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Preparation method of novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester

A technology of tetramethylpiperidine nitroxide radical and phosphite triester, which is applied in the field of preparation of new polymerization inhibitors, can solve the problem of tetramethylpiperidine nitroxide radical phosphite triester polymerization inhibitor alkoxy In order to achieve the effects of high economic value, high yield and high current efficiency due to the lack of chemical research reports

Active Publication Date: 2020-11-27
宿迁盛瑞新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few research reports on the alkoxylation of tetramethylpiperidine nitroxide radical phosphite triester inhibitor

Method used

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  • Preparation method of novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester
  • Preparation method of novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 110g of tetramethylpiperidine nitroxide free radical phosphite triester into the electrolytic reaction bottle, then respectively drop into 32g of water, 26g of ethanol, 22g of potassium phosphate, 10g of tetrabutylphosphorous hydroxide (40% aqueous solution), at 38 ℃ , 1200A / m 2 Electrolytic catalytic oxidation under current density, the anode material is DSA (shape stable anode), the cathode material is graphite plate, after 32 hours of electrolysis, the electrolyte is filtered to obtain the alkoxy group of tetramethylpiperidine nitroxide radical phosphite triester The product of the intermediate was 98g, the content (GC) was 96.82%, and the yield was about 88.32%.

[0030] .

[0031] figure 2 for in (CH 3 CH 2 CH 2 CH 2 ) 4 The infrared spectrogram of the product prepared under the POH environment; before the electrolysis of the polymerization inhibitor 705, there was no hydroxyl (νOH) characteristic peak in the functional group region, and the alkoxy gr...

Embodiment 2

[0034] Put 110g of tetramethylpiperidine nitroxide free radical phosphite triester into the electrolytic reaction bottle, then drop into 30g of water, 22g of ethanol, 15g of potassium phosphate, 15g of tetrabutylphosphorus hydroxide (40% aqueous solution), at 38°C , 600A / m 3 Electrolytic catalytic oxidation under current density, the anode material is DSA (shape stable anode), the cathode material is graphite plate, after 32 hours of electrolysis, the electrolyte is filtered to obtain the alkoxy group of tetramethylpiperidine nitroxide radical phosphite triester The product 85g of the chemical intermediate, content (GC) 89.35%, yield is about 75%.

Embodiment 3

[0036] Put 110g of tetramethylpiperidine nitroxide free radical phosphite triester into the electrolytic reaction bottle, then drop into 40g of water, 30g of ethanol, 8g of potassium phosphate, 12g of tetrabutylphosphine hydroxide (40% aqueous solution), at 40°C , 600A / m 3 Electrolytic catalytic oxidation under current density, the anode material is DSA (shape stable anode), the cathode material is graphite plate, after 32 hours of electrolysis, the electrolyte is filtered to obtain the alkoxy group of tetramethylpiperidine nitroxide radical phosphite triester The product 80g of the chemical intermediate, content (GC) 91.33%, yield is about 72%.

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Abstract

The invention relates to the technical field of light stabilizer preparation, in particular to a preparation method of a novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester. The preparation method comprises the step of carrying out electrolytic catalytic oxidation on tetramethylpiperidine nitroxide free radical phosphite triester in the presenceof water, alcohol, phosphate and (CH3CH2CH2CH2) 4POH to prepare an N-OH type polymerization inhibitor of tetramethylpiperidine nitroxide free radical phosphite triester. The method has the following beneficial effects: compared with the conventional reaction process, the reaction is simple and rapid; other catalysts are not needed, so that the environmental pollution can be greatly reduced; raw materials are wide in source and cheap; and the final yield of the product is high, the equipment investment is low, and the economic value is higher.

Description

technical field [0001] The invention relates to the technical field of light stabilizer preparation, in particular to a preparation method of a novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester. Background technique [0002] At present, we have carried out a series of research work on compounds containing three nitroxide radicals, such as tetramethylpiperidine nitroxide radical phosphite triester, EPR, NMR, photostability, biomolecular spin labeling, etc. . The use of tetramethylpiperidine nitroxide free radical phosphite triester as a polymerization inhibitor, especially for acrylic acid and its esters, has a very good polymerization inhibition effect. It has been reported that tetramethylpiperidine nitroxide radical phosphite triester is used as a stable free radical for polymerization. [0003] The inhibition performance of tetramethylpiperidine nitroxide radical phosphite triester is better than that of phenols, aro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/02C08K5/524
CPCC08K5/524
Inventor 韩炎王晶项有和赵飞胡方洲邓啸韬谢振海张少平乔旺徐硕
Owner 宿迁盛瑞新材料有限公司
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