CN218778875U - Device for separating and recovering alcohol and aldehyde from glyphosate mother liquor - Google Patents
Device for separating and recovering alcohol and aldehyde from glyphosate mother liquor Download PDFInfo
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- CN218778875U CN218778875U CN202222983576.7U CN202222983576U CN218778875U CN 218778875 U CN218778875 U CN 218778875U CN 202222983576 U CN202222983576 U CN 202222983576U CN 218778875 U CN218778875 U CN 218778875U
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Abstract
The utility model provides a separate device of retrieving alcohol, aldehyde from glyphosate mother liquor, the adsorption tower top is connected with desorption tail gas condenser, and desorption tail gas condenser bottom is connected with the collecting liquid groove, and the collecting liquid groove is connected with mixer one, mixer two in proper order, and mixer two is connected with the reaction liquid storage tank. The top of the adsorption tower is connected with a desorption tail gas water washing tower through a pipeline, and the desorption tail gas water washing tower is connected with a non-condensable gas absorption tower of the water washing tower; the desorption tail gas water scrubber is connected with the liquid collecting tank, and the top of the non-condensable gas absorption tower of the water scrubber is provided with a non-condensable gas tail gas pipeline. The utility model discloses can follow organic matters such as recovery methyl alcohol, methylal in the separation recovery triethylamine in the glyphosate alkali mother liquor, improve the quality of retrieving triethylamine on the one hand, on the other hand still organic matters such as resource recovery methyl alcohol. But continuous operation, be fit for batch processing, the device running cost is low moreover, the run length is long.
Description
Technical Field
The utility model belongs to the technical field of glycine method glyphosate, concretely relates to separate device of retrieving alcohol, aldehyde from glyphosate mother liquor.
Technical Field
The conventional process for producing glyphosate by using a glycine method comprises the following steps: 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, a synthetic solution is prepared, hydrochloric acid is added for acidolysis and hydrolysis reaction, the temperature is raised to remove the solvent, slurry containing glyphosate is obtained, glyphosate crystals are separated out through stirring, cooling and crystallization and alkali addition for adjusting the pH value in the crystallization process, then solid-liquid separation is carried out in the solid-liquid separation process, glyphosate wet powder and glyphosate acid mother liquor are obtained, and the glyphosate wet powder is dried to obtain a technical product.
The acid mother liquor contains a large amount of triethylamine hydrochloride and a small amount of organic matters such as alcohols, aldehydes and the like. The common treatment method for the glyphosate acid mother liquor is to add liquid caustic soda to the glyphosate acid mother liquor for treatment, firstly recover triethylamine in a layered manner, and the residual mother liquor is the alkali mother liquor, wherein the main components of the alkali mother liquor are water and sodium chloride, and the residual mother liquor also contains high-boiling-point substances such as phosphorus-containing substances (glyphosate, glyphosine, phosphorous acid, hydroxymethyl phosphoric acid, methyl glyphosate, phosphate ester, polyphosphate ester and the like), glycine and derivatives thereof, sodium hydroxide, other salts and the like, and a small amount of low-boiling-point substances such as ammonia, triethylamine, methanol and the like. Usually, low boiling substances such as triethylamine, ammonia, and alcohol are further separated and recovered from the alkali mother liquor by a distillation (rectification) method.
And distilling the alkali mother liquor by a rectifying tower, and separating to obtain a tower bottom mother liquor, a tower top fraction and a non-condensable gas, wherein the tower bottom mother liquor is subjected to a post-process to further recover salt, phosphorus and nitrogen resources, and the non-condensable gas is subjected to deep cooling or absorption recovery to obtain ammonia water. In the process, the distillate water extracted from the top of the triethylamine rectifying tower mainly comprises water and triethylamine, and in addition, the distillate water also comprises free ammonia, methanol and other organic matters.
According to literature and published reports, the overhead distillate water is generally applied to a crystallization process of glyphosate production, and enters mother liquor again after being used as industrial water, and triethylamine in the mother liquor is recycled. In the other method, the distillate water at the top of the tower is kept stand for layering, the separated upper-layer amine water mixed solution is dehydrated to obtain a triethylamine product, and the triethylamine product is recycled to synthesize glyphosate; and the lower-layer amine-water mixed liquor is merged into the alkali mother liquor for redistillation or is applied to the crystallization process of glyphosate production. According to the method, in the early-stage production operation of the system, the content of various impurities is low, but as the production time continues, methanol, free ammonia and other impurities in the distillate water are accumulated and enriched continuously because the methanol, the free ammonia and other impurities do not have discharge conditions until the quality of triethylamine is seriously influenced, and the energy efficiency and the conversion rate of the whole glyphosate production system are further influenced. The main problem is that the concentration of impurities reduces the glyphosate conversion rate; 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 water from the top fraction of a rectification column of alkali mother liquor in a glyphosate production process, wherein a recycling solution obtained by condensing a fraction obtained by rectifying the alkali mother liquor of glyphosate is added into a hydrolysis kettle in the glyphosate production process by a glycine method to be used as industrial water, and methanol is distilled out for recycling in the heating process of a hydrolysis procedure; and after the residual triethylamine hydrochloride completes the subsequent processes of glyphosate production crystallization and solid-liquid separation along with the mother liquor, the triethylamine hydrochloride enters the acid mother liquor again for circular treatment. The recovered ammonia water is used for preparing the ammonium glyphosate water agent. The patent realizes the recovery of amine, ammonia and alcohol in the alkali mother liquor, realizes the separation of alcohol from a mother liquor system in the distillation tower top fraction of the alkali mother liquor, and has certain effect on avoiding the enrichment of methanol in the system. Thus, the method has achieved certain efficacy, but many problems remain unsolved. Firstly, in the method of the patent, the removal of ammonia is not thorough, the ammonia dissolved in the overhead fraction is reused in the mother liquor along with the fraction water jacket 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 the ammonia are not fundamentally eliminated. Secondly, in the method, the recovered liquid obtained by condensing the fraction at the top of the tower is applied to a hydrolysis process to recover methanol, ammonia and triethylamine in the condensed liquid are alkaline substances, a large amount of hydrochloric acid is consumed to form hydrochloride, and in the subsequent neutralization process of acid mother liquid, a large amount of liquid alkali is consumed by the hydrochloride and is converted into ammonia, triethylamine and sodium chloride, so that the process needs to consume acid and alkali and increase the amount of sodium chloride salt, and the method is not economical. Thirdly, aldehyde resources are not recovered and the hybrid amine is not effectively removed.
SUMMERY OF THE UTILITY MODEL
Aiming at the defects of the prior art, the device for economically and efficiently separating and recovering the alcohol and the aldehyde from the glyphosate mother liquor is provided.
The utility model discloses the following technical scheme of accessible realizes:
the utility model provides a device of alcohol, aldehyde are retrieved in separation from glyphosate mother liquor, adsorption column top and desorption tail gas condenser are connected, and desorption tail gas condenser bottom is connected with the collecting liquid groove, and the collecting liquid groove is connected with blender one, blender two in proper order, and blender two is connected with the reaction liquid storage tank.
The top of the adsorption tower is connected with a desorption tail gas water washing tower through a pipeline, and the desorption tail gas water washing tower is connected with a non-condensable gas absorption tower of the water washing tower; the desorption tail gas water scrubber is connected with the liquid collecting tank, and the top of the non-condensable gas absorption tower of the water scrubber is provided with a non-condensable gas tail gas pipeline.
An oxidant pipeline is arranged on the first mixer; and a methanol pipeline is arranged on the second mixer.
The reaction liquid storage tank is connected with the glyphosate hydrolysis kettle.
The reaction liquid storage tank is connected with the rectifying tower of the glyphosate methanol recovery procedure through a pipeline.
The utility model discloses beneficial effect: the utility model discloses can follow organic matters such as recovery methyl alcohol, methylal in the separation recovery triethylamine in the glyphosate alkali mother liquor, improve the quality of retrieving triethylamine on the one hand, on the other hand still organic matters such as resource recovery methyl alcohol. But continuous operation, be fit for batch processing, the device running cost is low moreover, the run length is long.
Drawings
FIG. 1 is a device for separating and recovering alcohol and aldehyde from glyphosate mother liquor. 1. The device comprises an adsorption tower, 2a tail gas desorption condenser, 3 a tail gas desorption water scrubber, 4 a non-condensable gas absorption tower of the water scrubber, 5 a liquid collection tank, 6-1 a mixer I, 6-2 a mixer II, 7 a reaction liquid storage tank, 8 a glyphosate hydrolysis kettle and 9 a glyphosate methanol recovery process rectifying tower.
Detailed Description
The above utility model process is further explained by the following specific embodiments:
example 1
The utility model discloses a device that the method of following the separation of glyphosate alkali mother liquor and retrieving organic matter adopted, specifically be the device system of separation recovery alcohol, aldehyde, including adsorption tower, desorption tail gas condenser, desorption tail gas scrubbing tower, scrubbing tower noncondensable gas absorption tower, collection liquid tank, blender one, blender two, reaction liquid storage tank;
on the basis of embodiment 1, a device for separating and recovering alcohol and aldehyde from glyphosate mother liquor is provided, wherein the top of an adsorption tower 1 is connected with a desorption tail gas condenser 2, the bottom of the desorption tail gas condenser 2 is connected with a liquid collecting tank 5, the liquid collecting tank 5 is sequentially connected with a first mixer 6-1 and a second mixer 6-2, and the second mixer 6-2 is connected with a reaction liquid storage tank 7.
The top of the adsorption tower 1 is connected with a desorption tail gas water scrubber 3 through a pipeline, and the desorption tail gas water scrubber 3 is connected with a non-condensable gas absorption tower 4 of the water scrubber; desorption tail gas scrubbing tower 3 is connected with collection liquid tank 5, and 4 tops in scrubbing tower noncondensable gas absorption tower are provided with noncondensable gas tail gas pipeline.
An oxidant pipeline 10-1 is arranged at the upper part of the mixer I6-1; the upper part of the second mixer 6-2 is provided with a methanol pipeline 10-2. A reaction liquid storage tank 7 is connected with a glyphosate hydrolysis kettle 8; the reaction liquid storage tank 7 is also connected with a rectifying tower 9 of the glyphosate methanol recovery procedure through a pipeline.
Example 2
Mixing an acid mother liquor and 35% liquid caustic soda in a process of producing glyphosate by a glycine method in a neutralization mixer, obtaining triethylamine through neutralization and displacement reaction, standing for layering, layering to obtain triethylamine (an upper layer) and an alkali mother liquor (a lower layer), performing dehydration treatment on the triethylamine, and recovering to obtain triethylamine with the main content of 99.2% and the water content of 0.19%; conveying the alkali mother liquor into a triethylamine rectifying tower for rectification, controlling the tower top temperature to be 88-108 ℃ and the tower bottom temperature to be 120-125 ℃ by the rectifying tower, and condensing tower top fraction to obtain condensate; the non-condensable gas is sent to a tail gas tower to be absorbed to obtain ammonia water; and (3) oxidizing, crystallizing and distilling the distilled alkali mother liquor to extract salt and recover phosphorus and salt resources.
And (3) collecting the condensate into a collection 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%), and methylal (0.2%). And (3) conveying the upper organic phase to a dehydration kettle, adding 98% flake caustic soda, stirring and dehydrating, separating out a kettle bottom water phase 2, measuring the sodium hydroxide content by taking the water phase 2 as concentrated alkali liquor, and collecting for later use. After dehydration, a triethylamine crude product is obtained, the main content is 97.8 percent, and the water content is 0.21 percent.
Pumping the triethylamine crude product into the bottom of the adsorption tower at normal temperature (20-30 ℃). The adsorbent is 80% of calcium chloride and 20% of active carbon particles, and is uniformly paved. The triethylamine crude product passes through the adsorbent filling layer from bottom to top to remove impurity components through adsorption, refined triethylamine with the main content of 99.2% and the water content of 0.18% is obtained from the upper part of the adsorption tower and collected in a triethylamine storage tank for synthesizing glyphosate.
Example 3
After 40 days of continuous operation according to the method described in example 2, the adsorbent was regenerated by the apparatus described in example 1, and methanol and methylal resources were recovered. Stopping the adsorption tower, draining liquid in the tower from the lower part, closing a triethylamine feed valve at the bottom and a triethylamine discharge valve at the top, opening a desorption tail gas pipeline valve, opening a shell-pass steam valve and a condensate water drain valve of the adsorption tower, adjusting the steam valve to control the temperature of the top of the adsorption tower to be between 100 and 120 ℃, controlling micro negative pressure through a tail gas fan, sucking and desorbing for 100 minutes under the negative pressure, and supplementing a small amount of nitrogen from the bottom of the tower to drive organic steam in the tower. The desorption gas contains methanol, formaldehyde and ammonia, a small amount of triethylamine and other miscellaneous amines, the desorption gas is pumped out of the adsorption tower by a fan, and the desorption gas is condensed and washed by water to be absorbed, and the condensate and the washing liquid are collected to obtain a collecting liquid; and (4) absorbing the non-condensable gas by adopting a copper sulfate aqueous solution, and then emptying the absorbed non-condensable gas.
Adding 30% industrial hydrochloric acid into a collection tank to acidify the collected liquid, adjusting the pH value to 2-3, uniformly mixing, and pumping the mixture into a reaction liquid storage tank through a static mixer 1 and a static mixer 2 in sequence; uniformly adding 8% by mass of hydrogen peroxide into the feed side of the static mixer 1 according to 1.2% of the mass flow of the acidified collecting liquid, and uniformly mixing by the static mixer; uniformly adding methanol at the feed side of a static mixer 2 according to 2% of the mass flow of the acidified collecting solution, uniformly mixing by the static mixer, collecting the mixture into a reaction solution storage tank, standing for 30 minutes, then mechanically applying the reaction solution to the hydrolysis solution of the glycine-method glyphosate hydrolysis process, uniformly stirring and desolventizing, wherein the methanol and the methylal enter a methanol recovery system for recovery through a gas phase pipe of a hydrolysis kettle, and the triethylamine salt is left in the glyphosate slurry, crystallized by a crystallization kettle and separated by suction filtration to obtain glyphosate powder and acid mother liquor.
Claims (5)
1. The utility model provides a separate device of retrieving alcohol, aldehyde from glyphosate mother liquor which characterized in that, adsorption tower (1) top is connected with desorption tail gas condenser (2), and desorption tail gas condenser (2) bottom is connected with collecting liquid groove (5), and collecting liquid groove (5) are connected with blender one (6-1), blender two (6-2) in proper order, and blender two (6-2) are connected with reaction liquid storage tank (7).
2. The device for separating and recovering alcohol and aldehyde from glyphosate mother liquor according to claim 1, wherein the top of the adsorption tower (1) is connected with a desorption tail gas water scrubber (3) through a pipeline, and the desorption tail gas water scrubber (3) is connected with a non-condensable gas absorption tower (4) of the water scrubber; the desorption tail gas water scrubber (3) is connected with the liquid collecting tank (5), and the top of the non-condensable gas absorption tower (4) of the water scrubber is provided with a non-condensable gas tail gas pipeline.
3. The device for separating and recovering alcohol and aldehyde from glyphosate mother liquor according to claim 1, wherein an oxidant pipeline (10-1) is arranged on the first mixer (6-1); a methanol pipeline (10-2) is arranged on the second mixer (6-2).
4. The device for separating and recovering alcohol and aldehyde from glyphosate mother liquor according to claim 1, characterized in that the reaction solution storage tank (7) is connected with the glyphosate hydrolysis kettle (8).
5. The device for separating and recovering alcohol and aldehyde from glyphosate mother liquor according to claim 1, wherein the reaction solution storage tank (7) is connected with the rectifying tower (9) of the glyphosate methanol recovery process through a pipeline.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202222983576.7U CN218778875U (en) | 2022-11-09 | 2022-11-09 | Device for separating and recovering alcohol and aldehyde from glyphosate mother liquor |
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| CN202222983576.7U CN218778875U (en) | 2022-11-09 | 2022-11-09 | Device for separating and recovering alcohol and aldehyde from glyphosate mother liquor |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819250A (en) * | 2022-11-09 | 2023-03-21 | 湖北泰盛化工有限公司 | Method for separating and recovering organic matters from glyphosate alkali mother liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115819250A (en) * | 2022-11-09 | 2023-03-21 | 湖北泰盛化工有限公司 | Method for separating and recovering organic matters from glyphosate alkali mother liquor |
| CN115819250B (en) * | 2022-11-09 | 2024-09-10 | 湖北泰盛化工有限公司 | Method for separating and recovering organic matters from glyphosate alkali mother liquor |
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