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A kind of preparation method and application of modified nitroxide free radical inhibitor

A technology of nitroxide free radical and polymerization inhibitor, which is applied in the field of organic synthesis catalysis/inhibition, can solve the problems of affecting the polymerization inhibitory effect of the polymerization inhibitor and the difficulty of removing the high-efficiency polymerization inhibitor, and achieve the effect of convenient removal.

Active Publication Date: 2021-03-09
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nitroxide free radical polymer brush is a loaded heterogeneous polymerization inhibitor. Since the reaction system is a liquid phase system, the polymerization inhibitor can only have a polymerization inhibitory effect at the solid-liquid phase interface, thereby Greatly affected the inhibitory effect of the polymerization inhibitor
[0006] Therefore this area needs to develop a kind of simple and effective method, solves the difficult problem of removal of high-efficiency polymerization inhibitor at present

Method used

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  • A kind of preparation method and application of modified nitroxide free radical inhibitor
  • A kind of preparation method and application of modified nitroxide free radical inhibitor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] (1) Weigh 10g of sodium alginate with a molecular weight of 5000 and dissolve it in double distilled water, stir evenly, the system is in a completely dissolved state, slowly add HCl dropwise to the system, adjust the pH value to 4, and then pour the solution into ethanol : HCl=96:4 (v / v), the solid was collected by filtration, the obtained solid was washed with ethanol, and dried to obtain alginic acid solid.

[0059] (2) Take 5 g of alginic acid solid and disperse it in double distilled water, neutralize it with tetrabutylammonium hydroxide, finally adjust the pH value of the system to 6.5, and freeze-dry to obtain tetrabutyl alginate, an oil-soluble polysaccharide.

[0060] (3) Take 5g of tetrabutyl alginate, an oil-soluble polysaccharide, and dissolve it in 10ml of dimethylformamide solution, stir to dissolve it completely, then add 50mg of 2-chloro-1-methyliodopyridine, and place in an ice-water bath (0°C), catalyzed for 1 h under nitrogen. Then the temperature wa...

Embodiment 2

[0063] (1) Weigh 30g of sodium alginate with a molecular weight of 10,000 and dissolve it in double distilled water, stir evenly, the system is in a completely dissolved state, slowly add sulfuric acid to the system, adjust the pH value to 5, and then pour the solution into ethanol : HCl=90:10 (v / v), the solid was collected by filtration, the obtained solid was washed with methanol, and dried to obtain alginic acid solid.

[0064] (2) Take 20 g of alginic acid solid and disperse it in double distilled water, neutralize it with tetramethylammonium hydroxide, finally adjust the pH value of the system to 7.5, and freeze-dry to obtain tetramethyl alginate, an oil-soluble polysaccharide.

[0065] (3) Take 25g of tetramethyl alginate, an oil-soluble polysaccharide, and dissolve it in 25ml of diethylformamide solution, stir to dissolve it completely, then add 5g of 2-chloro-1-methyliodopyridine, and place in an ice-water bath (0°C), catalyzed for 1 h under nitrogen. Then the tempera...

Embodiment 3

[0073] (1) Weigh 50g of sodium alginate with a molecular weight of 12000 and dissolve it in double distilled water, stir evenly, the system is in a completely dissolved state, slowly add nitric acid dropwise to the system, adjust the pH value to 4.5, and then pour the solution into ethanol : HCl=98:2 (v / v), the solid was collected by filtration, the obtained solid was washed with propanol, and dried to obtain alginic acid solid.

[0074] (2) Take 40 g of alginic acid solid and disperse it in double distilled water, neutralize it with tetraethylammonium hydroxide, finally adjust the pH value of the system to 7, and freeze-dry to obtain tetraethyl alginate, an oil-soluble polysaccharide.

[0075] (3) Take 30g of oil-soluble polysaccharide alginic acid tetramethyl salt, dissolve it in 30ml of diethylformamide solution, stir to make it dissolve completely, then add 2.1g of 2-chloro-1-methyl iodopyridine, and put it on ice Water bath (0°C), catalyzed under nitrogen for 1h. Then th...

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Abstract

The invention relates to a preparation method and application of a modified nitroxide radical polymerization inhibitor. The modified nitrogen oxide radical polymerization inhibitor is based on the main chain structure of natural polysaccharide polymer sodium alginate to prepare oil-soluble polysaccharides, and the nitrogen oxide radical polymerization inhibitor is modified on the oily polysaccharide main chain through one-step esterification, Finally, a modified nitroxide radical polymerization inhibitor is obtained. The modified nitroxide free radical polymerization inhibitor is suitable for the special acrylate reaction system with acid alkenyl addition as the process. On the one hand, the polymerization inhibitor can effectively prevent the polymerization of raw materials and products, and on the other hand, it can efficiently separate the product and the polymerization inhibitor by using a simple method, so it has a good application prospect.

Description

technical field [0001] The invention relates to the field of organic synthesis catalysis / polymerization inhibition, in particular to a preparation method and application of a modified nitroxide radical polymerization inhibitor. Background technique [0002] Acrylic acid and esters are a kind of monomers containing double bonds. Due to their special chemical structure, they are very easy to polymerize during the reaction process. In order to effectively prevent the polymerization of monomers during the production process, a certain amount of polymerization inhibitors will be added to the reaction system to prevent polymerization from pre-laboratory research to industrial production. [0003] At present, there are many types of polymerization inhibitors in industry, including molecular polymerization inhibitors, such as p-tert-butylcatechol, phenothiazine, and tris(N-nitroso-N-phenylhydroxylamine) aluminum, etc., which have stable and free Radical inhibitors, such as 4-hydrox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/04C08F2/40
CPCC08B37/0084C08F2/40
Inventor 郭华鞠昌迅王明永孙双翼郑京涛陆国太黎源
Owner WANHUA CHEM GRP CO LTD