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Cross-linked polymer flame retardant and preparation method thereof

A technology of cross-linked polymers and flame retardants, which is applied in the direction of fire-resistant coatings, etc., can solve the problems of general flame-retardant effect, hinder wide application, reduce flame-retardant durability, etc., and achieve low cost, high yield, and high flame retardancy The effect of potency

Inactive Publication Date: 2020-09-08
马海社
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant effect is general, and it needs to be compounded with other flame retardants to improve the flame retardant effect when used, which hinders its wide application
In addition, as time goes on, chlorinated paraffins are easy to migrate out of the polymer network, reducing the durability of flame retardancy

Method used

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  • Cross-linked polymer flame retardant and preparation method thereof
  • Cross-linked polymer flame retardant and preparation method thereof
  • Cross-linked polymer flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of carboxyl-containing chlorinated paraffin 42: Dissolve 20 g of chlorinated paraffin 42 in 200 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 30 g of potassium carbonate, and react at 55° C. for 30 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol, and the product was vacuum-dried at 100° C. for 5 h to obtain carboxyl-containing chlorinated paraffin 42.

[0032] (2) Preparation of chlorinated paraffin 42 containing acid chloride: add 70mol carboxyl-containing chlorinated paraffin 42 to the reaction kettle, add dropwise 85mol phosphorus trichloride, stir and heat up to 70°C, react for 4h, cool to room temperature, and stand to separate Layer to obtain chlorinated paraffin 42 containing acid chloride.

[0033] (3) Preparation of dibasic hydroxyisocyanurate-containing modified chlorinated paraffin 42: add 100mol tris(2-hydroxyethyl)isocyanurate and an ...

Embodiment 2

[0037] (1) Preparation of carboxyl-containing chlorinated paraffin 52: Dissolve 20 g of chlorinated paraffin 52 in 200 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 30 g of potassium carbonate, and react at 80° C. for 10 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol. The product was vacuum-dried at 100° C. for 5 h to obtain carboxyl-containing chlorinated paraffin 52.

[0038] (2) Preparation of chlorinated paraffin 52 containing acid chloride: add 70 mol of chlorinated paraffin 52 containing carboxyl to the reaction kettle, dropwise add 85 mol of phosphorus trichloride, stir and heat up to 50°C, react for 6 hours, cool to room temperature, let stand to separate layer to obtain the chlorinated paraffin 52 containing the acid chloride.

[0039](3) Preparation of modified chlorinated paraffin 52 containing dihydroxyisocyanurate: add 100mol tris(2-hydroxyethyl)isocyanura...

Embodiment 3

[0043] (1) Preparation of carboxyl-containing chlorinated paraffin 70: Dissolve 20 g of chlorinated paraffin 70 in 200 mL of acetone, stir to dissolve, add 20 g of p-hydroxybenzoic acid and 30 g of potassium carbonate, and react at 65° C. for 24 h under nitrogen protection. After the reaction, the pH was adjusted to 3.0 with hydrochloric acid, and then extracted with ethanol, and the product was vacuum-dried at 100°C for 5 hours to obtain carboxyl-containing chlorinated paraffin 70.

[0044] (2) Preparation of chlorinated paraffin 70 containing acid chloride: add 70mol of carboxyl-containing chlorinated paraffin 52 to the reaction kettle, add 85mol of phosphorus trichloride dropwise, stir and heat up to 60°C, react for 5h, cool to room temperature, and stand to separate layer to obtain chlorinated paraffin 70 containing acid chloride.

[0045] (3) Preparation of dihydroxyisocyanurate-containing modified chlorinated paraffin 70: add 100mol tris(2-hydroxyethyl)isocyanurate and a...

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Abstract

The invention discloses a cross-linked polymer flame retardant and a preparation method thereof. The preparation method of the flame retardant comprises the following steps: reacting chlorinated paraffin with p-hydroxybenzoic acid to prepare carboxyl-containing chlorinated paraffin, acylating the carboxyl-containing chlorinated paraffin to obtain acyl chloride-containing chlorinated paraffin, then, carrying out esterification reaction with tris(2-hydroxyethyl)isocyanurate to obtain hydroxyl-containing isocyanurate modified chlorinated paraffin, then reacting with tetrabromophthalic anhydride to form novel binary acid and performing polycondensation with tris(2-hydroxyethyl)isocyanurate to form macromolecular flame retardant. The preparation method has the advantages that the operation is simple, the raw material source is wide, the reaction condition is mild, the industrial production is met, and the prepared macromolecular flame retardant has excellent flame-retardant performance dueto the synergistic effect of flame-retardant elements of chlorine, bromine and nitrogen and has good migration resistance.

Description

technical field [0001] The invention relates to a cross-linked polymer flame retardant and a preparation method thereof, belonging to the field of plastic rubber flame retardants. Background technique [0002] With the development of the national economy and the improvement of people's living standards, synthetic fibers, plastics, rubber and other polymer materials are more and more widely used in transportation, building materials, electronic appliances, daily furniture, interior decoration and other fields. However, these polymer materials are generally flammable and easy to cause fire accidents. In order to solve the problems of flame resistance and smoke suppression of synthetic materials and ensure the safety of synthetic materials, the most effective method is to add flame retardants. Due to the low addition amount, low price and good compatibility with synthetic materials, halogen-based flame retardants do not change the original mechanical processing properties of fl...

Claims

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Application Information

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IPC IPC(8): C08G63/685C08G63/682C09K21/14C08L75/04C08L67/00C08L91/06C08K3/22
CPCC08G63/6826C08G63/6856C08L75/04C08L2201/02C09K21/14C08L67/00C08K3/2279C08L91/06
Inventor 马海社
Owner 马海社
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