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Cellulose derivative microencapsulated halogen-free flame retardant and preparation method thereof

A cellulose derivative and microencapsulation technology, applied in the field of flame retardants, can solve the problems of physical health production equipment damage, inability to meet modern production, high toxicity of raw materials, etc., and achieves good recycling effect, dense surface, and water resistance. improved effect

Active Publication Date: 2012-01-18
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the microcapsule flame retardants prepared by this method have certain hydrolysis resistance and moisture absorption resistance, such microcapsule products will release harmful gas formaldehyde during actual production and use, which will affect human health and production. equipment causing harm
European patent EP0542373A1 describes a method that uses amino resin as a capsule material and reacts in a mixed solution of water and organic solvent to coat ammonium polyphosphate, but the raw materials used are highly toxic and difficult to obtain; Chinese patent CN1379078A discloses A method of using unsaturated polyester resin to initiate polymerization in an inert solvent to obtain a microencapsulated nitrogen-phosphorus halogen-free flame retardant, but requires the use of a large amount of organic solvent
As people pay more and more attention to environmental protection and health and consider the cost of production, the above methods can no longer meet the requirements of modern production

Method used

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  • Cellulose derivative microencapsulated halogen-free flame retardant and preparation method thereof

Examples

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preparation example Construction

[0056] The preparation method of the above-mentioned cross-linked cellulose derivative microencapsulated halogen-free flame retardant specifically comprises the following steps:

[0057] Get each raw material according to the prescription of above-mentioned microencapsulated halogen-free flame retardant;

[0058] Preparation of halogen-free flame retardant: add the cellulose derivative in the above raw materials into the solvent, stir the solvent, and raise the temperature to 30-90°C, stir for 0.5-24 hours to derivatize the cellulose in the solvent After the substance is completely dissolved, add a halogen-free flame retardant and a surfactant to the solvent, then add a catalyst and a cross-linking agent, stir and react at a temperature of 30-90°C for 1-24 hours, then cool down to room temperature, filter, and filter The obtained filter cake is dried at 80-120 DEG C for 4-24 hours, and the obtained product is the cross-linked cellulose derivative microencapsulated halogen-free...

Embodiment 1

[0061] This example provides a method for preparing a cellulose derivative microencapsulated halogen-free flame retardant, which specifically includes the following steps:

[0062] Add 10 grams of nitrocellulose into a 1000 ml three-necked bottle, add 400 grams of methyl tert-butyl ether, start stirring, raise the temperature to 50°C, and stir for 1 hour at the same time. After the nitrocellulose is dissolved, add 100 grams of dry Ammonium polyphosphate powder and 5 grams of OP-10, then add 1 gram of dibutyltin dilaurate and 5 grams of p-phenylene diisocyanate, react at 50 ° C for 4 hours, cool to room temperature, filter with suction, wash with water, dry, and filter cake Dry at 80° C. for 12 hours to obtain 112.5 grams of a cross-linked nitrocellulose microencapsulated halogen-free flame retardant product.

[0063] The solubility of the obtained product at 25°C is 0.065g / 100mlH 2 O.

[0064] If the OP-10 in this embodiment is replaced by Benze, Situma Ge, Pingpingjia, Emol...

Embodiment 2

[0066] This example provides a method for preparing a cellulose derivative microencapsulated halogen-free flame retardant, which specifically includes the following steps:

[0067] Add 2 grams of nitrocellulose into a 500 ml three-necked bottle, add 200 grams of methyl tert-butyl ether, start stirring, raise the temperature to 50°C, and stir for 0.5 hours. After the nitrocellulose is dissolved, add 100 grams of dry poly Ammonium phosphate powder and 0.5 g of OP-10, then add 1 g of stannous octoate and 2 g of p-phenylene diisocyanate, react at 50 ° C for 12 hours, cool to room temperature, filter with suction, wash with water, dry, and filter the cake at 90 ° C After drying for 12 hours, 102.9 grams of a cross-linked nitrocellulose microencapsulated halogen-free flame retardant product was obtained.

[0068] The solubility of the obtained product at 25°C is 0.115g / 100mlH 2 O.

[0069] If p-phenylene diisocyanate is replaced by benzene-2,4-diisocyanate, toluene-2,6-diisocyanate,...

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Abstract

The invention discloses a cellulose derivative microencapsulated halogen-free flame retardant and a preparation method thereof, relating to the field of flame retardants. The flame retardant is prepared from a cellulose derivative, a solvent, a halogen-free flame retardant, a surfactant, a catalyst and a cross-linking agent used as raw materials; and the microencapsulated halogen-free flame retardant with the cross-linked cellulose derivative as a coating layer and the halogen-free flame retardant as a core is prepared by reacting the cellulose derivative with other raw materials except the cross-linking agent under the action of the cross-linking agent, wherein the weight ratio of the cross-linked cellulose derivative as the coating layer to the halogen-free flame retardant as the core in the microencapsulated halogen-free flame retardant is (0.04-0.3):1. The cellulose derivative microencapsulated halogen-free flame retardant has the advantages that: the average particle size is not increased obviously, the particles have good free fluidity, the shell layer is uniform and compact, the aquosity is greatly reduced, and the high-temperature water resistance is significantly improved; and the cellulose derivative microencapsulated halogen-free flame retardant can be used as the flame retardant for polyolefin, polyurethane, rubber, foamed plastics and other polymer materials, and can also be used for flame retarding of paper, wood, fabrics and the like.

Description

technical field [0001] The invention relates to the field of flame retardants, in particular to a halogen-free flame retardant coated by in-situ polymerization with a cross-linked cellulose derivative as the capsule material and a halogen-free flame retardant as the core material and its preparation method. Background technique [0002] Flame retardant is an additive that can make polymers and related materials difficult to catch fire or slow down the burning speed, and can be divided into halogen-containing flame retardants and halogen-free flame retardants. Halogen-containing flame retardants will produce more smoke and toxic corrosive gases during the combustion process, which will pollute the environment. For this reason, the European Union announced the "Waste Electrical and Electronic Equipment Directive" (referred to as "WEEE") and "About The core of the two directives on the Prohibition of the Use of Certain Hazardous Substances in Electrical and Electronic Equipmen...

Claims

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Application Information

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IPC IPC(8): C09K21/14C08K9/10B01J13/14
Inventor 胡源汪碧波宋磊唐琴波
Owner UNIV OF SCI & TECH OF CHINA