CN112979729A - Production process method of emamectin benzoate B2 technical - Google Patents
Production process method of emamectin benzoate B2 technical Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 12
- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](NC)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 title abstract 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 230000003647 oxidation Effects 0.000 claims abstract description 38
- 238000006467 substitution reaction Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000005086 pumping Methods 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 14
- IBSREHMXUMOFBB-JFUDTMANSA-N 5u8924t11h Chemical compound O1[C@@H](C)[C@H](O)[C@@H](OC)C[C@@H]1O[C@@H]1[C@@H](OC)C[C@H](O[C@@H]2C(=C/C[C@@H]3C[C@@H](C[C@@]4(O3)C=C[C@H](C)[C@@H](C(C)C)O4)OC(=O)[C@@H]3C=C(C)[C@@H](O)[C@H]4OC\C([C@@]34O)=C/C=C/[C@@H]2C)/C)O[C@H]1C.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 IBSREHMXUMOFBB-JFUDTMANSA-N 0.000 claims abstract description 13
- 239000005660 Abamectin Substances 0.000 claims abstract description 13
- 229950008167 abamectin Drugs 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 13
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 238000004806 packaging method and process Methods 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000010511 deprotection reaction Methods 0.000 claims abstract description 6
- TXFOLHZMICYNRM-UHFFFAOYSA-N dichlorophosphoryloxybenzene Chemical compound ClP(Cl)(=O)OC1=CC=CC=C1 TXFOLHZMICYNRM-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 39
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 25
- 238000005576 amination reaction Methods 0.000 claims description 22
- GCKZANITAMOIAR-XWVCPFKXSA-N dsstox_cid_14566 Chemical compound [O-]C(=O)C1=CC=CC=C1.C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H]([NH2+]C)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 GCKZANITAMOIAR-XWVCPFKXSA-N 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 10
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- 238000005070 sampling Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 239000006227 byproduct Substances 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 6
- 239000005711 Benzoic acid Substances 0.000 claims description 5
- 235000010233 benzoic acid Nutrition 0.000 claims description 5
- 239000012141 concentrate Substances 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 238000000605 extraction Methods 0.000 claims description 5
- 239000012362 glacial acetic acid Substances 0.000 claims description 5
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000010865 sewage Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- QQKDTTWZXHEGAQ-UHFFFAOYSA-N propyl carbonochloridate Chemical compound CCCOC(Cl)=O QQKDTTWZXHEGAQ-UHFFFAOYSA-N 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000749 insecticidal effect Effects 0.000 abstract description 3
- 231100000053 low toxicity Toxicity 0.000 abstract description 3
- 229920000742 Cotton Polymers 0.000 abstract description 2
- 241000607479 Yersinia pestis Species 0.000 abstract description 2
- 235000013399 edible fruits Nutrition 0.000 abstract description 2
- 235000013311 vegetables Nutrition 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- QOSMNYMQXIVWKY-UHFFFAOYSA-N Propyl levulinate Chemical compound CCCOC(=O)CCC(C)=O QOSMNYMQXIVWKY-UHFFFAOYSA-N 0.000 description 1
- AOGYCOYQMAVAFD-UHFFFAOYSA-N chlorocarbonic acid Chemical compound OC(Cl)=O AOGYCOYQMAVAFD-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000017105 transposition Effects 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/08—Hetero rings containing eight or more ring members, e.g. erythromycins
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
Abstract
The invention relates to a process for preparing emamectin benzoate B2 technical raw material, which comprises the steps of adding abamectin B2 and dichloromethane into a 2T reaction kettle, heating up for concentration, vacuumizing, adding dichloromethane, cooling, performing substitution reaction, pumping tetramethyl ethylenediamine and dimethyl sulfoxide after the substitution is qualified, slowly dripping phenyl dichlorophosphate for oxidation reaction, performing oxidation liquid post-treatment, performing deprotection, adjusting acid and alkali, concentrating, crushing and packaging. The invention is an improvement based on emamectin benzoate process, produces derivatives different from emamectin benzoate according to different structures of abamectin, reduces time and dosage of acid and alkali compared with the emamectin benzoate process, simultaneously improves the yield of the oxidation liquid, has the characteristics of simplified process, less consumption of auxiliary materials, low production cost, high yield of the oxidation liquid, good insecticidal effect, low toxicity, low residue and no public nuisance, and can be widely used for controlling various pests of crops such as vegetables, fruit trees, cotton and the like.
Description
Technical Field
The invention relates to a production process method of emamectin benzoate B2 technical.
Background
The emamectin benzoate B2 is found in a finished product spectrogram of the emamectin benzoate, usually, the emamectin benzoate B2 is ignored as a byproduct or impurity, the emamectin benzoate B2 is not well and fully utilized, production resources are greatly wasted, the insecticidal effect of the emamectin benzoate B2 is equal to that of the emamectin benzoate, the price is low, the emamectin benzoate B is deeply favored by customers, but no mature production process exists at present in the emamectin benzoate B2, and therefore the emamectin benzoate B2 cannot be popularized and popularized.
Disclosure of Invention
The invention aims to overcome the defects and provide a production process method of emamectin benzoate B2 technical, which has the advantages of simple process, short production period, low cost, high yield, low toxicity and low residue. The technical scheme includes that a, substitution reaction is achieved, 400 kg-600 kg of abamectin B2 and 1100L-1600L of dichloromethane are added into a 2T reaction kettle, the temperature is raised to 50-60 ℃ for concentration, then the pressure is reduced to-0.8-1 MPA, after materials are dried by distillation, the materials are vacuumized for half an hour, 1100L-1600L of dichloromethane are added, after the materials are completely dissolved, substitution reaction is carried out after the moisture is measured to be less than or equal to 500PPM, the materials are cooled after entering the substitution reaction kettle, 50 kg-60 kg of chloroformic acid diluted propyl ester is pumped in when the temperature is less than or equal to-30 ℃, transposition is carried out for half an hour, 60 kg-70 kg of tetramethyl ethylenediamine is slowly dripped at the temperature of-20 ℃ to-30 ℃, the dripping time is 4-5 hours, analysis sampling is carried out after dripping is finished, the abamectin B2 is detected, and the residual content is less than or;
b. performing oxidation reaction, controlling the temperature to be-20 ℃ -30 ℃ after the substitution is qualified, pumping 60 kg-70 kg of tetramethylethylenediamine and 70 kg-80 kg of dimethyl sulfoxide, slowly dropwise adding 70 kg-80 kg of phenyl dichlorophosphate for 4-5 hours, controlling the dropwise adding temperature to be-15 ℃ -20 ℃, preserving the heat for 1 hour after the dropwise adding is finished, analyzing and detecting, wherein the substitution residue is not more than 2% which is qualified;
c. after the oxidation liquid is subjected to post-treatment, 1000L of water and 500L of dichloromethane are prepared in an oxidation termination kettle, after the oxidation is qualified, the feed liquid is pumped into the oxidation termination kettle, stirred for 30 minutes and stood for 2 hours, an oil phase is separated after the standing is finished, water phase extraction and oil phase combination are carried out, the oil phase is concentrated to remove water, the water content is less than or equal to 500PPM and qualified, and the feed liquid is discharged into a sewage treatment plant after the amination is carried out, and the water phase is; d. after amination and the moisture of the oxidation liquid is qualified, pumping the oxidation liquid into an amination kettle, cooling the oxidation liquid to be less than or equal to minus 10 ℃, pumping 100kg to 110kg of catalyst glacial acetic acid, slowly dropwise adding 95kg to 100kg of monomethylamine, keeping the dropwise adding temperature at 0 ℃ to minus 5 ℃, keeping the temperature for 3 hours to 4 hours after dropwise adding, and carrying out sampling detection after 2 hours of heat preservation is carried out after the dropwise adding is finished, wherein the raw material is qualified when the content of the raw material is less than or equal;
e. reducing and deprotecting, and after amination is qualified, reducing the temperature of a feed liquid to less than or equal to-10 ℃, adding 200L of methanol and 300-500 g of palladium tetrakis (triphenylphosphine) as a catalyst, slowly adding 30-40 kg of sodium borohydride, controlling the temperature to be between-5 ℃ and 5 ℃, feeding for 10-11 hours, preserving heat for 1 hour after feeding is finished, and determining that less than or equal to 1 percent of the raw material is qualified;
f. adjusting acid and alkali, concentrating, crushing, packaging, terminating the reaction by using 600L-700L of acetic acid after deprotection is qualified, removing redundant byproducts, adjusting the pH value of 7-8 by using 500L-600L of liquid alkali, standing for 1 hour, separating an oil phase to concentrate into salt, extracting a water phase twice, combining the water phase with an oil phase, adding 50kg of benzoic acid before concentrating the oil phase, concentrating to be viscous, performing decompression and desolventization for 10-20 minutes, then discharging the materials into an oven, drying the materials for 7-8 hours, crushing and packaging after drying.
The following table shows some of the finished product specifications
The invention is an improvement based on emamectin benzoate process, produces derivatives different from emamectin benzoate according to different structures of abamectin, reduces time and dosage of acid and alkali compared with the emamectin benzoate process, simultaneously improves the yield of the oxidation liquid, has the characteristics of simplified process, less consumption of auxiliary materials, low production cost, high yield of the oxidation liquid, good insecticidal effect, low toxicity, low residue and no public nuisance, and can be widely used for controlling various pests of crops such as vegetables, fruit trees, cotton and the like.
Description of the drawings:
FIG. 1 shows a qualified substitution reaction spectrum of the remaining < 2% of the emamectin benzoate B2 technical product.
FIG. 2 shows a qualified oxidation reaction spectrum of emamectin benzoate B2 instead of the rest of 2%.
FIG. 3 shows that the qualified oxidation reaction spectrogram contains not more than 5% of raw materials of emamectin benzoate B2.
FIG. 4 shows an oxidation reaction spectrum of qualified raw materials with a residual content of 1% or less in the production process of emamectin benzoate B2.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1, best mode
a. A substitution reaction, namely adding 400kg of abamectin B2 and 1100L of dichloromethane into a 2T reaction kettle, heating to 50 ℃ for concentration, then reducing the pressure to 0.8MPA, evaporating the materials to dryness, vacuumizing for half an hour, adding 1100L of dichloromethane, after completely dissolving, carrying out substitution reaction after measuring the water content to be less than or equal to 500PPM, cooling the materials after entering the substitution reaction kettle, cooling to the temperature of less than or equal to-30 ℃, pumping 50kg of dilute propyl chloroformate, shifting for half an hour, slowly dripping 60kg of tetramethylethylenediamine at the temperature of-20 ℃, carrying out analysis sampling after dripping for 4 hours, detecting the abamectin B2, and determining that the residual content is less than or equal to 2 percent;
b. performing oxidation reaction, controlling the temperature to be-20 ℃ after the substitution is qualified, pumping 60kg of tetramethylethylenediamine and 70kg of dimethyl sulfoxide, slowly dropwise adding 70kg of phenyl dichlorophosphate, controlling the dropwise adding time to be 4 hours, controlling the dropwise adding temperature to be-15 ℃, preserving the temperature for 1 hour after the dropwise adding is finished, analyzing and detecting, and determining that the substitution residue is not more than 2 percent to be qualified;
c. after the oxidation liquid is subjected to post-treatment, 1000L of water and 500L of dichloromethane are prepared in an oxidation termination kettle, after the oxidation is qualified, the feed liquid is pumped into the oxidation termination kettle, stirred for 30 minutes and stood for 2 hours, an oil phase is separated after the standing is finished, water phase extraction and oil phase combination are carried out, the oil phase is concentrated to remove water, the water content is less than or equal to 500PPM and qualified, and the feed liquid is discharged into a sewage treatment plant after the amination is carried out, and the water phase is;
d. after amination and the moisture of the oxidation liquid is qualified, pumping the oxidation liquid into an amination kettle, cooling the oxidation liquid to less than or equal to-10 ℃, pumping 100kg of catalyst glacial acetic acid, slowly dropwise adding 95kg of monomethylamine, keeping the dropwise adding temperature at 0 ℃, keeping the dropwise adding time for 3 hours, preserving the temperature for 2 hours after the dropwise adding is finished, and carrying out sampling detection, wherein the raw material is qualified when the content is less than or equal to 5%;
e. reducing and deprotecting, and after amination is qualified, reducing the temperature of the feed liquid to less than or equal to-10 ℃, adding 200L of methanol and 300g of palladium tetrakis (triphenylphosphine) as a catalyst, slowly adding 30kg of sodium borohydride, controlling the temperature to be-5 ℃, feeding for 10 hours, preserving heat for 1 hour after feeding is finished, and determining that less than or equal to 1 percent of the raw material is qualified;
f. adjusting acid and alkali, concentrating, crushing, packaging, terminating the reaction by using 600L of acetic acid after deprotection is qualified, removing redundant byproducts, adjusting the pH to 7-8 by using 500L of liquid alkali, standing for 1 hour, separating oil phases to concentrate into salt, extracting a water phase twice, combining the water phase with an oil phase, adding 50kg of benzoic acid before the oil phase is concentrated to be viscous, decompressing and desolventizing for 10 minutes after the oil phase is concentrated to be viscous, then discharging the materials into an oven, drying the materials for 7 hours, crushing and packaging after drying;
example 2, a, substitution reaction, adding 500kg of abamectin B2 and 1300L of dichloromethane into a 2T reaction kettle, heating to 55 ℃ for concentration, reducing the pressure to 0.9MPA, evaporating the material to dryness, vacuumizing for half an hour, adding 1400L of dichloromethane, after the materials are completely dissolved, measuring the moisture content to be less than or equal to 500PPM, carrying out substitution reaction, cooling the material after entering the substitution reaction kettle, cooling to less than or equal to-30 ℃, pumping 55kg of dilute propyl chloroformate, shifting for half an hour, slowly dropping 65kg of tetramethylethylenediamine at-25 ℃, the dropping time is 4.5 hours, analyzing and sampling after the dropping is finished, detecting abamectin B2, and determining that the residual content is less than or equal to 2 percent;
b. performing oxidation reaction, controlling the temperature to be-25 ℃ after the substitution is qualified, pumping 65kg of tetramethylethylenediamine and 75kg of dimethyl sulfoxide, slowly dropwise adding 75kg of phenyl dichlorophosphate, controlling the dropwise adding time to be 4.5 hours, controlling the dropwise adding temperature to be-17 ℃, preserving the temperature for 1 hour after the dropwise adding is finished, analyzing and detecting, and determining that the substitution residue is not more than 2 percent to be qualified;
c. after the oxidation liquid is subjected to post-treatment, 1000L of water and 500L of dichloromethane are prepared in an oxidation termination kettle, after the oxidation is qualified, the feed liquid is pumped into the oxidation termination kettle, stirred for 30 minutes and stood for 2 hours, an oil phase is separated after the standing is finished, water phase extraction and oil phase combination are carried out, the oil phase is concentrated to remove water, the water content is less than or equal to 500PPM and qualified, and the feed liquid is discharged into a sewage treatment plant after the amination is carried out, and the water phase is;
d. after the water content of the amination and oxidation liquid is qualified, pumping the amination liquid into an amination kettle, cooling the oxidation liquid to less than or equal to-10 ℃, pumping 100kg of catalyst glacial acetic acid, slowly dropwise adding 100kg of monomethylamine, keeping the dropwise adding temperature at-3 ℃, keeping the dropwise adding time for 3.5 hours, preserving the temperature for 2 hours after the dropwise adding is finished, and carrying out sampling detection, wherein the raw material is qualified when the content is less than or equal to 5%;
e. reducing and deprotecting, and after amination is qualified, reducing the temperature of the feed liquid to less than or equal to-10 ℃, adding 200L of methanol and 400g of palladium tetrakis (triphenylphosphine) as a catalyst, slowly adding 35kg of sodium borohydride, controlling the temperature at 2 ℃, feeding for 10 hours, preserving heat for 1 hour after feeding is finished, and determining that less than or equal to 1 percent of the raw material is qualified;
f. adjusting acid and alkali, concentrating, crushing and packaging, terminating the reaction by using 650L of acetic acid after deprotection is qualified, removing redundant byproducts, adjusting the pH to 7-8 by using 550L of liquid alkali, standing for 1 hour, separating oil phases to concentrate into salt, extracting a water phase twice, combining the water phase with an oil phase, adding 50kg of benzoic acid before the oil phase is concentrated to be viscous, decompressing and desolventizing for 15 minutes after the oil phase is concentrated to be viscous, then discharging the materials into an oven, drying the materials for 7.5 hours, crushing and packaging after drying;
example 3, a, substitution reaction, adding 600kg of abamectin B2 and 1600L of dichloromethane into a 2T reaction kettle, heating to 60 ℃ for concentration, reducing the pressure to 1MPA, evaporating the material to dryness, vacuumizing for half an hour, adding 1600L of dichloromethane, after completely dissolving, measuring the moisture content to be less than or equal to 500PPM, performing substitution reaction, cooling the material after entering the substitution reaction kettle, cooling to less than or equal to-30 ℃, pumping in 60kg of dilute propyl chloroformate, shifting for half an hour, slowly dropping 70kg of tetramethylethylenediamine at-30 ℃, performing analysis sampling detection on abamectin B2 after dropping for 5 hours, and determining that the residual content is less than or equal to 2 percent;
b. performing oxidation reaction, controlling the temperature to be-30 ℃ after the substitution is qualified, pumping 70kg of tetramethylethylenediamine and 80kg of dimethyl sulfoxide, slowly dropwise adding 80kg of phenyl dichlorophosphate, controlling the dropwise adding time to be 5 hours, controlling the dropwise adding temperature to be-20 ℃, preserving the temperature for 1 hour after the dropwise adding is finished, analyzing and detecting, and determining that the substitution residue is not more than 2 percent to be qualified;
c. after the oxidation liquid is subjected to post-treatment, 1000L of water and 500L of dichloromethane are prepared in an oxidation termination kettle, after the oxidation is qualified, the feed liquid is pumped into the oxidation termination kettle, stirred for 30 minutes and stood for 2 hours, an oil phase is separated after the standing is finished, water phase extraction and oil phase combination are carried out, the oil phase is concentrated to remove water, the water content is less than or equal to 500PPM and qualified, and the feed liquid is discharged into a sewage treatment plant after the amination is carried out, and the water phase is; d. after the water content of the amination and oxidation liquid is qualified, pumping the amination liquid into an amination kettle, cooling the oxidation liquid to less than or equal to-10 ℃, pumping a catalyst of glacial acetic acid of 110kg, slowly dropwise adding monomethylamine of 100kg, wherein the dropwise adding temperature is at-5 ℃, the dropwise adding time is 4 hours, after the dropwise adding is finished, preserving the heat for 2 hours, and carrying out sampling detection, wherein the raw material of less than or equal to 5 percent is qualified;
e. reducing and deprotecting, and after amination is qualified, reducing the temperature of the feed liquid to less than or equal to-10 ℃, adding 200L of methanol and 500g of palladium tetrakis (triphenylphosphine) as a catalyst, slowly adding 40kg of sodium borohydride, controlling the temperature at 5 ℃, feeding for 11 hours, preserving heat for 1 hour after feeding is finished, and determining that less than or equal to 1 percent of the raw material is qualified;
f. adjusting acid and alkali, concentrating, crushing, packaging, terminating the reaction by using 700L of acetic acid after deprotection is qualified, removing redundant byproducts, adjusting the pH to 7-8 by using 600L of liquid alkali, standing for 1 hour, separating oil phases to concentrate into salt, extracting a water phase twice, combining the water phase with an oil phase, adding 50kg of benzoic acid before the oil phase is concentrated to be viscous, decompressing and desolventizing for 20 minutes after the oil phase is concentrated to be viscous, then discharging the materials into an oven, drying the materials for 8 hours, crushing and packaging.
Claims (1)
1. A production process method of emamectin benzoate B2 technical is characterized by comprising the following steps:
a. performing substitution reaction, namely adding 400 kg-600 kg of abamectin B2 and 1100L-1600L of dichloromethane into a 2T reaction kettle, heating to 50-60 ℃ for concentration, then decompressing to-0.8-1 MPA, evaporating the materials, vacuumizing for half an hour, adding 1100L-1600L of dichloromethane, after the materials are completely dissolved, performing substitution reaction after the water content is measured to be less than or equal to 500PPM, cooling the materials after the materials enter a substitution reaction kettle, cooling to the temperature of less than or equal to-30 ℃, pumping 50 kg-60 kg of dilute propyl chloroformate, indexing for half an hour, slowly dripping 60 kg-70 kg of tetramethylethylenediamine at the temperature of-20 ℃ to-30 ℃, performing analysis sampling after dripping for 4-5 hours, detecting abamectin B2, and determining that the residual content is less than or equal to 2 percent to be qualified;
b. performing oxidation reaction, controlling the temperature to be-20 ℃ -30 ℃ after the substitution is qualified, pumping 60 kg-70 kg of tetramethylethylenediamine and 70 kg-80 kg of dimethyl sulfoxide, slowly dropwise adding 70 kg-80 kg of phenyl dichlorophosphate for 4-5 hours, controlling the dropwise adding temperature to be-15 ℃ -20 ℃, preserving the heat for 1 hour after the dropwise adding is finished, analyzing and detecting, wherein the substitution residue is not more than 2% which is qualified;
c. after the oxidation liquid is subjected to post-treatment, 1000L of water and 500L of dichloromethane are prepared in an oxidation termination kettle, after the oxidation is qualified, the feed liquid is pumped into the oxidation termination kettle, stirred for 30 minutes and stood for 2 hours, an oil phase is separated after the standing is finished, water phase extraction and oil phase combination are carried out, the oil phase is concentrated to remove water, the water content is less than or equal to 500PPM and qualified, and the feed liquid is discharged into a sewage treatment plant after the amination is carried out, and the water phase is;
d. after amination and the moisture of the oxidation liquid is qualified, pumping the oxidation liquid into an amination kettle, cooling the oxidation liquid to be less than or equal to minus 10 ℃, pumping 100kg to 110kg of catalyst glacial acetic acid, slowly dropwise adding 95kg to 100kg of monomethylamine, keeping the dropwise adding temperature at 0 ℃ to minus 5 ℃, keeping the temperature for 3 hours to 4 hours after dropwise adding, and carrying out sampling detection after 2 hours of heat preservation is carried out after the dropwise adding is finished, wherein the raw material is qualified when the content of the raw material is less than or equal;
e. reducing and deprotecting, and after amination is qualified, reducing the temperature of a feed liquid to less than or equal to-10 ℃, adding 200L of methanol and 300-500 g of palladium tetrakis (triphenylphosphine) as a catalyst, slowly adding 30-40 kg of sodium borohydride, controlling the temperature to be between-5 ℃ and 5 ℃, feeding for 10-11 hours, preserving heat for 1 hour after feeding is finished, and determining that less than or equal to 1 percent of the raw material is qualified;
f. adjusting acid and alkali, concentrating, crushing, packaging, terminating the reaction by using 600L-700L of acetic acid after deprotection is qualified, removing redundant byproducts, adjusting the pH value of 7-8 by using 500L-600L of liquid alkali, standing for 1 hour, separating an oil phase to concentrate into salt, extracting a water phase twice, combining the water phase with an oil phase, adding 50kg of benzoic acid before concentrating the oil phase, concentrating to be viscous, performing decompression and desolventization for 10-20 minutes, then discharging the materials into an oven, drying the materials for 7-8 hours, crushing and packaging after drying.
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