CN209940878U - Device for producing low-sodium glyphosate technical - Google Patents
Device for producing low-sodium glyphosate technical Download PDFInfo
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- CN209940878U CN209940878U CN201920783245.4U CN201920783245U CN209940878U CN 209940878 U CN209940878 U CN 209940878U CN 201920783245 U CN201920783245 U CN 201920783245U CN 209940878 U CN209940878 U CN 209940878U
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Abstract
The utility model provides a device of production low sodium glyphosate original medicine, the cauldron of hydrolysising is connected with the one-level crystallizer, and the one-level crystallizer is connected with one-level solid-liquid separation equipment, and one-level solid-liquid separation equipment is connected with the second grade crystallizer, and the second grade crystallizer is connected with the second grade solid-liquid separation equipment, and the second grade solid-liquid separation equipment is connected with drying device, and drying device is connected to the product packaging district. A triethylamine feeder is arranged at the upper part of the primary crystallizer; an alkali feeder is arranged on the secondary crystallizer. The first-stage solid-liquid separation device is connected with the drying device through a pipeline. Adopt the technical scheme of the utility model the stability of preparation product quality has been improved, sodium ion content in the preparation product has been reduced, the soil environmental problem that causes hardens is avoided etc. The utility model belongs to the technical field of alkyl ester method glyphosate production crystallization, this production system reduces sodium ion content in with former medicine by about 1000ppm to below 150ppm, about 90ppm, improves product quality's stability, improves the environmental protection benefit and the product quality of glyphosate production.
Description
Technical Field
The utility model belongs to alkyl ester method glyphosate technical crystallization production technology and device belongs to the chemical industry equipment field.
Background
Glyphosate is a highly effective, low toxicity, broad spectrum, biocidal, non-selective herbicide with excellent biological properties. At present, the domestic main production process of glyphosate has two routes: alkyl ester processes and iminodiacetic acid processes. The foreign production process is mainly the iminodiacetic acid method of Monsanto company in America, the mainstream process for producing glyphosate in China is glycine-dialkyl phosphite, and the specific flow is as follows: taking triethylamine as a catalyst, depolymerizing paraformaldehyde in a solvent methanol to generate hemiacetal, further reacting with glycine, esterifying with dimethyl phosphite, and then pre-adding acid, carrying out acidolysis, desolventizing, deacidifying, crystallizing, separating and drying the synthetic liquid to obtain the solid glyphosate. The route has the following defects in the production process: 1. and a large amount of hydrochloric acid is added in the pre-acid adding stage to acidify the reaction system, and liquid caustic soda (sodium hydroxide) is used for adjusting the pH value of the reaction system to an optimal range (0.3-1.8) in the crystallization link so as to separate out glyphosate crystals and obtain better granularity (crystal form). The liquid caustic soda added into the system reacts with acid substances such as hydrochloric acid in the glyphosate slurry to produce sodium salt. In the subsequent washing process, most of sodium salt is carried away by the washing water, but more than 1000ppm of sodium ions (about 5000ppm on average, and more than 10000ppm even in the case of high sodium salt) still remain in the raw materials.
The high content of sodium in the raw materials may cause crystallization of the aqueous solution of glyphosate or granules, block spraying equipment and influence the use effect. Meanwhile, the active ingredients of the glyphosate content of the preparation are influenced. A series of environmental protection problems such as soil hardening, salinization, fertility reduction and the like can be caused in the using process. The conventional method in the industry at present increases the water quantity of washing materials or increases the water temperature of the washing materials, and the like, and the measures have certain effect on reducing the content of sodium ions in the original medicine, but simultaneously increase the dissolution loss of glyphosate, reduce the yield, greatly increase the production of mother liquor, and increase the environmental protection treatment cost. Therefore, a new production process and a new production device need to be developed, and the reduction of the content of sodium ions while ensuring the drug effect and the product quality of glyphosate has profound significance for the development of the industry.
Disclosure of Invention
Aiming at the problems and the defects, the utility model provides a crystallization process for producing low-sodium glyphosate technical product by alkyl ester method, which adjusts the crystallization pH by adding triethylamine, reduces the consumption of sodium base, recovers the triethylamine in the link of recovering mother liquor, and reduces the treatment cost of salt in the crystallization liquid; and through fractional crystallization and material washing, the content of sodium ions in the original medicine is reduced, and the improvement of the stability of the aqueous solution is greatly influenced.
The utility model provides a low sodium glyphosate raw medicine fractional crystallization device and implementation step are as follows:
a crystallization device for producing low-sodium glyphosate by an alkyl ester method specifically comprises a hydrolysis kettle, a primary crystallizer, a primary solid-liquid separation device, a secondary crystallizer, a secondary solid-liquid separation device, a triethylamine feeder, an alkali feeder, a drying device and the like.
The hydrolysis kettle is connected with the primary crystallizer, the primary crystallizer is connected with the primary solid-liquid separation device, the primary solid-liquid separation device is connected with the secondary crystallizer, the secondary crystallizer is connected with the secondary solid-liquid separation device, the secondary solid-liquid separation device is connected with the drying device, and the drying device is connected to the product packaging area.
A triethylamine feeder is arranged at the upper part of the primary crystallizer; an alkali feeder is arranged on the secondary crystallizer.
The first-stage solid-liquid separation device is connected with the drying device through a pipeline.
And the secondary solid-liquid separation device is connected to the mother liquor recovery area through a pipeline.
In a preferable scheme, the primary crystallizer and the secondary crystallizer are enamel crystallization kettles and are provided with stirring devices.
In the preferred scheme, the triethylamine adding device of the primary crystallizer can be controlled by a valve, is connected with pH on-line monitoring and is interlocked with the pH value in the primary crystallizer.
In the preferred scheme, the primary solid-liquid separation device can be one of a centrifugal material washing machine and a suction filtration type material washing machine.
In the preferred scheme, the alkali feeder of the secondary crystallizer is a liquid alkali buffer tank (groove) which is controlled by a valve and is connected with pH on-line monitoring.
In the preferred scheme, the wet powder discharge port of the first solid-liquid separator and the wet powder discharge port of the second solid-liquid separator are connected with a belt conveyor or a scraper conveyor, and the device is connected with a drying system
The utility model provides a low sodium glyphosate raw chemicals production crystallization device, beneficial effect is as follows: 1. the content of sodium ions in the glyphosate technical is effectively controlled, and the requirements of high-end customers at home and abroad are met. 2. The cost is saved, the consumption is reduced, the addition amount of alkali is reduced, and triethylamine is added for recycling completely, so that the method is used in the glyphosate synthesis and crystallization links. The soft water consumption in the material washing process is reduced proportionally, and the pressure of wastewater treatment is reduced. 3. The stability of the quality of the preparation product is improved, the content of sodium ions in the preparation product is reduced, and the problem of soil hardening environment is avoided. The utility model belongs to the technical field of alkyl ester method glyphosate production crystallization, this production system reduces sodium ion content by about 1000ppm to below 150ppm, about 90ppm in with former medicine, improves product quality's stability, has reduced manufacturing cost, has alleviateed environmental protection pressure, improves the environmental protection benefit and the product quality of glyphosate production.
Drawings
FIG. 1 is a diagram of a crystallization apparatus for producing low-sodium glyphosate by alkyl ester method, wherein, 1 is a hydrolysis kettle, 2 is a primary crystallizer, 3 is a primary solid-liquid separation device, 4 is a secondary crystallizer, 5 is a secondary solid-liquid separation device, 6 is a drying device, 7 is a triethylamine feeder, and 8 is an alkali feeder.
Detailed Description
Example 1
The utility model provides a device for producing low sodium glyphosate original medicine, hydrolysis kettle 1 is connected with one-level crystallizer 2, and one-level crystallizer 2 is connected with one-level solid-liquid separation equipment 3, and one-level solid-liquid separation equipment 3 is connected with second grade crystallizer 4, and second grade crystallizer 4 is connected with second grade solid-liquid separation equipment 5, and second grade solid-liquid separation equipment 5 is connected with drying device 6, and drying device 6 is connected to the product packaging district.
A triethylamine feeder 7 is arranged at the upper part of the primary crystallizer 2; an alkali feeder 8 is arranged on the secondary crystallizer 4.
The first-stage solid-liquid separation device 3 is connected with a drying device 6 through a pipeline.
The secondary solid-liquid separation device 5 is connected to the mother liquor recovery zone through a pipeline.
Example 2
Transferring the slurry subjected to hydrolysis and dealcoholization to a crystallizer for cooling, wherein the pH value range in the slurry for crystallization is-1 to-0.3, the temperature of the slurry is generally controlled to be about 80 to 90 ℃ when the slurry enters a primary crystallizer, triethylamine is added when the temperature is reduced to 60 to 70 ℃ after the slurry is cooled for 1 hour, the pH value in the slurry for crystallization is adjusted by the addition amount of the triethylamine at the moment and is controlled to be 0.1 to 0.6, when the temperature is reduced to 30 to 40 ℃, the material enters a primary washing device for solid-liquid separation, and is separately dried and packaged after separation, so that glyphosate with low sodium ion content (the average content is below 100 ppm) is obtained, and the crystal form condition is better; and (3) transferring the primary mother liquor after solid-liquid separation to a secondary crystallizer because triethylamine is weak in alkalinity and a small amount of glyphosate in the mother liquor is not effectively recovered, adding a sodium hydroxide solution into the secondary crystallizer, controlling the pH value of crystallization to be between 0.6 and 1.8, cooling the crystallization for 1 to 2 hours, cooling the crystallization to about 30 ℃ to enter a secondary washing device for solid-liquid separation, and packaging after drying (the average concentration is about 500 plus 1000 ppm).
Claims (4)
1. The device for producing the glyphosate technical with low sodium content is characterized in that a hydrolysis kettle (1) is connected with a primary crystallizer (2), the primary crystallizer (2) is connected with a primary solid-liquid separation device (3), the primary solid-liquid separation device (3) is connected with a secondary crystallizer (4), the secondary crystallizer (4) is connected with a secondary solid-liquid separation device (5), the secondary solid-liquid separation device (5) is connected with a drying device (6), and the drying device (6) is connected to a product packaging area.
2. The device for producing the glyphosate technical material with low sodium content according to claim 1, wherein a triethylamine adder (7) is arranged at the upper part of the primary crystallizer (2); an alkali feeder (8) is arranged on the secondary crystallizer (4).
3. The device for producing the glyphosate technical with low sodium content as claimed in claim 1, wherein the primary solid-liquid separation device (3) is connected with the drying device (6) through a pipeline.
4. The apparatus for producing a low-sodium glyphosate bulk drug according to claim 1, wherein the secondary solid-liquid separation device (5) is connected to the mother liquor recovery zone via a pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920783245.4U CN209940878U (en) | 2019-05-28 | 2019-05-28 | Device for producing low-sodium glyphosate technical |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920783245.4U CN209940878U (en) | 2019-05-28 | 2019-05-28 | Device for producing low-sodium glyphosate technical |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407871A (en) * | 2019-08-30 | 2019-11-05 | 湖北泰盛化工有限公司 | Glyphosate crystal device and method for crystallising |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110407871A (en) * | 2019-08-30 | 2019-11-05 | 湖北泰盛化工有限公司 | Glyphosate crystal device and method for crystallising |
| CN110407871B (en) * | 2019-08-30 | 2022-04-08 | 湖北泰盛化工有限公司 | Glyphosate crystallization device and crystallization method |
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