CN106496215A - The environmental protection synthetic method in high yield of Diacloden - Google Patents
The environmental protection synthetic method in high yield of Diacloden Download PDFInfo
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- CN106496215A CN106496215A CN201610979438.8A CN201610979438A CN106496215A CN 106496215 A CN106496215 A CN 106496215A CN 201610979438 A CN201610979438 A CN 201610979438A CN 106496215 A CN106496215 A CN 106496215A
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- diacloden
- environmental protection
- high yield
- synthetic method
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- NWWZPOKUUAIXIW-DHZHZOJOSA-N (E)-thiamethoxam Chemical compound [O-][N+](=O)/N=C/1N(C)COCN\1CC1=CN=C(Cl)S1 NWWZPOKUUAIXIW-DHZHZOJOSA-N 0.000 title claims abstract description 23
- 230000007613 environmental effect Effects 0.000 title claims abstract description 15
- 238000010189 synthetic method Methods 0.000 title claims abstract description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 36
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 32
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 18
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000003287 bathing Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000006227 byproduct Substances 0.000 claims abstract description 7
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 125000001841 imino group Chemical group [H]N=* 0.000 claims abstract description 7
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 7
- SEEPANYCNGTZFQ-UHFFFAOYSA-N sulfadiazine Chemical compound C1=CC(N)=CC=C1S(=O)(=O)NC1=NC=CC=N1 SEEPANYCNGTZFQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000004821 distillation Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 5
- 238000007710 freezing Methods 0.000 claims abstract description 5
- 239000012452 mother liquor Substances 0.000 claims abstract description 5
- 238000011084 recovery Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 238000013461 design Methods 0.000 claims abstract description 3
- 239000002920 hazardous waste Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 14
- SCYULBFZEHDVBN-UHFFFAOYSA-N 1,1-Dichloroethane Chemical class CC(Cl)Cl SCYULBFZEHDVBN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000012805 post-processing Methods 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- -1 potassium halide Chemical class 0.000 claims description 4
- VRMUIVKEHJSADG-UHFFFAOYSA-N 2-chloro-5-(chloromethyl)-1,3-thiazole Chemical compound ClCC1=CN=C(Cl)S1 VRMUIVKEHJSADG-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 3
- UZAOOCPKYMGRHG-UHFFFAOYSA-N 5-(chloromethyl)-1,3-thiazole Chemical compound ClCC1=CN=CS1 UZAOOCPKYMGRHG-UHFFFAOYSA-N 0.000 abstract 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 239000000460 chlorine Substances 0.000 abstract 1
- 229910052801 chlorine Inorganic materials 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 241000238631 Hexapoda Species 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 210000003298 dental enamel Anatomy 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000001988 toxicity Effects 0.000 description 2
- 231100000419 toxicity Toxicity 0.000 description 2
- MTXSIJUGVMTTMU-JTQLQIEISA-N (S)-anabasine Chemical compound N1CCCC[C@H]1C1=CC=CN=C1 MTXSIJUGVMTTMU-JTQLQIEISA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical compound NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 1
- 108090000371 Esterases Proteins 0.000 description 1
- 239000005906 Imidacloprid Substances 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- 206010033799 Paralysis Diseases 0.000 description 1
- OIPILFWXSMYKGL-UHFFFAOYSA-N acetylcholine Chemical compound CC(=O)OCC[N+](C)(C)C OIPILFWXSMYKGL-UHFFFAOYSA-N 0.000 description 1
- 229960004373 acetylcholine Drugs 0.000 description 1
- 229930014345 anabasine Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- HFNQLYDPNAZRCH-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O.OC(O)=O HFNQLYDPNAZRCH-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- NHSCRWJPZDNMBU-UHFFFAOYSA-L dipotassium carbonic acid carbonate Chemical compound [K+].[K+].OC([O-])=O.OC([O-])=O NHSCRWJPZDNMBU-UHFFFAOYSA-L 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- YWTYJOPNNQFBPC-UHFFFAOYSA-N imidacloprid Chemical compound [O-][N+](=O)\N=C1/NCCN1CC1=CC=C(Cl)N=C1 YWTYJOPNNQFBPC-UHFFFAOYSA-N 0.000 description 1
- 229940056881 imidacloprid Drugs 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 239000003992 organochlorine insecticide Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D417/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00
- C07D417/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00 containing two hetero rings
- C07D417/06—Heterocyclic compounds containing two or more hetero rings, at least one ring having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by group C07D415/00 containing two hetero rings linked by a carbon chain containing only aliphatic carbon atoms
Abstract
The invention discloses a kind of Diacloden in high yield and environmental protection synthetic method：A, weigh 0.5 1.5 parts of imino group diazine, 0.5 1.5 parts of 2 chlorine, 5 5-chloromethyl thiazole, 0.2 2 parts of dimethylformamide, 0.2 2 parts of butanone, 0.2 2 parts of toluene, 0.5 1.5 parts of potassium carbonate, 0.001 0.01 parts of catalyst, put in synthesis reactor and mix, stirring reaction；B, step A products therefrom are warmed up to 30 70 DEG C and add bathing preparation to be embathed, and subsequent centrifugal filtration obtains salinity as side-product, and organic supernatant is sent to crystallization kettle, and freezing and crystallizing is centrifuged to obtain Diacloden solid, and centrifuge mother liquor is sent to solvent recovery column distillation reuse.Selection and proportioning and innovative design to synthesis route and precise control of the present invention by improvement reaction raw materials, have reached higher product yield and have not produced extra hazardous waste.
Description
Technical field
The present invention relates to the Diacloden green synthesis process method of technical field of medicine synthesis, especially environmental protection and energy saving.
Background technology
Diacloden is the anabasine insecticide that is developed by Novartis Co., Ltd in 1991, and its mechanism of action is similar to imidacloprid,
Alternative suppression insect CNS nicotinic acetylcholine esterase receptor, and then block insect CNS
Normal conduction, causes insect to occur dead during paralysis machine.Not only have tag, stomach toxicity, systemic activity, and with higher work
Property, more preferable safety, wider array of insecticidal spectrum and work fast, the features such as the lasting period is long, be to replace those to mammal
Toxicity is high, have residual and environmental problem organophosphors, carbamate, the preferable kind of organochlorine insecticides.Diacloden
In building-up process, at this stage mainly with DMF as solvent, potassium carbonate as acid binding agent, after completion of the reaction, add 5 to 10 times of volumes
Water separates out product, after being then centrifuged for drying, uses methanol solvate recrystallization, and content is 93 to 96%.The advantage of this method is work
Skill is simple, but potassium carbonate of DMF and excess etc. is all untreated, and wastewater flow rate is big, and COD and salinity are also especially high, and environmental protection pressure is huge
Greatly, cause yield low containing a small amount of Diacloden finished product in waste water（76%）.
（Chemosynthesis equation）
The administering method of country's Diacloden waste water is mainly burning method, triple effect evaporation method, big energy-consuming, high cost at present, while giving up
Slag yield is big, increased the cost of burning.
Content of the invention
The technical problem to be solved in the present invention is a variety of deficiencies for overcoming prior art, by improving the selection of reaction raw materials
With proportioning and the innovative design to synthesis route and precise control, there is provided a kind of environmental protection in high yield of Diacloden is closed
Into method, higher yield can be reached and do not produce extra hazardous waste.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows.
Diacloden in high yield and environmental protection synthetic method, comprise the steps：
A, synthetic reaction：Following reaction raw materials are weighed by ratio of weight and the number of copies：Imino group diazine 0.5-1.5 parts, the chloro- 5- chloromethyls of 2-
Thiazole 0.5-1.5 parts, dimethylformamide 0.2-2 parts, butanone 0.2-2 parts, toluene 0.2-2 parts, potassium carbonate 0.5-1.5 parts, urge
Agent 0.001-0.01 part, puts in synthesis reactor and mixes, control synthesis reactor pressure for open normal pressure while temperature is set in
Between 32 DEG C -50 DEG C, stirring reaction 3-6 hour；
B, synthesis post processing：Step A products therefrom is warmed up to 30-70 DEG C and adds bathing preparation to be embathed, and subsequent centrifugal filtration is obtained
Salinity is obtained as side-product, organic supernatant is sent to crystallization kettle, and freezing and crystallizing is carried out under conditions of -10 DEG C -5 DEG C, centrifugation
Diacloden solid, centrifuge mother liquor is sent to solvent recovery column distillation reuse, by rectification can reclaim to toluene, dichloroethanes,
Dimethylformamide, butanone etc. are re-used.
As a preferred technical solution of the present invention, in step A, the dimethylformamide, butanone, toluene three
Consumption weight ratio is 1:（1-3）:（2-4）.
As a preferred technical solution of the present invention, in step A, the catalyst adopts potassium halide, preferentially adopts iodine
Change potassium.
As a preferred technical solution of the present invention, in step B, the bathing preparation adopts dichloroethanes, butanone or two
The mixture of person.
As a preferred technical solution of the present invention, in step B, the weight of the bathing preparation and the imino group diazine
Than for（1-5）:1.
Used as a preferred technical solution of the present invention, the method comprises the steps：
A, synthetic reaction：Following reaction raw materials are weighed by ratio of weight and the number of copies：1 part of imino group diazine, 2- chloro-5-chloromethyl thiazoles 1
Part, 0.5 part of dimethylformamide, 1 part of butanone, toluene 1-1.5 parts, 1 part of potassium carbonate, 0.004 part of catalyst, put into synthesis reactor
In and mix, it is open normal pressure while temperature is set between 45 DEG C to control synthesis reactor pressure, stirring reaction 5 hours；
B, synthesis post processing：Step A products therefrom is warmed up to 35-60 DEG C and adds bathing preparation to be embathed, and subsequent centrifugal filtration is obtained
Salinity is obtained as side-product, organic supernatant is sent to crystallization kettle, carries out freezing and crystallizing, be centrifuged under conditions of -3 DEG C -3 DEG C
Diacloden solid, centrifuge mother liquor are sent to solvent recovery column distillation reuse, by rectification can reclaim to toluene, dichloroethanes, two
Methylformamide, butanone etc. are re-used.
It is using the beneficial effect produced by above-mentioned technical proposal：
The present invention utilizes Diacloden different solubilities in organic solvent, being added in combination for multi-solvent to significantly improve Diacloden
Dissolubility, while having saved the usage amount of acid binding agent, improve reaction conversion ratio, fairly obvious for product yield brought up to
More than 91%（Prior art 76% or so）, and product purity is maintained at more than 98%（Now with regard to technology up to 95% or so）.Its
In, the combination of multi-solvent and consumption proportion are affected less for product purity, but are single use or proportioning is unbalance for product
The impact of product yield is larger, for example, toluene is used alone, and product purity is close to 97%, but yield falls back to a state of the art left side
Right.
Meanwhile, under the combined treatment of multi-solvent, salt slag is substantially insoluble in organic solvent, by a centrifugation, raw
Into salt slag again through rake type drier drying after can be sold as side-product；It can be said that the present invention is using synthesis, dissolving
The effective handling process such as filtration, crystallization, it is achieved that the zero-emission of the waste water in course of reaction.
As fully visible, this technique improves reaction yield and product by the integrated application of multi-solvent and supporting technology means
Product content, at the same more thoroughly solve in waste water generation, solve problem of environmental pollution from source.
Present invention one-time investment in actual production process is larger, but can be with improving production efficiency, especially effectively
Reduce discharge of wastewater, from the point of view of long term productivity especially environmental protection and the ecological value, still there is very high promotional value.
Specific embodiment
Following examples are described in detail the present invention.Various raw materials used in the present invention and items of equipment are conventional city
Product is sold, can be directly obtained by market purchase.
Embodiment 1
The concrete technology step of the preferred embodiments of the present invention is as follows：
1) in dry 3000L enamel stills, 400kg imino group diazines, 200kg dimethylformamides, 400kg fourths are added
Ketone, 400kg toluene, O.5Kg 400kg carbonic acid potassium carbonate, potassium iodide, Deca 400kg2- chloro-5-chloromethyl thiazole;Open and steam
Steam valve door is heated, and controls temperature for temperature 45 C;
2) the equal-volume proportioning mixture of 1000-1200kg dichloroethanes and butanone, slow temperature rise, after reacting 5 hours, are added
To 60 DEG C, 1 hour is incubated, opens bottom valve, material is entered into the separation of automatic centrifugal machine, nitrogen is protected, and filtering residue is transferred to rake
Formula drying machine is dried to obtain salinity side-product；Filtrate is entered in crystallization kettle, decrease temperature crystalline, is incubated in -3 to 3 DEG C of hours,
The separation of automatic centrifugal machine is put into, nitrogen is protected, and solid material is dried with vacuum bipyramid, and solvent can be passed through with condensation process
Rectification is recycled to toluene, dichloroethanes, dimethylformamide, butanone etc.；Mother solution is obtained through concentration, crystallization
16kg products, yield have 76 liftings of prior art to 91%, purity 98%；Discharge of wastewater is by 15 tons of high-concentration waste water/tons simultaneously
Product is reduced to 0.3 ton of low concentration wastewater, flushing waste water etc. of this waste water essentially from workshop.
As a comparison, another kind of processing step that implements in present invention research and development the following is, and its yield advantage is relatively low, but ring
Value of supporting value is still obvious：
1) synthesize：In dry 3000L enamel stills, 400kg imino group diazines, 800kg butanone, 400kg carbonic acid carbonic acid is added
Potassium, O.5Kg catalyst, Deca 400kg2- chloro-5-chloromethyl thiazole;Steam valve heating is opened, and temperature is controlled for temperature 45
℃;
2) dissolving crystallized：After reaction 5 hours, 800kg butanone, slow temperature rise to 60 DEG C is added to be incubated 1 hour, open bottom valve,
Material is entered into the separation of automatic centrifugal machine, nitrogen is protected, filtering residue is transferred to rake type drier drying；Filtrate enters into crystallization
In kettle, decrease temperature crystalline is incubated in -3 to 5 DEG C of hours, puts into the separation of automatic centrifugal machine, and nitrogen is protected, and material is with very
Empty bipyramid is dried, and obtains 15kg products.After this post processing, 81 or so, discharge of wastewater is reduced to 0.3 ton of low concentration to yield
Waste water.
This gives the proportioning of the most effective embodiment of the present invention, wherein each processing step and component can be with micro-
Adjust, within the scope of the present invention.
Claims (6)
1. Diacloden in high yield and environmental protection synthetic method, by improving selection and the proportioning of reaction raw materials, and pairing
Into innovative design and the precise control of process route, reach higher yield and do not produce extra hazardous waste, its feature exists
In：The method comprises the steps：
A, synthetic reaction：Following reaction raw materials are weighed by ratio of weight and the number of copies：Imino group diazine 0.5-1.5 parts, dimethylformamide
0.2-2 parts, butanone 0.2-2 parts, toluene 0.2-2 parts, potassium carbonate 0.5-1.5 parts, catalyst 0.001-0.01 parts, put into synthesis
In kettle and mix, be simultaneously added dropwise 2- chloro-5-chloromethyl thiazole 0.5-1.5 parts, it is open normal pressure while temperature to control synthesis reactor pressure
Degree is set between 32 DEG C -50 DEG C, stirring reaction 3-6 hour；
B, synthesis post processing：Step A products therefrom is warmed up to 30-70 DEG C and adds bathing preparation to be embathed, and subsequent centrifugal filtration is obtained
Salinity is obtained as side-product, organic supernatant is sent to crystallization kettle, and freezing and crystallizing is carried out under conditions of -10 DEG C -5 DEG C, centrifugation
Diacloden solid is obtained, centrifuge mother liquor is sent to solvent recovery column distillation reuse.
2. Diacloden according to claim 1 in high yield and environmental protection synthetic method, it is characterised in that：In step A,
The dimethylformamide, butanone, the consumption weight ratio of toluene three are 1:（1-3）:（2-4）.
3. Diacloden according to claim 1 in high yield and environmental protection synthetic method, it is characterised in that：In step A,
The catalyst adopts potassium halide.
4. Diacloden according to claim 1 in high yield and environmental protection synthetic method, it is characterised in that：In step B,
The bathing preparation adopts dichloroethanes, butanone or the mixture of the two.
5. Diacloden according to claim 1 in high yield and environmental protection synthetic method, it is characterised in that：In step B,
The bathing preparation with the weight ratio of the imino group diazine is（1-5）:1.
6. the Diacloden according to any one of claim 1-5 in high yield and environmental protection synthetic method, it is characterised in that：
The method comprises the steps：
A, synthetic reaction：Following reaction raw materials are weighed by ratio of weight and the number of copies：1 part of imino group diazine, 0.5 part of dimethylformamide,
1 part of butanone, toluene 1-1.5 parts, 1 part of potassium carbonate, 0.004 part of catalyst, put in synthesis reactor and mix, be simultaneously added dropwise 2-
1 part of chloro-5-chloromethyl thiazole, it is open normal pressure while temperature is set between 45 DEG C to control synthesis reactor pressure, and stirring reaction 5 is little
When；
B, synthesis post processing：Step A products therefrom is warmed up to 35-60 DEG C and adds bathing preparation to be embathed, and subsequent centrifugal filtration is obtained
Salinity is obtained as side-product, organic supernatant is sent to crystallization kettle, carries out freezing and crystallizing, be centrifuged under conditions of -3 DEG C -3 DEG C
Diacloden solid, centrifuge mother liquor are sent to solvent recovery column distillation reuse.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108822098A (en) * | 2018-06-29 | 2018-11-16 | 湖北犇星农化有限责任公司 | A kind of preparation method of Diacloden |
| CN111036158A (en) * | 2019-12-28 | 2020-04-21 | 邯郸市瑞田农药有限公司 | 2 chlorine-5 chloromethyl thiazole synthesis reaction system |
| CN115286624A (en) * | 2022-08-04 | 2022-11-04 | 内蒙古犇星化学有限公司 | Preparation method of thiamethoxam |
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|---|---|---|---|---|
| CN108822098A (en) * | 2018-06-29 | 2018-11-16 | 湖北犇星农化有限责任公司 | A kind of preparation method of Diacloden |
| CN111036158A (en) * | 2019-12-28 | 2020-04-21 | 邯郸市瑞田农药有限公司 | 2 chlorine-5 chloromethyl thiazole synthesis reaction system |
| CN115286624A (en) * | 2022-08-04 | 2022-11-04 | 内蒙古犇星化学有限公司 | Preparation method of thiamethoxam |
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| CN106496215B (en) | 2020-04-07 |
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Denomination of invention: High yield green synthesis method of thiamethoxam Effective date of registration: 20230105 Granted publication date: 20200407 Pledgee: Bank of China Limited by Share Ltd. Handan branch Pledgor: Handan Ruitian Pesticide Co.,Ltd. Registration number: Y2023130000005 |
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Denomination of invention: High yield green and environmentally friendly synthesis method of thiamethoxam Granted publication date: 20200407 Pledgee: Bank of China Limited by Share Ltd. Handan branch Pledgor: Handan Ruitian Pesticide Co.,Ltd. Registration number: Y2024980002341 |
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Denomination of invention: High yield green and environmentally friendly synthesis method of thiamethoxam Granted publication date: 20200407 Pledgee: Bank of China Limited by Share Ltd. Handan branch Pledgor: Handan Ruitian Pesticide Co.,Ltd. Registration number: Y2024980005890 |