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Composite catalyst for propiconazole cyclization reaction and preparation method thereof

A technology for composite catalysts and cyclization reactions, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the impact of impurities, general catalytic effect, and inconvenient recycling Bromination reaction and other problems, to achieve the effect of increasing yield, good catalytic effect, and maintaining acidic reaction environment

Active Publication Date: 2019-06-04
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

A composite catalyst for propiconazole cyclization reaction and a preparation method thereof are disclosed, the composite catalyst is prepared from the following raw materials in parts by weight: 1.5-3.5 parts of zinc trifluoromethanesulfonate, 0.8 to 2.2 parts of sodium trinitrobenzene sulfonate, 0.6 to 1.4 parts of sodium dichromate and 9.5-10.6 parts of a catalyst carrier; according to the preparation method disclosed by the invention, the zinc trifluoromethanesulfonate, the sodium trinitrobenzene sulfonate and the sodium dichromate are compounded together through the catalyst carrier to prepare the composite catalyst, and the composite catalyst is good in stability and excellent in performance, so that the reaction medium environment of the propiconazole cyclization reaction can be improved, the rate of the propiconazole cyclization reaction and the yield of a cyclization substance are increased, the recovery is convenient and thorough, no impurities can be brought to the subsequent bromination reaction, the yield of the bromination reaction is not affected, and the yield and purity of the final propiconazole original medicine are improved.

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 Applications(China)
IPC IPC(8): B01J31/34C07D317/16
Inventor 陈华曾挺潘光飞
Owner JIANGSU HEBEN BIOCHEM
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