a collecting tank, and is divided into an upper layer, a middle layer and a lower layer after standing; the supernatant was the amine layer and was pooled into the condensate collection tank of example 1 for uniform treatment; the lower layer is a slurry layer, and is discharged into a ton barrel for periodic decontamination primary station treatment; the middle layer is a methanol solution of calcium chloride, the methanol solution is pumped into a spray granulation tower, the temperature is controlled at 260 ℃, calcium chloride particles are obtained through high temperature, and the adsorption tower is paved again according to the proportion of 95% of recovered calcium chloride particles and 5% of activated carbon.
Claims (4)
1. The device for regenerating the organic matter adsorbent in the glyphosate mother liquor is characterized in that the bottom of an adsorption tower (1) is connected with a liquefied liquid collecting tank (2) through a pipeline, the liquefied liquid collecting tank (2) is connected with a rectifying tower (3), the rectifying tower (3) is connected with a layering tank (6), the layering tank (6) is connected with a middle tank (7), and the middle tank (7) is connected with a spray granulation tower (8).
2. The device for regenerating the adsorbent for recycling organic matters in the glyphosate mother liquor according to claim 1, wherein the top of the rectifying tower (3) is connected with a rectifying tower condenser (4), the rectifying tower condenser (4) is connected with a rectifying tower fraction condensate storage tank (5), and the rectifying tower fraction condensate storage tank (5) is connected with the adsorption tower (1).
3. The device for regenerating the adsorbent for recycling organic matters from the glyphosate mother liquor according to claim 1, wherein the layering tank (6) is connected to a condensate collecting tank after triethylamine is separated from the glyphosate mother liquor; the lower part of the layering groove (6) is also provided with a slurry discharging pipeline (9).
4. The device for regenerating the organic matter recovered from the glyphosate mother liquor according to claim 1, wherein the lower part of the spray granulation tower (8) is connected to a regenerated adsorbent packing port.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222982657.5U CN218944414U (en) | 2022-11-09 | 2022-11-09 | Adsorbent regenerating device for recycling organic matters in glyphosate mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202222982657.5U CN218944414U (en) | 2022-11-09 | 2022-11-09 | Adsorbent regenerating device for recycling organic matters in glyphosate mother liquor |
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