CN218951289U - Device for separating and recovering triethylamine from glyphosate alkali mother liquor - Google Patents
Device for separating and recovering triethylamine from glyphosate alkali mother liquor Download PDFInfo
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- CN218951289U CN218951289U CN202222982658.XU CN202222982658U CN218951289U CN 218951289 U CN218951289 U CN 218951289U CN 202222982658 U CN202222982658 U CN 202222982658U CN 218951289 U CN218951289 U CN 218951289U
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Abstract
The utility model discloses a device for separating and recovering triethylamine from glyphosate alkali mother liquor, wherein an alkali mother liquor pipeline is connected with the upper part of a rectifying tower, and the top of the rectifying tower is connected with a condenser through a gas phase pipeline; the bottom of the condenser is connected with the collecting tank through a liquid phase pipeline; the collecting tank is connected with the material transferring pump through a pipeline and then connected with the dehydration kettle; the dehydration kettle is connected with the lower part of the adsorption tower through a material pump; the adsorption tower is connected with a triethylamine storage tank through a pipeline. The utility model effectively avoids the adverse effect of impurity component accumulation in the fraction on the production of glyphosate, simplifies the technical treatment process, reduces the acid and alkali consumption in the treatment process, 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 device for refining and recovering triethylamine from glyphosate alkali 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 and drying are carried out, and the obtained mother solution after solid-liquid separation is glyphosate acid mother solution.
The common treatment method is to add liquid alkali to the glyphosate acid mother liquor, wherein the triethylamine is subjected to layered recovery, and the rest mother liquor is alkali mother liquor, and the main components of the glyphosate acid mother liquor are water and sodium chloride, and the glyphosate acid mother liquor 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 a small amount of ammonia, triethylamine, methanol and other organic matters. Further separation and recovery of triethylamine, ammonia and alcohol from the alkaline mother liquor is usually further carried out by distillation (rectification). 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 methanol, free ammonia and other substances.
As described in patent document CN113827992a, in industrial production, overhead water is generally used as industrial water in a crystallization or hydrolysis step of glyphosate production, and then the overhead water is reused as mother liquor to recycle triethylamine therein. In another method, as described in the literature such as continuous recovery of triethylamine in the alkyl ester method glyphosate production process, standing and layering the overhead fraction water, dehydrating the separated upper amine water mixed solution to obtain a triethylamine product, and reusing the triethylamine product for synthesis 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 utility model 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 the 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, the ammonia is not thoroughly removed in the method, 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 the ammonia are not radically eliminated. Secondly, the recovery liquid obtained by condensing the overhead fraction is applied to the hydrolysis process, wherein ammonia and triethylamine 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 and converted into ammonia, triethylamine and sodium chloride, so that the process needs to consume acid and alkali and increase the sodium chloride salt amount, and the process is economically disadvantageous.
In addition, other impurities such as aldehyde, acetal, hetero amine and the like are also present in the condensate of the evaporation of the base mother liquor, and no solutions are pointed out or given in the prior literature. The aldehyde and the acetal come from the way of desolventizing residues in a hydrolysis kettle, alkaline hydrolysis of phosphate and polyphosphate, and the like, and the amine is derived from hydrogen-containing amine such as monoethylamine, diethylamine and the like brought by triethylamine as a raw material, and amine substances generated by degradation of triethylamine and glycine in the processes of glyphosate production and mother liquor treatment. The enrichment of the impurities in the glyphosate production system can not be separated from the discharge system, and the enrichment effect is continuously increased along with the time extension, so that the normal production is affected. And (3) applying aldehyde in the overhead fraction to a hydrolysis process, and then carrying out side reaction with glyphosate to reduce the conversion rate.
Disclosure of Invention
Aiming at the defects of the prior art, the device for recycling triethylamine, which has high efficiency in removing impurities such as ammonia, alcohol, aldehyde, hydrogen-containing hybrid amine and the like in the glyphosate alkali mother solution, is simple to operate and has good running economy, is provided.
A device system for separating and recovering triethylamine from glyphosate alkali mother liquor mainly comprises a rectifying tower, a dehydration kettle, an adsorption tower, a condenser and a pump.
The alkali mother liquor pipeline after the triethylamine amine is neutralized and recovered is connected with the upper part of a rectifying tower, the bottom of the rectifying tower is connected with the alkali mother liquor pipeline after the distillation, the top of the rectifying tower is connected with a condenser through a gas phase pipeline, and the condenser is connected with a collecting tank through a liquid phase pipeline; the bottom of the collecting tank is provided with a liquid discharge pipeline, the middle upper part of the collecting tank is provided with another liquid discharge pipeline, and the collecting tank is connected with a material pump through the liquid discharge pipeline and then connected with the upper part of the dehydration kettle; the bottom of the dehydration kettle is provided with a bottom valve and a bottom discharge pipeline; the upper middle part of the dehydration kettle is provided with a triethylamine outlet and a pipeline, the triethylamine outlet and the pipeline are connected with the lower part of the adsorption tower through a material pump, the upper part of the adsorption tower is provided with a pipeline which is connected with a triethylamine storage tank, and triethylamine flows in the adsorption tower in a downward and upward manner; or, the triethylamine discharge pipeline at the middle upper part of the dehydration kettle is connected with the upper part of the adsorption tower through a material pump, the lower part of the adsorption tower is provided with a pipeline which is connected with a triethylamine storage tank, and the triethylamine flows in the adsorption tower according to the upper inlet and the lower outlet; or the adsorption tower is horizontally arranged, a triethylamine discharge pipeline at the upper middle part of the dehydration kettle is connected with one end of the adsorption tower through a material pump, the other end of the adsorption tower is provided with a pipeline which is connected with a triethylamine storage tank, and triethylamine horizontally flows in the adsorption tower; the triethylamine storage tank is connected with the glyphosate synthesis device.
The bottom of the dehydration kettle is provided with a water phase discharge pipeline.
The upper part of the adsorption tower is also provided with a desorption tail gas pipeline which is connected with a tail gas treatment device; the tail gas treatment device comprises a condensing device, an absorbing device and a collecting tank.
The upper part and the lower part of the adsorption tower are respectively connected with a steam pipeline and a steam condensate water discharge pipeline.
The adsorption tower is a shell-and-tube tower or a packed tower. In one of the working conditions, the adsorption tower is a shell-and-tube tower, the adsorbent is filled in the tube, and the steam goes through the shell side.
The utility model has the beneficial effects that: the utility model has simple flow, large single filling and absorbing capacity of the adsorption tower, continuous operation, suitability for batch treatment, low running cost and long running period of the device; refined triethylamine can be directly recovered from the alkali mother liquor distillate without repeated consumption of hydrochloric acid and liquid alkali, so that the economy is good; the quality of the recovered refined triethylamine is stable, the main content reaches 98.5-99.6%, and the adverse effect of fraction accumulation on the production of glyphosate in the treatment process of the traditional method for recycling to crystallization and hydrolysis is effectively avoided.
Drawings
FIG. 1 is a diagram showing the construction of the apparatus of the present utility model, wherein an E1 rectifying tower, an E2 collecting tank, an E3 dehydrating kettle, an E4 condenser, an E5 adsorption tower, a transfer pump E6, a material pump E7, a triethylamine storage tank E8 and an alkaline mother liquor pipeline P1.
Detailed Description
The above-described inventive process is further illustrated by the following specific examples:
example 1
A method and a device for separating and recovering triethylamine from glyphosate alkali mother liquor, wherein an alkali mother liquor pipeline P1 is connected with the upper part of a rectifying tower E1, and the top of the rectifying tower E1 is connected with a condenser E4 through a gas phase pipeline;
the bottom of the condenser E4 is connected with a collecting tank E2 through a liquid phase pipeline;
the collecting tank E2 is connected with a material transferring pump E6 through a pipeline and then connected with a dehydration kettle E3;
the dehydration kettle E3 is connected with the lower part of the adsorption tower E5 through a material pump E7; the bottom of the dehydration kettle E3 is provided with a water phase discharge pipeline;
the adsorption tower E5 is connected with a triethylamine storage tank E8 through a pipeline.
The bottom of the rectifying tower E1 is provided with an alkali mother liquor pipeline; the bottom of the collecting tank E2 is provided with a liquid discharge pipeline.
The adsorption tower E5 is a shell-and-tube tower or a packed tower; when the adsorption tower is a shell-and-tube tower, the adsorbent is filled in the tube, and the steam goes through the shell pass.
Example 2
The device of example 2 differs from the basic system of example 1 in that: the triethylamine discharge pipeline at the middle upper part of the dehydration kettle E3 is connected with the upper part of an adsorption tower through a material pump, the lower part of the adsorption tower E5 is provided with a pipeline which is connected with a triethylamine storage tank E8, and triethylamine flows in the adsorption tower E5 according to the upper inlet and the lower outlet.
Example 3
Mixing acid mother liquor and liquid alkali with the content of 33% in a mixer in the process of producing glyphosate by a glycine method, carrying out neutralization and displacement reaction to obtain triethylamine, standing for layering to obtain triethylamine (an upper layer) and alkali mother liquor (a lower layer), carrying out dehydration treatment on the triethylamine, and recovering to obtain triethylamine with the main content of 99.3% and the water content of 0.21%; 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 86-98 ℃, the temperature of the bottom of the rectifying tower is controlled to be 108-112 ℃, 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 and recycle phosphate and sodium chloride. Collecting condensate liquid in a collecting tank, standing and layering to obtain an upper organic phase, and performing quality inspection analysis: ammonia (mass content 2.1%), triethylamine (mass content 72%), methanol (mass content 1.3%), formaldehyde (mass content 1.2%), methylal (0.6%). The upper organic phase is conveyed to a dehydration kettle, liquid alkali with the content of 35% is added for stirring and dehydration, a kettle bottom water phase 1 is separated, 98% caustic soda flakes are added for stirring and dehydration, a kettle bottom water phase 2 is separated, the water phase 2 is concentrated alkali solution, the content of sodium hydroxide is measured to be 48%, and the mixture is collected for standby. And obtaining a triethylamine crude product after dehydration, wherein the main content is 96.8% and the water content is 0.19%.
And (3) cooling the triethylamine crude product to 0-20 ℃, pumping the triethylamine crude product into the bottom of an adsorption tower, passing through an adsorbent filling layer from bottom to top, adsorbing and removing impurity components, extracting the refined triethylamine with the main content of 99.0% and the water content of 0.19% from the upper part of the adsorption tower, and collecting the triethylamine crude product in a triethylamine storage tank for synthesizing glyphosate. The adsorbent is particles with 90% of calcium chloride and 10% of active carbon, and is paved uniformly.
Example 4
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.
Claims (4)
1. A device for separating and recovering triethylamine from glyphosate alkali mother liquor is characterized in that,
the alkali mother liquor pipeline (P1) is connected with the upper part of the rectifying tower (E1), and the top of the rectifying tower (E1) is connected with the condenser (E4) through a gas phase pipeline;
the bottom of the condenser (E4) is connected with the collecting tank (E2) through a liquid phase pipeline;
the collecting tank (E2) is connected with the material transferring pump (E6) through a pipeline and then connected with the dehydration kettle (E3);
the dehydration kettle (E3) is connected with the lower part of the adsorption tower (E5) through a material pump (E7);
the adsorption tower (E5) is connected with a triethylamine storage tank (E8) through a pipeline.
2. The device for separating and recovering triethylamine from glyphosate alkali mother liquor according to claim 1, wherein an alkali mother liquor pipeline is arranged at the bottom of the rectifying tower (E1); the bottom of the collecting tank (E2) is provided with a liquid discharge pipeline.
3. The device for separating and recovering triethylamine from glyphosate alkali mother liquor according to claim 1, wherein a water phase discharge pipeline is arranged at the bottom of the dehydration kettle (E3).
4. The device for separating and recovering triethylamine from glyphosate base mother liquor according to claim 1, wherein the adsorption tower (E5) is a shell-and-tube tower or a packed tower; when the adsorption tower is a shell-and-tube tower, the adsorbent is filled in the tube, and the steam goes through the shell pass.
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| CN202222982658.XU CN218951289U (en) | 2022-11-09 | 2022-11-09 | Device for separating and recovering triethylamine from glyphosate alkali mother liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677510A (en) * | 2022-11-09 | 2023-02-03 | 湖北泰盛化工有限公司 | Method for separating and recovering triethylamine from glyphosate base mother liquor |
| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677510A (en) * | 2022-11-09 | 2023-02-03 | 湖北泰盛化工有限公司 | Method for separating and recovering triethylamine from glyphosate base mother liquor |
| 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 |
| CN115677510B (en) * | 2022-11-09 | 2024-09-10 | 湖北泰盛化工有限公司 | Method for separating and recovering triethylamine from glyphosate alkali mother liquor |
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