CN110407871A - Glyphosate crystal device and method for crystallising - Google Patents
Glyphosate crystal device and method for crystallising Download PDFInfo
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- CN110407871A CN110407871A CN201910815615.2A CN201910815615A CN110407871A CN 110407871 A CN110407871 A CN 110407871A CN 201910815615 A CN201910815615 A CN 201910815615A CN 110407871 A CN110407871 A CN 110407871A
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- glyphosate
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- mother liquor
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- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 143
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 143
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 51
- 238000002425 crystallisation Methods 0.000 claims abstract description 47
- 230000008025 crystallization Effects 0.000 claims abstract description 47
- 239000012452 mother liquor Substances 0.000 claims abstract description 45
- 239000002002 slurry Substances 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- 239000010413 mother solution Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 230000007062 hydrolysis Effects 0.000 claims abstract description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- 239000000243 solution Substances 0.000 claims abstract description 9
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 238000002791 soaking Methods 0.000 claims abstract description 5
- 238000001238 wet grinding Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 11
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 claims description 10
- 244000025254 Cannabis sativa Species 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 235000009508 confectionery Nutrition 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 230000032050 esterification Effects 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 3
- 229960002218 sodium chlorite Drugs 0.000 claims description 3
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000005708 Sodium hypochlorite Substances 0.000 claims 1
- -1 alchlor Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000000498 cooling water Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims 1
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000706 filtrate Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 8
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 4
- 239000004471 Glycine Substances 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 229920002472 Starch Polymers 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000002363 herbicidal effect Effects 0.000 description 1
- 239000004009 herbicide Substances 0.000 description 1
- KQPBSBAEBKRAAU-UHFFFAOYSA-N hypochlorous acid;sodium Chemical compound [Na].ClO KQPBSBAEBKRAAU-UHFFFAOYSA-N 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000009261 transgenic effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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 Table
- 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 ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
- C07F9/3804—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
Abstract
The present invention provides glyphosate crystal device and method for crystallising.Auxiliary agent is added in glyphosate hydrolysis slurry, when slurry is reduced to 70~100 DEG C, is transferred to one section and washes material device, filtered, be centrifuged and isolate mother liquor, obtain glyphosate A and glyphosate mother solution 1, glyphosate mother solution 1 goes to mother liquor medial launder；It is washed in material device to one section and glyphosate aqueous solution is added, washing by soaking is carried out to glyphosate A, filtered, be centrifugated out cleaning solution B, obtain glyphosate wet-milling, drying obtains glyphosate technicals；Glyphosate mother solution 1 and alkaline matter by carry out neutralization reaction.This method is crystallized and is cleaned to glyphosate technicals, and crystallization time is greatly shortened, and mother liquor glyphosate content is low, and glyphosate crystal form is good, granularity is moderate, has significant economy, quality and environmental benefit.
Description
Technical field
The invention belongs to glyphosate by using glycine production technical field, specially a kind of glyphosate technicals crystallization and cleaning side
Method.
Background technique
Glyphosate have efficiently, low toxicity, spectrum, raw characteristic of going out, superior performance is global volume of production and marketing maximum and most by joyous
The herbicide met provides wide opportunity for glyphosate with the development of population in the world sharply increased with transgenic technology.
Currently, the mainstream judgement to glyphosate is safety, low toxicity, but query carcinogenic about glyphosate in recent years is had no end to disputes, grass
More stringent requirements are proposed for purity of the Gan Lin major consumers state to glyphosate technicals.Secondly, glyphosate crystal technique exists at present
Defect, conventional indirect process crystallization then have that crystallization time long (generally up to 7 hours), land occupation is big, equipment investment is big, continuously
Method crystallization has that mother liquor glyphosate content is high, raw medicine yield is low.Therefore glyphosate crystal, cleaning, purification techniques are attacked
There is also the demands further increased for pass.
China is the major producing country of glyphosate in the world, and production capacity and yield account for the whole world 70% or so.The production of glyphosate mainstream
Method has 2 kinds, first is that IDA method, second is that with glycine method.In China, glycine method synthesizing glyphosate technique occupies leading position,
Account for about national glyphosate production capacity 75%, actual production 80%.Therefore, constantly improve alkyl esterification method glyphosate production technique for
There is extremely strong realistic meaning for China.The present invention is also exactly in product upgrading upgrading, saving energy, lowering energy consumption and reducing pollutants discharge, ecological ideas hair
Open up the achievement that pilot development is carried out under this background.
Summary of the invention
In view of the problems of the existing technology, the present invention provides the methods and dress of a kind of crystallization of glyphosate technicals and cleaning
It sets, glyphosate slurry is handled using auxiliary agent, while being classified into two sections, slurry is carried out using glyphosate aqueous solution clear
It washes, crystallization time can be shortened, reduce mother liquor amount and glyphosate meltage, avoid occurring outburst On The Nucleation, glyphosate when crystallization
Granularity is good, purity improves, and promotes clean manufacturing.
A kind of device of glyphosate technicals crystallization and cleaning:
A kind of glyphosate crystal device, glyphosate hydrolysis kettle connect with one section of crystallization kettle (or glyphosate hydrolysis kettle directly with one section
Wash the connection of material device), one section of crystallization kettle is washed material device with one section and is connect, and washes material device for one section and connect with drying tower.
One section wash material device connect with mother liquor medial launder, mother liquor medial launder with neutralization mixer connect, neutralization mixer and
Two sections of crystallization kettle connections, two sections of crystallization kettles are washed material device with two sections and are connect.
It can also be by adding alkaline matter to adjust slurry pH value in two sections of crystallization kettles.
It washes material device for two sections to connect with mother liquor tank, mother liquor tank is connect with mother liquor recovering device.Two sections wash material device also with baking
Dry tower connection.
It is provided with auxiliary agent feed pipe on the first degree crystalline kettle, and is connected in auxiliary groove.
Described one section is washed on material device and is provided with the water-soluble liquid bath of glyphosate and water enters pipe one.
Alkaline matter feed pipe is provided on the neutralization mixer.
Described two sections, which are washed, expects that being provided with water on device enters pipe two.
For achieving the above object, the present invention uses following technical method:
(1) one section of crystallization and separation of solid and liquid: glyphosate hydrolyzate in hydrolysis kettle is transferred in crystallization kettle.The logical cooling of crystallization kettle collet
Water cools down to slurry, does not add alkaline matter, and uncomfortable material all in one piece starches pH value, is reduced to 70~100 DEG C to slurry temperature.It can also be straight
It connects when slurry being reduced to 70~100 DEG C in hydrolysis kettle.Then it is transferred to one section and washes material device and the separation such as filtered, be centrifuged
Means isolate mother liquor, obtain glyphosate A and filtrate (glyphosate mother solution 1), and filtrate goes to mother liquor medial launder.
The glyphosate hydrolyzate is that glycine-alkyl esterification method glyphosate is hydrolyzed in acid condition, acidolysis and removed molten
The glyphosate slurry obtained after agent, 115 ± 15 DEG C of temperature, pH value is below 0.
Preferably, auxiliary agent is added in slurry, improves crystallization effect.The auxiliary agent is hydrogen peroxide, alchlor, hypochlorous acid
Sodium, sodium chlorite, sodium chlorate etc. have the substance of oxidisability and peptizaiton.
It is described wash material device and wash material process refer to that the interval such as centrifuge, slot type suction filtration machine washes material device and mode, can also
By be belt vacuum rotary vacuum filter etc. continuously wash material device and in a manner of.
(2) first wash: washing in material device to one section and glyphosate aqueous solution be added, and impregnate to glyphosate A and wash
It washs, dissolves out impurity, then the separation means such as filtered, be centrifuged and isolating cleaning solution B, obtain glyphosate wet-milling, drying obtains grass
Sweet phosphine raw medicine.
The glyphosate aqueous solution is the aqueous solution of glyphosate content 0-3%.
Preferably, the glyphosate aqueous solution sodium ions content is lower than 1000ppm.
The additional amount of the glyphosate aqueous solution is 0.6-2 times (weight ratio) of solid content in slurry.
The glyphosate aqueous solution can be added at one time, and can also be added several times.Preferably, using fresh glyphosate
The cleaning solution that aqueous solution obtains when washing is back to the cleaning for the first time of next batch glyphosate A.Cleaning solution part B goes to mother
Reuse in hydrolysis kettle or crystallization kettle slurry is added in liquid medial launder, part.
(3) one times mother liquor neutralizes: the glyphosate mother solution 1 and alkaline matter of (2) described mother liquor medial launder are through pipe-line mixer
Neutralization reaction is carried out, pH value is adjusted and is adjusted to 0-2.0 range.It can also be by adding alkaline matter to adjust material in two sections of crystallizers
Starch pH value.The alkaline matter refers to any one in sodium hydroxide, potassium hydroxide, potassium carbonate, sodium carbonate and ammonia or organic amine
Kind.
(4) two sections crystallize, are separated by solid-liquid separation, washing material: (3) described neutralization post mother liquor goes to two sections of crystallization kettles, gentle cooling knot
Crystalline substance, crystallization time 2-7 hours.When slurry temperature is reduced to 30 DEG C or less, it is transferred to two sections and washes material device, filtered, be centrifuged equal part
Mother liquor is isolated from means, obtains glyphosate B and filtrate (glyphosate mother solution 2).Glyphosate B is carried out using water
Cleaning, obtains glyphosate wet-milling, drying obtains glyphosate technicals.The ejected wash water obtained using fresh washing material is preferentially back to
Next group slurry is washed, then gained ejected wash water enters mother liquor.
Preferably, a small amount of (2) described one section of crystallization drying gained glyphosate technicals are added as crystal seed, the additive amount of crystal seed
For the 0.01-1% of crystallizer internal solvent quality.
(5) mother liquid disposal: (4) described filtrate (glyphosate mother solution 2) is gone to mother liquor postprocessing working procedures recycling triethylamine and is contained
Phosphorus substance.
Beneficial effect
The present invention provides the method and devices of a kind of glyphosate crystal and cleaning.This method to glyphosate technicals carry out crystallization and
Cleaning, crystallization time shortened to 3 hours or so by 7 hours of traditional handicraft, shortened 50% or more, and crystallization apparatus takes up little area, equipment
It is with low investment.Glyphosate crystal form is good, granularity is moderate, dust is small, and mother liquor glyphosate content also low (0.1-0.2%), has
Significant economy, quality and environmental benefit.
Detailed description of the invention
Fig. 1 is the process flow chart of glyphosate crystal and cleaning.Fig. 2 is glyphosate crystal and cleaning device.Wherein, 1. grass
Sweet phosphine hydrolysis kettle, 2. 1 sections of crystallization kettles, 3. 1 sections are washed material device, 4. mother liquor medial launders, in 5. and mixer, 6. drying towers, and 7.
Two sections are washed material device, 8. mother liquor tanks, 9. mother liquor recovering devices, 10. 2 sections of crystallization kettles, 11. auxiliary grooves, 12. glyphosate aqueous solutions
Slot, 13. water enter pipe one, and 14. alkaline matters enter pipe, and 15. water enter pipe two.
Specific embodiment
Embodiment 1
A kind of glyphosate crystal device, glyphosate hydrolysis kettle 1 are connect with one section of crystallization kettle 2, and one section of crystallization kettle 2 and one section wash material dress
3 connections are set, material device 3 is washed for one section and is connect with drying tower 6；
One section wash material device 3 connect with mother liquor medial launder 4, mother liquor medial launder 4 with neutralization mixer 5 connect, neutralization mixer 5 and
Two sections of crystallization kettles 10 connect, and two sections of crystallization kettles 10 are washed material device 7 with two sections and connect, and wash material device 7 for two sections and connect with drying tower 6；
Drying tower 6 is connect with glyphosate technicals packing device.
It washes material device 7 for two sections to connect with mother liquor tank 8, mother liquor tank 8 is connect with mother liquor recovering device 9, is washed material device 3 for one section and is divided
It is not connect with one section of crystallization kettle 2 and mother liquor medial launder 4.
It is provided with auxiliary groove 11 on one section of crystallization kettle 2, washes on material device 3 for described one section and is provided with glyphosate water
Solution tank 12 and water enter pipe 1.
It is provided with alkaline matter feed pipe 14 on the neutralization mixer 5, washes on material device 7 for described two sections and is provided with
Water enters pipe 2 15.
Embodiment 2
Take glyphosate to hydrolyze slurry 520g, sodium chlorite 0.15%(mass ratio be added), decrease temperature crystalline 30 minutes, it is cooled to 100 DEG C
When, glyphosate slurry is transferred to centrifugation material washing machine, mother liquor is isolated, obtains glyphosate 160g.Collect filtrate (grass it is sweet
Phosphine mother liquor 1)) 360g.
The glyphosate aqueous solution that 80g1.5% is added carries out washing by soaking to glyphosate, is centrifugated out and filters 98g, obtains
To glyphosate 142g.The glyphosate aqueous solution that 60g1.5% is added into material washing machine again, which impregnate to glyphosate, to be washed
It washs, is centrifugated out filtrate 67g, obtain glyphosate 135g.It is dried through baking oven, the main content 96.9% of gained glyphosate technicals,
92 μm of average grain diameter.
The glyphosate mother solution 1 of collection and 32% caustic lye of soda alkali pump are entered into pipe-line mixer, neutralized, control mixing
Liquid pH value 1.1, goes to the gentle decrease temperature crystalline of two sections of crystallization kettles 4 hours, when slurry temperature is reduced to 30 DEG C or less, is transferred to two sections and washes
Expect device, mother liquor is isolated through filtering, obtains glyphosate 35g and filtrate (glyphosate mother solution 2) 362g.30g water is added
Washing by soaking is carried out to glyphosate, is centrifugated out filtrate (cleaning solution B1) 39g；Obtain glyphosate 24g.Through baking oven
Drying, the main content 95.6% of gained glyphosate technicals, 102 μm of average grain diameter, surveying mother liquor glyphosate content is 1.36%.
Embodiment 3
It takes glyphosate to hydrolyze slurry 500g, 10% hydrogen peroxide 3g is added, it is decrease temperature crystalline 1.8 hours, when being cooled to 88 DEG C, grass is sweet
Phosphine slurry is transferred to centrifugation material washing machine, and mother liquor is isolated, and obtains glyphosate 152g.Collect to obtain filtrate (glyphosate mother solution 1))
351g。
The glyphosate aqueous solution that 80g1.3% is added carries out washing by soaking to glyphosate, is centrifugated out and filters 98g, obtains
To glyphosate 134g.The glyphosate aqueous solution that 50g1.3% is added into material washing machine again, which impregnate to glyphosate, to be washed
It washs, is centrifugated out filtrate 59g, obtain glyphosate 125g.It is dried through baking oven, the main content 96.6% of gained glyphosate technicals,
80 μm of average grain diameter, raw medicine good fluidity, dust are small.
The glyphosate mother solution 1 of collection and 30% potassium hydroxide solution alkali pump are entered into pipe-line mixer, neutralized, control mixing
Liquid pH value 1.2 is uniformly added into one section of crystallization raw medicine 0.5g as crystal seed, goes to the gentle decrease temperature crystalline of two sections of crystallization kettles 6 hours, material
When slurry temperature degree is reduced to 30 DEG C or less, it is transferred to two sections and washes material device, isolate mother liquor through filtering, obtain glyphosate 30g
With filtrate (glyphosate mother solution 2) 375g.The obtained B2 cleaning solution of 39g embodiment 2 is added, water impregnates glyphosate
Washing, is centrifugated out filtrate (cleaning solution B2) 46g, goes to mother liquor tank；Obtain glyphosate 23g.It is dried through baking oven, gained
The main content 95.2% of glyphosate technicals, 105 μm of average grain diameter, surveying mother liquor glyphosate content is 1.43%.
Claims (9)
1. a kind of glyphosate crystal device, which is characterized in that glyphosate hydrolysis kettle (1) is connect with one section of crystallization kettle (2), one section of knot
Brilliant kettle (2) is washed material device (3) with one section and is connect, and washes material device (3) for one section and connect with drying tower (6)；Or glyphosate hydrolysis kettle (1)
Material device (3) is directly washed with one section to connect；
It washes material device (3) for one section to connect with mother liquor medial launder (4), mother liquor medial launder (4) is connect with mixer (5) are neutralized, and is neutralized
Mixer (5) is connect with two sections of crystallization kettles (10), and two sections of crystallization kettles (10) are washed material device (7) with two sections and connect, and two sections are washed material dress
(7) are set to connect with drying tower (6)；
Drying tower (6) is connected to glyphosate technicals device.
2. glyphosate crystal device according to claim 1, which is characterized in that two sections are washed material device (7) and mother liquor tank (8)
Connection, mother liquor tank (8) are connect with mother liquor recovering device (9).
3. glyphosate crystal device according to claim 1, which is characterized in that be arranged on the first degree crystalline kettle (2)
Have auxiliary groove (11), washes on material device (3) for described one section and be provided with the water-soluble liquid bath of glyphosate (12) and water enters pipe one (13)；
Material device (3) is washed for one section to connect with one section of crystallization kettle (2) and mother liquor medial launder (4) respectively.
4. glyphosate crystal device according to claim 1, which is characterized in that be arranged on the neutralization mixer (5)
Have alkaline matter feed pipe (14), washes for described two sections and expect that being provided with water on device (7) enters pipe two (15).
5. the method for crystallising carried out using the described in any item glyphosate crystal devices of claim 1-4, which is characterized in that including
Following steps:
(1) one section of crystallization and separation of solid and liquid: glyphosate hydrolyzate in hydrolysis kettle is transferred in crystallization kettle, and auxiliary agent, crystallization kettle is added
When the logical cooling water of collet is reduced to 70~100 DEG C to slurry, or slurry is directly cooled to 70-100 DEG C in hydrolysis kettle
And auxiliary agent is added, it is transferred to one section and washes material device, filtered, be centrifuged and isolate mother liquor, obtain glyphosate A and glyphosate is female
Liquid 1, glyphosate mother solution 1 go to mother liquor medial launder；
(2) first wash: washing in material device to one section and glyphosate aqueous solution be added, and carries out washing by soaking to glyphosate A, molten
Impurity out, then filtered, be centrifugated out cleaning solution B, glyphosate wet-milling is obtained, drying obtains glyphosate technicals；
(3) mother liquors neutralize: by step (1) glyphosate mother solution 1 and alkaline matter through pipe-line mixer neutralize it is anti-
It answers, adjusts pH value and be adjusted to 0-2.0 range；
(4) two sections crystallize, are separated by solid-liquid separation, washing material: the glyphosate mother solution 1 after step (3) are neutralized goes to two sections of crystallization kettles, through dropping
Temperature is to 30-40 DEG C, crystallization time 2-7 hours, when slurry temperature is reduced to 30 DEG C or less, is transferred to two sections and washes material device, filtered,
Mother liquor is isolated in centrifugation, is obtained glyphosate B and glyphosate mother solution 2, is cleaned, obtained to glyphosate B using water
To glyphosate wet-milling, drying obtains glyphosate technicals.
6. glyphosate crystal method according to claim 5, which is characterized in that glyphosate hydrolyzate described in step (1)
It hydrolyzed in acid condition for glycine-alkyl esterification method glyphosate, acidolysis and remove the glyphosate slurry obtained after solvent, temperature
115 ± 15 DEG C of degree, pH value is below 0.
7. glyphosate crystal method according to claim 5, which is characterized in that auxiliary agent as described in step (1) includes double
Oxygen water, alchlor, sodium hypochlorite, sodium chlorite, any one in sodium chlorate.
8. glyphosate crystal method according to claim 5, which is characterized in that the grass of drying gained described in step (2) is sweet
Phosphine raw medicine is added to one section of crystallization kettle and/or two sections of crystallization kettles as crystal seed.
9. glyphosate crystal method according to claim 5, which is characterized in that the glyphosate aqueous solution contains for glyphosate
Measure the aqueous solution of 0-3%；The additional amount of the glyphosate aqueous solution is 0.6-2 times (weight ratio) of solid content in slurry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910815615.2A CN110407871B (en) | 2019-08-30 | 2019-08-30 | Glyphosate crystallization device and crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910815615.2A CN110407871B (en) | 2019-08-30 | 2019-08-30 | Glyphosate crystallization device and crystallization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110407871A true CN110407871A (en) | 2019-11-05 |
| CN110407871B CN110407871B (en) | 2022-04-08 |
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| CN201910815615.2A Active CN110407871B (en) | 2019-08-30 | 2019-08-30 | Glyphosate crystallization device and crystallization method |
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| CN110407871B (en) | 2022-04-08 |
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