Cartap environment-friendly type preparing method

Abstract

The invention discloses an environmental protection preparation method for cartap hydrochloride; rhodanide solution, water and catalyst are arranged inside a reactor, and chlorine hydride gas is input in the reactor for hydrolysis reaction for 15 to 24 hours under -18 to 25 DEG C, so that the cartap hydrochloride can be produced. The hydrolysis processing technique of the invention firstly adopts a hydrolyst method instead of a methyl alcohol alcoholysis for solving the problems of the exhaust gas and waste water from the prior processing technique, furthermore, the hydrolysis rate can reach 95 percent, the quality stability of the cartap hydrochloride product is good, and the processing to the recovery solvent and the mother liquor has unparalleled advantages than the prior art, which fully embodies the call of nation on energy saving and pollutants discharge reduction, thereby the invention has a great social and economic efficiency.

Description

technical field

[0001] The invention belongs to the field of agricultural insecticides, and in particular relates to a preparation method of a nereistin derivative bionic insecticide. Background technique

[0002] Nereistin derivatives are a class of high-efficiency, low-toxicity, broad-spectrum biomimetic insecticides, such as dimehydramine, cyclodime, dimehypo, dimehypo, monosultap, cartap, etc. In the 1970s, China began to develop nereist poison biomimetic insecticides, which have been industrially produced and widely used, mainly including three varieties of dimehypo, monosultap and cartap.

[0003] The classic synthetic method of cartap is to use dimehypo as the starting material, react with sodium cyanide to generate thiocyanide and sodium sulfite, then dissolve the thiocyanide in methanol solvent, and introduce hydrogen chloride gas to generate thiocyanide Dan and by-product chloromethane gas (see "Pesticide Synthesis and Application" edited by Chen Wanyi, Chemical I...

Examples

Embodiment 1

[0024] The ethylene dichloride solution (mass content is 25%) of the thiocyanide of 0.2mol and the water of 2.8mol, 0.5g benzyl trioctyl ammonium chloride catalyst are placed in reactor together, pass into hydrogen chloride gas then, The feed rate is 0.35mol, the reaction temperature is controlled at 20°C, and the hydrolysis reaction is carried out for 20 hours, and the reaction formula is

[0025]

[0026] Finally, the obtained crude cartap was recrystallized with water to obtain 0.19 mol of cartap product.

Embodiment 2

[0028] The toluene solution (mass content is 30%) of the thiocyanide of 0.2mol and the water of 2.2mol, 0.5g butyl trioctyl ammonium bromide catalyst are placed in reactor together, then pass into hydrogen chloride gas, pass into amount The reaction temperature is controlled at -10°C for 0.5 mol, and the hydrolysis reaction is carried out for 15 hours. Finally, the crude cartap obtained is recrystallized with water to obtain 0.186 mol of cartap product.

Embodiment 3

[0030] The carbon tetrachloride solution (mass content is 20%) of the thiocyanide of 0.2mol and the water of 2.5mol, 0.4g benzyltributylammonium chloride catalyst are placed in the reactor together, then pass into hydrogen chloride gas, The feeding amount is 0.4 mol, the reaction temperature is controlled at 10° C., and the hydrolysis reaction is carried out for 24 hours. Finally, the obtained cartap crude product is recrystallized with water to obtain about 0.188 mol of cartap product.

technical field

[0001] The invention belongs to the field of agricultural insecticides, and in particular relates to a preparation method of a nereistin derivative bionic insecticide. Background technique

[0002] Nereistin derivatives are a class of high-efficiency, low-toxicity, broad-spectrum biomimetic insecticides, such as dimehydramine, cyclodime, dimehypo, dimehypo, monosultap, cartap, etc. In the 1970s, China began to develop nereist poison biomimetic insecticides, which have been industrially produced and widely used, mainly including three varieties of dimehypo, monosultap and cartap.

[0003] The classic synthetic method of cartap is to use dimehypo as the starting material, react with sodium cyanide to generate thiocyanide and sodium sulfite, then dissolve the thiocyanide in methanol solvent, and introduce hydrogen chloride gas to generate thiocyanide Dan and by-product chloromethane gas (see "Pesticide Synthesis and Application" edited by Chen Wanyi, Chemical I...

Examples

Embodiment 1

[0024] The ethylene dichloride solution (mass content is 25%) of the thiocyanide of 0.2mol and the water of 2.8mol, 0.5g benzyl trioctyl ammonium chloride catalyst are placed in reactor together, pass into hydrogen chloride gas then, The feed rate is 0.35mol, the reaction temperature is controlled at 20°C, and the hydrolysis reaction is carried out for 20 hours, and the reaction formula is

[0025]

[0026] Finally, the obtained crude cartap was recrystallized with water to obtain 0.19 mol of cartap product.

Embodiment 2

[0028] The toluene solution (mass content is 30%) of the thiocyanide of 0.2mol and the water of 2.2mol, 0.5g butyl trioctyl ammonium bromide catalyst are placed in reactor together, then pass into hydrogen chloride gas, pass into amount The reaction temperature is controlled at -10°C for 0.5 mol, and the hydrolysis reaction is carried out for 15 hours. Finally, the crude cartap obtained is recrystallized with water to obtain 0.186 mol of cartap product.

Embodiment 3

[0030] The carbon tetrachloride solution (mass content is 20%) of the thiocyanide of 0.2mol and the water of 2.5mol, 0.4g benzyltributylammonium chloride catalyst are placed in the reactor together, then pass into hydrogen chloride gas, The feeding amount is 0.4 mol, the reaction temperature is controlled at 10° C., and the hydrolysis reaction is carried out for 24 hours. Finally, the obtained cartap crude product is recrystallized with water to obtain about 0.188 mol of cartap product.

Images