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

A technology of tetramethylpiperidine nitroxide free radical and phosphite triester is applied in the field of preparation of novel polymerization inhibitors, which can solve the problem of tetramethylpiperidine nitroxide radical phosphite triester polymerization inhibitor alkoxy There are few problems in chemical research reports, so as to achieve the effect of reducing interaction, less equipment investment and high current efficiency

Active Publication Date: 2021-06-29
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 a novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester
  • Preparation method of a 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 method for preparing a novel polymerization inhibitor based on tetramethylpiperidine nitroxide free radical phosphite triester; comprising the following steps: making tetramethylpiperidine nitroxide free Phosphite triester in water, alcohol, phosphate, (CH 3 CH 2 CH 2 CH 2 ) 4 Under the condition that POH exists, it is electrolytically catalyzed and oxidized to obtain its N-OH type polymerization inhibitor; the present invention has the following beneficial effects: the reaction is simpler and quicker than the conventional reaction process; without using other catalysts, environmental pollution can be greatly reduced; the raw material The source is wide and cheap; and the final yield of the product is high, and the investment in equipment is small, which makes it more economically valuable.

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 Patents(China)
IPC IPC(8): C25B3/23C25B3/05C25B3/07C25B3/09C08K5/524
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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