CN110407871B - Glyphosate crystallization device and crystallization method - Google Patents
Glyphosate crystallization device and crystallization method Download PDFInfo
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- CN110407871B CN110407871B CN201910815615.2A CN201910815615A CN110407871B CN 110407871 B CN110407871 B CN 110407871B CN 201910815615 A CN201910815615 A CN 201910815615A CN 110407871 B CN110407871 B CN 110407871B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/38—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se)
- C07F9/3804—Phosphonic acids RP(=O)(OH)2; Thiophosphonic acids, i.e. RP(=X)(XH)2 (X = S, Se) not used, see subgroups
- C07F9/3808—Acyclic saturated acids which can have further substituents on alkyl
- C07F9/3813—N-Phosphonomethylglycine; Salts or complexes thereof
Abstract
The invention provides a glyphosate crystallization device and a crystallization method. Adding an auxiliary agent into the glyphosate hydrolysis slurry, cooling the slurry to 70-100 ℃, transferring the slurry into a first-stage material washing device, performing suction filtration and centrifugation to separate out the mother liquor to obtain glyphosate solid A and glyphosate mother liquor 1, and conveying the glyphosate mother liquor 1 to a mother liquor intermediate tank; adding a glyphosate aqueous solution into a first-stage material washing device, soaking and washing glyphosate solid A, performing suction filtration and centrifugal separation to obtain a washing solution B to obtain glyphosate wet powder, and drying to obtain glyphosate raw pesticide; and (3) carrying out neutralization reaction on the glyphosate mother liquor 1 and an alkaline substance. The method has the advantages that the glyphosate technical product is crystallized and washed, the crystallization time is greatly shortened, the glyphosate content in the mother liquor is low, the glyphosate crystal form is good, the granularity is moderate, and the method has obvious economic, quality and environmental protection benefits.
Description
Technical Field
The invention belongs to the technical field of glyphosate production by a glycine method, and particularly relates to a method for crystallizing and cleaning glyphosate technical.
Background
The glyphosate has the characteristics of high efficiency, low toxicity, spectrum and extinction, has excellent performance, is the most popular herbicide with the largest global yield and sale, and provides wide opportunity for the glyphosate along with the rapid increase of global population and the development of transgenic technology. At present, the mainstream judgment of glyphosate is safe and low-toxicity, but in recent years, the suspected wind wave of glyphosate carcinogenesis is continuous, and the main consumer countries of glyphosate put higher requirements on the purity of glyphosate raw pesticide. Secondly, the prior glyphosate crystallization process has defects, the traditional indirect method crystallization has the problems of long crystallization time (generally reaching 7 hours), large occupied area and large equipment investment, and the continuous method crystallization has the problems of high glyphosate content in mother liquor and low yield of raw pesticide. Therefore, the glyphosate crystallization, cleaning and refining technology still has further improved requirements.
China is the main world producing nation of glyphosate, and the capacity and the yield account for about 70 percent of the world. There are 2 mainstream production methods for glyphosate, namely an IDA method and a glycine method. In China, the process for synthesizing glyphosate by a glycine method is dominant, and accounts for about 75% of national glyphosate yield and 80% of actual yield. Therefore, the continuous perfection of the alkyl ester method glyphosate production process has strong practical significance for China. The invention is also the result of experimental development under the background of quality improvement and upgrading of products, energy conservation, consumption reduction, emission reduction and ecological green development.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method and a device for crystallizing and cleaning glyphosate technical, which are characterized in that an auxiliary agent is used for treating glyphosate slurry, the glyphosate slurry is divided into two sections at the same time, and the glyphosate aqueous solution is used for cleaning the slurry, so that the crystallization time can be shortened, the mother liquor amount and the glyphosate dissolution amount can be reduced, the problem of explosive nucleation during crystallization can be avoided, the glyphosate granularity is good, the purity is improved, and the clean production is promoted.
A glyphosate bulk drug crystallization and abluent device:
a glyphosate crystallization device is characterized in that a glyphosate hydrolysis kettle is connected with a first section crystallization kettle (or the glyphosate hydrolysis kettle is directly connected with a first section washing device), the first section crystallization kettle is connected with the first section washing device, and the first section washing device is connected with a drying tower.
The first-stage washing device is connected with a mother liquid intermediate tank, the mother liquid intermediate tank is connected with a neutralization mixer, the neutralization mixer is connected with a second-stage crystallization kettle, and the second-stage crystallization kettle is connected with the second-stage washing device.
The pH value of the slurry can also be adjusted by adding an alkaline substance into the two-stage crystallization kettle.
The two-stage washing device is connected with a mother liquor tank, and the mother liquor tank is connected with a mother liquor recovery device. The two-section washing device is also connected with the drying tower.
And the first-stage crystallization kettle is provided with an auxiliary agent feeding pipe and is connected with the auxiliary agent groove.
The first section of the material washing device is provided with a glyphosate aqueous solution tank and a water inlet pipe I.
The neutralization mixer is provided with an alkaline substance feeding pipe.
And a water inlet pipe II is arranged on the two-stage washing device.
In order to achieve the purpose, the invention adopts the following technical method:
(1) first-stage crystallization and solid-liquid separation: transferring the glyphosate hydrolysate in the hydrolysis kettle into a crystallization kettle. And (3) cooling the slurry by introducing cooling water into a jacket of the crystallization kettle, adding no alkaline substance, regulating the pH value of the slurry, and cooling the slurry to 70-100 ℃. Or directly cooling the slurry in the hydrolysis kettle to 70-100 ℃. And then transferring the glyphosate into a section of washing device, separating the mother liquor by means of suction filtration, centrifugation and the like to obtain glyphosate solid A and filtrate (glyphosate mother liquor 1), and conveying the filtrate to a mother liquor intermediate tank.
The glyphosate hydrolysate is glyphosate slurry obtained by hydrolyzing and acidolyzing glyphosate by glycine-alkyl ester method under acidic condition and removing solvent, and the temperature is 115 +/-15 ℃ and the pH value is below 0.
Preferably, an auxiliary agent is added into the slurry to improve the crystallization effect. The auxiliary agent is substances with oxidizing and dispersing effects such as hydrogen peroxide, aluminum trichloride, sodium hypochlorite, sodium chlorite, sodium chlorate and the like.
The material washing device and the material washing process refer to intermittent material washing devices and modes such as a centrifugal machine, a trough type suction filter and the like, and can also refer to continuous material washing devices and modes such as a belt type vacuum suction filter and the like.
(2) First-stage washing: adding a glyphosate aqueous solution into a first-stage material washing device, soaking and washing the glyphosate solid A, dissolving out impurities, separating out a washing solution B through separation means such as suction filtration, centrifugation and the like to obtain glyphosate wet powder, and drying to obtain glyphosate raw pesticide.
The glyphosate aqueous solution is an aqueous solution with the glyphosate content of 0-3%.
Preferably, the aqueous glyphosate solution has a sodium ion content of less than 1000 ppm.
The addition amount of the glyphosate aqueous solution is 0.6-2 times (weight ratio) of the solid content in the slurry.
The glyphosate aqueous solution can be added at one time or added in multiple times. Preferably, the washing liquid obtained from the washing with the fresh glyphosate aqueous solution is reused for the first washing of the next batch of glyphosate solid A. Part of the washing liquid B is sent to a mother liquid intermediate tank, and part of the washing liquid B is added into the slurry of the hydrolysis kettle or the crystallization kettle for recycling.
(3) Primary mother liquor neutralization: (2) and (3) carrying out neutralization reaction on the glyphosate mother liquor 1 in the mother liquor intermediate tank and an alkaline substance through a pipeline mixer, and adjusting the pH value to be in a range of 0-2.0. The pH value of the slurry can also be adjusted by adding an alkaline substance into the two-stage crystallizer. The alkaline substance is any one of sodium hydroxide, potassium carbonate, sodium carbonate and ammonia or organic amine.
(4) Two-stage crystallization, solid-liquid separation and washing: (3) and (4) the neutralized mother liquor is sent to a two-stage crystallization kettle, and is slowly cooled for crystallization, wherein the crystallization time is 2-7 hours. When the temperature of the slurry is reduced to below 30 ℃, the slurry is transferred to a two-stage material washing device, and the mother liquor is separated by means of separation such as suction filtration, centrifugation and the like, so as to obtain glyphosate solid B and filtrate (glyphosate mother liquor 2). And (3) washing the glyphosate solid B by using water to obtain glyphosate wet powder, and drying to obtain glyphosate technical product. The wash water from the fresh water wash is preferably recycled to wash the next batch of slurry and the wash water is recycled to the mother liquor.
Preferably, a small amount of glyphosate technical product obtained by (2) the first-stage crystallization drying is added as seed crystal, and the addition amount of the seed crystal is 0.01-1% of the mass of the solvent in the crystallizer.
(5) Mother liquor treatment: (4) and (3) returning the filtrate (glyphosate mother liquor 2) to a mother liquor post-treatment process to recover triethylamine and phosphorus-containing substances.
Advantageous effects
The invention provides a method and a device for crystallizing and cleaning glyphosate. The method is used for crystallizing and cleaning glyphosate technical product, the crystallization time is shortened to about 3 hours from 7 hours in the traditional process, the crystallization time is shortened by more than 50 percent, the crystallization device occupies small area, and the equipment investment is saved. The glyphosate has good crystal form, moderate granularity and small dust, the glyphosate content in the mother liquor is low (0.1-0.2 percent), and the glyphosate has obvious economic, quality and environmental protection benefits.
Drawings
FIG. 1 is a process flow diagram for glyphosate crystallization and washing. Figure 2 is a glyphosate crystallization and cleaning apparatus. The equipment comprises a glyphosate hydrolysis kettle 1, a first-stage crystallization kettle 2, a first-stage washing device 3, a mother liquor intermediate tank 4, a neutralization mixer 5, a drying tower 6, a second-stage washing device 7, a mother liquor tank 8, a mother liquor recovery device 9, a second-stage crystallization kettle 10, an auxiliary agent tank 11, a glyphosate aqueous solution tank 12, a water inlet pipe I13, an alkaline substance inlet pipe 14 and a water inlet pipe II 15.
Detailed Description
Example 1
A glyphosate crystallization device, a glyphosate hydrolysis kettle 1 is connected with a first section crystallization kettle 2, the first section crystallization kettle 2 is connected with a first section washing device 3, and the first section washing device 3 is connected with a drying tower 6;
the first-stage washing device 3 is connected with a mother liquor intermediate tank 4, the mother liquor intermediate tank 4 is connected with a neutralization mixer 5, the neutralization mixer 5 is connected with a second-stage crystallization kettle 10, the second-stage crystallization kettle 10 is connected with a second-stage washing device 7, and the second-stage washing device 7 is connected with a drying tower 6;
the drying tower 6 is connected with a glyphosate technical product packaging device.
The second-stage washing device 7 is connected with a mother liquor tank 8, the mother liquor tank 8 is connected with a mother liquor recovery device 9, and the first-stage washing device 3 is respectively connected with the first-stage crystallization kettle 2 and the mother liquor intermediate tank 4.
An auxiliary agent tank 11 is arranged on the first section of crystallization kettle 2, and a glyphosate aqueous solution tank 12 and a water inlet pipe 13 are arranged on the first section of washing device 3.
The neutralization mixer 5 is provided with an alkaline substance feeding pipe 14, and the two-stage washing device 7 is provided with a water inlet pipe II 15.
Example 2
Taking 520g of glyphosate hydrolysis slurry, adding 0.15 percent (mass ratio) of sodium chlorite, cooling and crystallizing for 30 minutes, transferring the glyphosate hydrolysis slurry into a centrifugal washing machine when the temperature is reduced to 100 ℃, and separating mother liquor to obtain 160g of glyphosate solid. The filtrate (glyphosate mother liquor 1)) was collected in an amount of 360 g.
80g of 1.5% glyphosate aqueous solution is added to soak and wash the glyphosate solid, 98g of glyphosate solid is obtained after centrifugal separation and filtration. And then 60g of 1.5% glyphosate aqueous solution is added into the material washing machine to soak and wash the glyphosate solid, and 67g of filtrate is separated by centrifugation to obtain 135g of glyphosate solid. Drying in a baking oven to obtain glyphosate with the main content of 96.9 percent and the average grain diameter of 92 mu m.
Pumping the collected glyphosate mother liquor 1 and 32% sodium hydroxide liquid caustic soda into a pipeline mixer for neutralization, controlling the pH value of the mixed liquor to be 1.1, slowly cooling and crystallizing for 4 hours in a two-stage crystallization kettle, transferring into a two-stage material washing device when the temperature of slurry is reduced to be below 30 ℃, and separating out the mother liquor through suction filtration to obtain 35g of glyphosate solid and 362g of filtrate (glyphosate mother liquor 2). Adding 30g of water to soak and wash the glyphosate solid, and centrifugally separating 39g of filtrate (washing solution B1); 24g of glyphosate solid was obtained. Drying in a baking oven to obtain glyphosate raw pesticide with main content of 95.6% and average particle size of 102 μm, wherein the glyphosate content in the mother liquor is 1.36%.
Example 3
Taking 500g of glyphosate hydrolysis slurry, adding 3g of 10% hydrogen peroxide, cooling and crystallizing for 1.8 hours, cooling to 88 ℃, transferring the glyphosate hydrolysis slurry into a centrifugal washing machine, and separating mother liquor to obtain 152g of glyphosate solid. The filtrate (glyphosate mother liquor 1)) was collected in 351 g.
80g of 1.3 percent glyphosate aqueous solution is added to soak and wash the glyphosate solid, 98g of glyphosate solid is obtained after centrifugal separation and filtration. And then 50g of 1.3% glyphosate aqueous solution is added into the material washing machine to soak and wash the glyphosate solid, and 59g of filtrate is separated by centrifugation to obtain 125g of glyphosate solid. After being dried by a drying oven, the obtained glyphosate technical has the main content of 96.6 percent, the average grain diameter of 80 mu m, good technical fluidity and little dust.
Pumping the collected glyphosate mother liquor 1 and 30% potassium hydroxide liquid caustic soda into a pipeline mixer for neutralization, controlling the pH value of the mixed liquor to be 1.2, uniformly adding 0.5g of primary crystal raw medicine as seed crystals, slowly cooling and crystallizing for 6 hours in a two-stage crystallization kettle, transferring into a two-stage material washing device when the temperature of slurry is reduced to be below 30 ℃, and separating the mother liquor by suction filtration to obtain 30g of glyphosate solid and 375g of filtrate (glyphosate mother liquor 2). Adding 39g of the B2 washing solution obtained in example 2, soaking and washing glyphosate solid by water, and centrifugally separating out 46g of filtrate (washing solution B2) to a mother liquor tank; 23g of glyphosate solid was obtained. Drying in a baking oven to obtain glyphosate with the main content of 95.2% and the average particle size of 105 μm, and measuring the glyphosate content in the mother liquor to be 1.43%.
Claims (7)
1. The crystallization method of the glyphosate crystallization device is characterized by comprising the following steps:
(1) first-stage crystallization and solid-liquid separation: transferring the glyphosate hydrolysate in the hydrolysis kettle into a crystallization kettle, adding an auxiliary agent, introducing cooling water into a jacket of the crystallization kettle to cool the slurry to 70-100 ℃, or directly cooling the slurry to 70-100 ℃ in the hydrolysis kettle and adding the auxiliary agent, transferring into a section of material washing device, separating out the mother liquor through suction filtration and centrifugation to obtain glyphosate solid A and glyphosate mother liquor 1, and transferring the glyphosate mother liquor 1 to a mother liquor intermediate tank, wherein the auxiliary agent comprises any one of hydrogen peroxide, sodium hypochlorite, sodium chlorite and sodium chlorate;
(2) first-stage washing: adding a glyphosate aqueous solution into a first-stage material washing device, soaking and washing the glyphosate solid A, dissolving out impurities, performing suction filtration and centrifugal separation to obtain a washing solution B to obtain glyphosate wet powder, and drying to obtain a glyphosate original drug;
(3) primary mother liquor neutralization: carrying out neutralization reaction on the glyphosate mother liquor 1 in the step (1) and an alkaline substance through a pipeline mixer, and adjusting the pH value to be in a range of 0-2.0;
(4) two-stage crystallization, solid-liquid separation and washing: sending the glyphosate mother liquor 1 neutralized in the step (3) to a two-stage crystallization kettle, cooling to 30-40 ℃, crystallizing for 2-7 hours, transferring to a two-stage material washing device when the temperature of the slurry is reduced to below 30 ℃, separating the mother liquor by suction filtration and centrifugation to obtain glyphosate solid B and glyphosate mother liquor 2, washing the glyphosate solid B by using water to obtain glyphosate wet powder, and drying to obtain glyphosate raw drug;
the glyphosate hydrolysis kettle (1) is connected with a first-stage crystallization kettle (2), an auxiliary agent groove (11) is arranged on the first-stage crystallization kettle (2), the first-stage crystallization kettle (2) is connected with a first-stage washing device (3), and the first-stage washing device (3) is connected with a drying tower (6); or the glyphosate hydrolysis kettle (1) is directly connected with the first section of the washing device (3);
one section is washed material device (3) and is connected with one section crystallization kettle (2) and mother liquor intermediate tank (4) respectively, and mother liquor intermediate tank (4) is connected with neutralizer mixer (5), and neutralizer mixer (5) are connected with two sections crystallization kettle (10), and two sections crystallization kettle (10) are connected with two sections washing material device (7), and two sections washing material device (7) are connected with drying tower (6), and drying tower (6) are connected to the former medicine device of glyphosate.
2. The glyphosate crystallization method according to claim 1, wherein the glyphosate hydrolysate in step (1) is glyphosate slurry obtained by hydrolyzing glyphosate by glycine-alkyl ester method under acidic condition, performing acidolysis and removing solvent, and the temperature is 115 +/-15 ℃ and the pH value is below 0.
3. The glyphosate crystallization method according to claim 1, characterized in that glyphosate bulk drug obtained by drying in the step (2) is added to the first-stage crystallization kettle and/or the second-stage crystallization kettle as seed crystal.
4. The method of crystallizing glyphosate according to claim 1, wherein the aqueous glyphosate solution is an aqueous solution having a glyphosate content of 0-3%; the addition amount of the glyphosate aqueous solution is 0.6-2 times (weight ratio) of the solid content in the slurry.
5. The glyphosate crystallization process according to claim 1, wherein an alkaline material feeding pipe (14) is arranged on the neutralization mixer (5), and a water inlet pipe II (15) is arranged on the secondary washing device (7).
6. The glyphosate crystallization process according to claim 1, characterized in that the secondary wash unit (7) is connected to a mother liquor tank (8), and the mother liquor tank (8) is connected to a mother liquor recovery unit (9).
7. The glyphosate crystallization method according to claim 1, characterized in that the first washing device (3) is provided with a glyphosate aqueous solution tank (12) and a water inlet pipe I (13).
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