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A kind of composite catalyst for propiconazole cyclization reaction and preparation method thereof

A composite catalyst, cyclization reaction technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the influence of impurities, general catalytic effect, and inconvenient recovery Bromination reaction and other problems, to achieve the effect of improving yield, good catalysis, and improving the environment of the reaction medium

Active Publication Date: 2021-08-27
JIANGSU HEBEN BIOCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of the present invention is to provide a composite catalyst for the cyclization reaction of propiconazole, which solves the problem that the catalysis of the catalyst for the cyclization reaction in the preparation process of the original propiconazole is general, and the recovery is inconvenient to bring impurities into the bromination reaction. problem of influence

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A kind of composite catalyst for propiconazole cyclization reaction

[0035] The raw material composition and mass fraction of the composite catalyst for propiconazole cyclization reaction are: zinc trifluoromethanesulfonate 1.5kg, sodium trinitrobenzenesulfonate 0.8kg, sodium dichromate 0.6kg, catalyst carrier 9.5kg The raw material of the catalyst carrier is composed of activated carbon, diatomite, zeolite powder, ceramic powder and calcium carbonate in a mass ratio of 1:2.5:3.0:1.5:0.8; the particle size of the zeolite powder is 80 mesh.

[0036] Prepared by:

[0037] S10, making the zinc trifluoromethanesulfonate, sodium trinitrobenzenesulfonate and sodium dichromate in the parts by weight into a zinc trifluoromethanesulfonate aqueous solution with a mass fraction of 65%, and a zinc trifluoromethanesulfonate aqueous solution with a mass fraction of 75%. Sodium trinitrobenzene sulfonate aqueous solution, mass fraction are 78% sodium dichromate aqueous solution, for su...

Embodiment 2

[0043] A kind of composite catalyst for propiconazole cyclization reaction

[0044] The raw material composition and mass fraction of the composite catalyst for propiconazole cyclization reaction are: zinc trifluoromethanesulfonate 3.5kg, sodium trinitrobenzenesulfonate 2.2kg, sodium dichromate 1.4kg, catalyst carrier 10.6kg The raw material of the catalyst carrier is composed of activated carbon, diatomite, zeolite powder, ceramic powder and calcium carbonate in a mass ratio of 1:4:6.5:5.5:1.6; the particle size of the zeolite powder is 140 mesh.

[0045] Prepared by:

[0046] S10, making the zinc trifluoromethanesulfonate, sodium trinitrobenzenesulfonate and sodium dichromate in the parts by weight into an aqueous zinc trifluoromethanesulfonate solution with a mass fraction of 85%, and a zinc trifluoromethanesulfonate aqueous solution with a mass fraction of 95%. Sodium trinitrobenzene sulfonate aqueous solution, mass fraction are the sodium dichromate aqueous solution of 8...

Embodiment 3

[0052] A kind of composite catalyst for propiconazole cyclization reaction

[0053] The raw material composition and mass fraction of the composite catalyst for propiconazole cyclization reaction are: zinc trifluoromethanesulfonate 1.9kg, sodium trinitrobenzenesulfonate 1.0kg, sodium dichromate 0.8kg, catalyst carrier 9.7kg The raw material of the catalyst carrier is composed of activated carbon, diatomite, zeolite powder, ceramic powder and calcium carbonate in a mass ratio of 1:3.0:3.5:2.5:1.0; the particle size of the zeolite powder is 100 mesh.

[0054] Prepared by:

[0055] S10, the zinc trifluoromethanesulfonate, sodium trinitrobenzenesulfonate and sodium dichromate of the weight parts are respectively made into a zinc trifluoromethanesulfonate aqueous solution with a mass fraction of 67%, and a zinc trifluoromethanesulfonate aqueous solution with a mass fraction of 77%. Sodium trinitrobenzene sulfonate aqueous solution, mass fraction are 80% sodium dichromate aqueous s...

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Abstract

The invention relates to a composite catalyst for propiconazole cyclization reaction and a preparation method thereof. The raw material composition and parts by weight of the composite catalyst for propiconazole cyclization reaction are: 1.5 parts of zinc trifluoromethanesulfonate to 3.5 parts, 0.8 parts to 2.2 parts of sodium trinitrobenzenesulfonate, 0.6 parts to 1.4 parts of sodium dichromate, 9.5 parts to 10.6 parts of catalyst carrier; Sodium benzene sulfonate and sodium dichromate are used together to make a composite catalyst through the catalyst carrier, which has good stability and excellent performance, so it can improve the reaction medium environment of the propiconazole cyclization reaction, improve the propiconazole cyclization reaction rate and ring The yield of the compound, the recovery is convenient and thorough, does not bring impurities into the subsequent bromination reaction, does not affect the yield of the bromination reaction, and improves the yield and purity of the final propiconazole technical drug.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a composite catalyst for propiconazole cyclization reaction and a preparation method thereof. Background technique [0002] The chemical structural formula of propiconazole is: [0003] The appearance of propiconazole technical product is light yellow viscose liquid, boiling point (13.3Pa) 180°C, vapor pressure (20°C) 0.133mPa, refractive index 1.5468, specific gravity (20°C) 1.27g / cm 3 . The solubility in water is 110mg / L, easily soluble in organic solvents. Stable below 320°C, relatively stable to light, and not obvious in hydrolysis. It is relatively stable in acidic and alkaline media and does not corrode metals. Storage stability for 3 years. [0004] Propiconazole is a low-toxic fungicide, and under the test conditions, no teratogenic, carcinogenic, or mutagenic effects were seen. The original drug has an acute oral LD50>1517mg / kg for rats, and an a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/34C07D317/16
Inventor 陈华曾挺潘光飞
Owner JIANGSU HEBEN BIOCHEM
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