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Flax cellulose-based phosphorus expansion type flame retardant and preparation method and application thereof

A technology of intumescent flame retardant and flax fiber, which is applied in the field of flax cellulose-based phosphorus-based intumescent flame retardant and its preparation, can solve the problems of high destructiveness of cellulose, leftover by-products, complicated process, etc., and achieve synergy High flame retardant efficiency, uniform and dense carbon layer structure, and high mechanical properties

Inactive Publication Date: 2016-10-26
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, although there have been reports on the preparation of carboxycellulose at home and abroad, the preparation process is complicated and the conditions are harsh, and it must be prepared in a strongly acidic or alkaline medium.
The selected oxidizing agent is not only destructive to the cellulose itself, but also has by-products left over, which has a certain impact on the environment

Method used

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  • Flax cellulose-based phosphorus expansion type flame retardant and preparation method and application thereof
  • Flax cellulose-based phosphorus expansion type flame retardant and preparation method and application thereof
  • Flax cellulose-based phosphorus expansion type flame retardant and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0052] Soak 100 parts of flax fiber in 1500 parts of distilled water, and drop in pre-configured 0.1mol / L CuSO 4 Solution 2 parts, slowly add 24.6 parts of hydrogen peroxide (H 2 o 2 Content 30%) solution, placed in 30 DEG C constant temperature stirring reaction for 72 hours, suction filtered and washed with distilled water carboxy flax fiber, put into 80 DEG C drying box and dry for 12 hours. After taking it out, it was pulverized with a high-speed mixer for 6 minutes to obtain a solid product. The carboxyl content was measured to be about 12.6% by titration method, and the marked sample was OLF12.6.

Embodiment 2

[0054] Soak 100 parts of flax fibers in 1500 parts of distilled water, drop in the pre-configured 0.05mol / L FeCl 2 Solution 3 parts, slowly add 48.6 parts of hydrogen peroxide (H 2 o 2 Content 30%) solution, placed in 35 ℃ constant temperature stirring reaction for 60 hours, suction filtered and washed with distilled water carboxy flax fiber, put into 85 ℃ drying box to dry for 12 hours. After taking out, the fiber was pulverized with a high-speed mixer for 6 minutes to obtain a solid product. The carboxyl content was measured to be about 27.4% by titration method, and the marked sample was OLF27.4.

Embodiment 3

[0056] Soak 100 parts of flax fiber in 1500 parts of distilled water, drop in the pre-configured 0.05mol / L CoCl 2 Solution 3 parts, slowly add 50.9 parts of hydrogen peroxide (H 2 o 2 Content 30%) solution, placed in 40 ° C constant temperature stirring reaction for 70 hours, will be suction filtered and washed with distilled water carboxy flax fiber, put into 85 ° C drying oven to dry for 12 hours. After taking it out, the fiber was pulverized with a high-speed mixer for 6 minutes to obtain a solid product. The carboxyl content was measured to be about 28.4% by titration method, and the marked sample was OLF28.4.

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Abstract

The invention belongs to the technical field of phosphorous expansion type flame retardants, and discloses a flax cellulose-based phosphorus expansion type flame retardant and a preparation method and application thereof. The flame retardant is prepared from, by weight, 2-10 parts of carbon source, 1-10 parts of acid source and 1-10 parts of air source; the carbon source is carboxyl flax fiber high in carbonyl content, the carboxyl flax fiber high in carbonyl content is prepared through the following steps that the flax fiber is soaked in water, H2O2 and a catalyst are added, a stirring reaction is conducted, and the carboxyl flax fiber high in carbonyl content is obtained. The invention further provides an epoxy resin composite material based on the flame retardant. The flame retardant takes the carboxyl flax fiber high in carbonyl content as the carbon source, the char yield ranges from 20% to 27.2%, and combustible gas released through thermolysis is less. The limit oxygen index of the obtained epoxy resin composite material exceeds 29, the vertical flame rating is V-0, the release quantity of the gross heat of combustion is decreased by more that 60%, and the flame retardant has the advantages of being low in water absorption, high in mechanical property and the like.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing intumescent flame retardants, and in particular relates to a flax cellulose-based phosphorus-based intumescent flame retardant and a preparation method and application thereof. Background technique [0002] Cellulose is the most widely distributed and most abundant polysaccharide in nature, accounting for more than 50% of the carbon content in the plant kingdom. As a kind of cellulose derivative, carboxylated flax fiber has the characteristics of good biocompatibility, biodegradability, environmental friendliness and non-toxicity, and has been widely used in many industries. with hydrogen peroxide (H 2 o 2 ) to prepare carboxylated flax fiber has attracted much attention due to its advantages of greenness, environmental protection and high purity. After cellulose is oxidized, its performance is greatly improved compared with natural cellulose. For example, Chinese patent applicat...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L1/04C08K9/10C08K5/3492C08K3/32C08B15/04
CPCC08B15/04C08L63/00C08L2201/02C08L1/04C08K9/10C08K5/34922C08K2003/323
Inventor 张水洞殷悦彭华乔江金辉
Owner SOUTH CHINA UNIV OF TECH
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