(:https://www.bloomtechz.com/synthetic-chemical/api-researching-only/acephate-powder-cas-30560-19-1.html) is a pesticide with a long history of use in organic phosphorus pesticides. Its characteristic is that it is an endothermic insecticide with gastric toxicity and contact killing effects, and can kill eggs. It has a certain fumigation effect and is a slow-acting insecticide. Its basic insecticidal principle is to inhibit the insect acetylcholine acetate enzyme. Suitable for vegetables, tobacco, fruit trees, cotton, citrus, rice, and wheat, to prevent and control various chewing and sucking mouthparts pests and pythons. If mixed with pesticides such as carbaryl and dimethoate, it has a synergistic effect and can extend the shelf life.

Metode 1: A enkel, høj udbytte, lave omkostninger, og høj renhed metode til tilberedning acephat; Det kan overvinde den neutralisering proces krævet til separering eddikesyre, reducere nedbrydning tab af acetylmethylamin forårsaget ved neutralisering, og ikke kræve en stor mængde af organisk opløsningsmiddel ekstraktion proces og generere en stor mængde af spildevand. Den tekniske løsning omfatter den følgende syntese reaktion proces:

(1) Brug ethylen keton og O% 2c O-dimethylthiophosphoramid as rå materialer% 2c under betingelserne for acylering katalysator og organisk opløsningsmiddel% 2c ethylen keton gennemgår acetylering reaktion med O% 2c O-dimethylthiophosphoramid til O-dimethylthiophosphoramid% 3b Blandt dem% 2c mass forholdet af ethylen keton til O% 2c O-dimethylthiophosphoramid is (0.15-0.40): 1;

(2) React acetylated O, O-dimethylthiophosphoramid under isomerization catalyst conditions to prepare acetomethamidophos solution;

(3) Acetylmethamidophos solution was crystallized, solid-liquid separated, and dried to prepare Acetylmethamidophos raw powder.

Det kemiske reaktion ligning er som følger:

Metode 2:

De rå materialer til produktion acephat inkluderer methyl chlorid% 2c ammoniak% 2c dichlorethan% 2c ethylen glycol% 2c og dimethyl sulfat eddike. opnået gennem reaktion trin sådan som aminering% 2c acylering% 2c og isomerisering.

1. Amination:

Tilføj methyl chlorid og tilsvarende proportional mængde dichlorethan vandret ind i aminering kedel fra det høje niveau måling % 2c og start den omrøring og frysning saltlage. Når temperaturen i kedlen falder til 15C , langsomt dryp nitrogen vand ind kedlen fra høj niveau måling af ammoniak vand % 2c og temperaturen i kedlen ved % 7b {1% 7d % 7d procent C for 35.4{% 7b9% 7d% 7d min. Efter tilsætning ammoniak vand% 2c juster den frosne saltlage for at reducere temperaturen i kedlen til % 7b% 7b4% 7dC. Oprethold temperaturen og rør for % 7b% 7b5% 7d% 7d minutter% 2c derefter tilføj 6L af vand. Efter omrøring for % 7b{7}% 7d minutter% 2c stop omrøring og pumpe materialet ind i aminering separator for stratificering. Efter 3% 7b% 7b10% 7d% 7d minutter% 2c sted den organiske fase i den modtagende tank til måling. Dette organiske fase er amin forbindelse med opløsningsmiddel (0,0 dimethyl thiophosphoramid).

2. Acylering:

(1) Acetic anhydride method: Put the amine with solvent into the acylation kettle from the high level measuring tank, start stirring, then add acetic anhydride into the acylation kettle from the high level measuring tank of acetic anhydride, and then turn on frozen brine. When the temperature in the kettle drops to 10 degree C, slowly add concentrated sulfuric acid from the high level measuring tank into the reaction kettle. After adding sulfuric acid, turn on air pressure, discharge the frozen brine from the jacket, and slowly heat it with steam to raise the temperature in the kettle to 55-60 degree C, Maintain the reaction for 50 minutes, complete the reaction, and then lower the temperature inside the kettle to 10C. Add chlorine water dropwise from the high level tank of ammonia water to neutralize the acid generated by the reaction, and neutralize it to a pH value of 7-8. During the neutralization process, the temperature should be controlled below 30 degree C. After neutralization, the material should be pumped into a separator for static separation, and the lower organic phase should be separated into the crude acylate storage tank. Then, it should be pumped into the distillation kettle for vacuum distillation and desorption (vacuum degree 86.kPa, 70C, 15-20 minutes), The acylated compound (0,0-dimethyl-N-yl thiophosphoramide) is obtained.

(2) Acetyl chloride method: Place the amine compound with solvent into the acylation kettle from a high-level measuring tank, start stirring, and add acetyl chloride from the high-level measuring tank of ethyl chloride. Then slowly raise the temperature in the reactor to 50 degree C, maintain the temperature for 2 hours, and react more. Reduce the temperature in the reactor to 10 degree C, and then slowly add nitrogen water from the ammonia water high-level measuring tank to neutralize the acid generated by the reaction. Neutralize it to a pH value of 7. During the neutralization process, the temperature in the reactor should be controlled below 30 degree C. After neutralization, add an appropriate amount of water. Dissolve the plating salt generated during the neutralization process, stir for 2-3 minutes, and extract the material to the separator for static separation. Separate the lower organic phase and extract it into a distillation kettle for vacuum desorption (vacuum degree 86.7kPa, 70C, 15-20min) to obtain the compound. The acylation reaction using acetic anhydride or acetyl chloride as the acylating agent can achieve good results.

3. Isomerisering:

Put a quantitative amount of acylated substance into the isomerization kettle from the high-level metering tank of acylated substance, start stirring, and then add dimethyl sulfate vinegar proportionally to the isomerization kettle from the high-level metering tank of dimethyl sulfate vinegar. Slowly raise the temperature to 65-70 degree C, maintain the temperature for 2 hours, and discharge to obtain acephate crude oil. For each production of 1 ton of 50 percent concentration crude oil, the following raw materials are consumed: 1953 kg of methanol (98 percent ), 1660 kg of triple phosphated phosphorus (98 percent ), 120 kg of caustic soda (30 percent ), 3220 kg of dimethyl sulfate (98 percent ), 2450 kg of ammonia (18 percent ), 315 kg of sulfur (98 percent ), 295 kg of acetic acid (98 percent ), 1700 kg of aminated KO (40 percent ), 490 kg of ethylene (69 percent ), and 250 kg of sulfurized (industrial) dichlorane (98 percent ).

Metode 3:

Brug af dimethyl thiophosphat chlorid som det rå materiale% 2c under omrøring% 2c aminering er båret ud med ammoniak vand % 2c efterfulgt af acetylering med eddikesyre anhydrid. acetylering er båret ud i tilstedeværelsen af svovlsyre syre. Under acetylering proces , del af eddikesyre eddikesyre af eddikesyre som derefter neutraliseret med ammoniak. Acetyl chlorid kan også bruges som en acylating agent. Efter acylering% 2c den opløsning er venstre til stå og organisk blandet i det nederste lag. Efter adskillelse% 2c dimethyl sulfat er brugt til isomerisering% 2c efterfulgt af vakuum destillation for at rense produktet , koncentration , og krystallisering til opnå acephat.

[ 1 ] : acephat

Metode 4:

1. Første isomerisering efterfulgt af acylering. Første, i tilstedeværelsen af a lille mængde af dimethyl sulfat, 0, 0-dimethylthiotenamid is opvarmet for isomerisering til generere O, S-dimethylthiotenamid, som derefter reagerer med ethylen eller acetyl chlorid til producere acephat

2. For det første, acylering efterfulgt af isomerisering involverer reaktionen af 0,0-dimethylthioacetamid med a køling middel i a opløsningsmiddel af di-ethan eller benzen. Almindeligt anvendt acylating midler inkluderer eddikesyre plus zink trichlorid, eddike pasta, acetyl chlorid, vinyl keton, etc. Den køling reaktion genererer O, 0-dimethyl-N-ethylthiotenamid, som er er derefter opvarmet og isomeriseret til ethyl methamidophos i den tilstedeværelsen af en lille mængde af dimethyl sulfat.

3. By using new catalysts and special crystalline solvents, high-purity raw materials can be prepared. The process involves adding 200g of methamidophos crude oil to a reaction flask, stirring and heating to the reaction temperature. Under the action of the catalyst, acylating agent acetic acid is added dropwise, and the reaction temperature is controlled. After dropwise addition, the crude crude oil of methamidophos is incubated for several hours, and then neutralized and extracted to separate the organic and aqueous phases, Organic phase purification of acephate refined crude oil is carried out by adding solvent A and crystal forming additives, slowly stirring, cooling, crystallization, filtration, and rinsing to obtain the finished product. After processing the mother liquor, qualified finished products can be recovered, with a total product yield of>78 percent and a content of 298.0 percent .