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Method for producing alkyl peroxycarboxylate based on titanium silicalite molecular sieve composite catalyst

A technology for peroxidizing alkyl carboxylate and titanium-silicon molecular sieve is applied in molecular sieve catalysts, peroxy compound preparation, chemical instruments and methods, etc. It can solve the problems of expensive acid chloride and corrosion, avoid corrosive substances and save chemical The effect of raw materials

Active Publication Date: 2021-04-16
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

One disadvantage of using acid chlorides is that the acid chlorides themselves are very expensive, another disadvantage is that the use of acid chlorides will form the corrosive substance hydrogen chloride
In addition, using acid chlorides as raw materials will also cause environmental problems in the form of chloride wastewater and waste solids.

Method used

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  • Method for producing alkyl peroxycarboxylate based on titanium silicalite molecular sieve composite catalyst
  • Method for producing alkyl peroxycarboxylate based on titanium silicalite molecular sieve composite catalyst
  • Method for producing alkyl peroxycarboxylate based on titanium silicalite molecular sieve composite catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] In a 500ml three-necked flask, 20ml of isododecane was added, 30g of tert-butyl hydroperoxide with a purity of 99.5wt.%, 57.3g of neodecanoic acid, and 20g of composite catalyst A were added. The mixture was stirred at 0°C for 6 hours. The composite catalyst A was recovered by filtration with a sand core filter to obtain 74.5 g of a solution containing tert-butyl peroxyneodecanoate. Based on the mass of input raw materials, the yield is 78%. According to gas chromatography analysis, the solution contained 60.8% of tert-butyl peroxyneodecanoate. See figure 1 .

[0053] Gas chromatography experimental conditions: 2m×φ3mm stainless steel column; stationary phase: 60-80 mesh white carrier coated with 5% SE-30; column temperature 40°C, vaporization temperature 90°C, detector FID temperature 110°C.

Embodiment 2

[0055] In a 500ml three-necked flask, 50ml of isododecane was added, 30g of tert-butyl hydroperoxide with a purity of 99.5wt.%, 57.3g of neodecanoic acid, and 15g of composite catalyst B were added. The mixture was stirred at 10°C for 6 hours. The composite catalyst B was recovered by filtration with a sand core filter to obtain 112.4 g of a solution containing tert-butyl peroxyneodecanoate, with a yield of 86% based on the mass of the input raw materials. According to gas chromatography analysis, the solution contained 19.0% tert-butyl peroxyneodecanoate.

Embodiment 3

[0057] In a 500ml three-necked flask, 100ml of toluene was added, 30g of tert-butyl hydroperoxide with a purity of 99.5wt.%, 57.3g of neodecanoic acid, and 15g of composite catalyst C were added. The reaction mixture was stirred at 20°C for 4 hours. The composite catalyst C was recovered by filtration with a sand core filter to obtain 161.6 g of a solution containing tert-butyl peroxyneodecanoate, with a yield of 89% based on the mass of the input raw materials. According to gas chromatography analysis, the solution contained 17.5% of tert-butyl peroxyneodecanoate.

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Abstract

The invention relates to a method for synthesizing alkyl peroxycarboxylate based on a titanium silicalite molecular sieve composite catalyst, and belongs to the technical field of peroxide production. According to the method, the defects in the prior art are overcome, and alkyl peroxycarboxylate is synthesized by adopting a titanium silicalite molecular sieve and a metal oxide composite catalyst. In the chemical reaction process that tert-butyl hydroperoxide or tert-amyl hydroperoxide reacts with carboxylic acid to generate tert-butyl peroxycarboxylate or tert-amyl peroxycarboxylate, reaction water is generated. The reaction water is to be removed from the reaction mixture in time. Azeotropic distillation and molecular distillation dehydration are generally adopted. However, these process operations require higher temperatures, which are not conducive to the stabilization and safety of alkyl peroxycarboxylate. The catalyst disclosed by the invention contains metal oxide, so that water generated by reaction can be adsorbed in time, and the synthesis reaction can be smoothly completed.

Description

technical field [0001] The invention relates to a method for producing an alkyl peroxycarboxylate based on a titanium-silicon molecular sieve composite catalyst, and belongs to the technical field of peroxide production. Background technique [0002] tert-butyl peroxycarboxylate and tert-amyl peroxycarboxylate are commercially important monomer polymerization initiators, especially for polyacrylic acid, polyethylene, polyvinyl chloride and polystyrene products. [0003] Chinese patent CN110981778A discloses a preparation method of cumene neodecanoate and solvent-based CNP. The preparation method uses cumene hydroperoxide, lye and neodecanoyl chloride to react to obtain a water-in-oil emulsion. [0004] Chinese patent CN106902869A discloses a solid-supported phase-transfer catalyst, which is prepared by the following method: add the carrier to an organic solvent containing a phase-transfer catalyst, heat to reflux, react for 10-20 hours, and then wash and filter to obtain a s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00B01J29/89
CPCY02P20/584
Inventor 黄燕民陈唐建翟志强薛育宴王跟泉孔祥伦
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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