Method for preparing melamine phosphate (borate) fire retardant

A technology of melamine salt and flame retardant, which is applied in the field of preparation of intumescent flame retardants, can solve the problems affecting the yield and performance of final products, and achieve the effects of avoiding equipment corrosion, reducing environmental hazards and improving yield.

Inactive Publication Date: 2008-03-19
应急管理部四川消防研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction solution of the intermediate prepared by this method is acidic in the aqueous phase, thus causing the hydrolysis of part of the phosphoric acid ester, which affects the yield and performance of the final product (halogen-free flame retardant pentaerythritol diphosphate melamine salt [J]. Science and Technology, 2006, 14(3): 15-18.)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Mix 0.2 mol of pentaerythritol, 0.6 mol of phosphoric acid, and 0.27 g of aluminum chloride uniformly, heat up to 120° C., react for 2 hours, cool to room temperature, then add 0.9 mol of melamine and mix uniformly to obtain a white lumpy solid. The solid is crushed to a fine powder that can pass through a 120-mesh sieve, and then transferred to the reactor, reacted for 1.5 hours at a reaction temperature of 230°C, and cooled to room temperature; the product was washed with water and ethanol in sequence until the filtrate was neutral, and filtered , drying, and crushing to obtain a phosphate ester melamine salt flame retardant with a yield of 82.2%. After the filtrate is sealed, it can be used as a flame retardant solution for wood and fabrics.

Embodiment 2

[0025] Mix 0.2mol of dipentaerythritol, 0.4mol of polyphosphoric acid, and 0.76g of ferric chloride uniformly, heat up to 135°C, react for 3 hours, cool to room temperature, then add 1.0mol of melamine to it and mix uniformly to obtain a white lumpy solid , crush the solid to a fine powder that can pass through a 120-mesh sieve, then transfer it to a reactor, react for 2 hours at a reaction temperature of 215°C, and cool to room temperature; wash the product with water and ethanol in sequence until the filtrate is neutral , after filtering, drying and pulverizing, the phosphate melamine salt flame retardant was obtained, and the yield was 81.7%. After the filtrate is sealed, it can be used as a flame retardant solution for wood and fabrics.

Embodiment 3

[0027] Mix 0.2 mol of tripentaerythritol, 0.5 mol of boric acid, and 0.89 g of zinc chloride uniformly, heat up to 150°C, react for 2.5 hours, cool to room temperature, then add 0.75 mol of melamine and mix uniformly to obtain a white lumpy solid. The solid is crushed to a fine powder that can pass through a 120-mesh sieve, and then transferred to a reactor, reacted for 3.5 hours at a reaction temperature of 205°C, and cooled to room temperature; the product is washed with water and ethanol in sequence until the filtrate is neutral, After filtering, drying and crushing, the borate melamine salt flame retardant is obtained, and the yield is 80.5%. After the filtrate is sealed, it can be used as a flame retardant solution for wood and fabrics.

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PUM

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Abstract

The present invention discloses a method which can prepare a phosphate (borate) melamine salt flame retardant by a dry process. According to the molar ratio of 1:2 to 4, small molecular polyol and inorganic acid containing phosphor or boron are uniformly mixed with lewis acid catalyst with one to one point five percent of the weight of the small molecular polyol, the temperature of the produced solution is raised to 100 to 150 DEG C, reaction lasts two to five hours, after melamine with the molar ratio of 1:1.5 to 2.5 of inorganic acid containing phosphor or boron is added, the produced solid is smashed into fine powder which can pass through a sieve with one hundred and twenty meshes, under a reaction temperature between 180 DEG C and 230 DEG C, reaction lasts one point five to four hours, and after the generated product is washed until the filtrate is neutral, the phosphate (borate) melamine salt flame retardant is produced by filtration, drying and smash. Because the dry process is applied, the present invention avoids the problem that the organic solvents used by the prior art harm environment and erode equipment, reduces energy consumption and production cost and avoids the problem of the hydrolysis of phosphate, which is caused by a reaction under the water phase; moreover, the present invention has the advantages of simple technique and convenient operation and is suitable for industrialized production.

Description

technical field [0001] The invention belongs to the technical field of preparation methods of intumescent flame retardants, and in particular relates to a dry method for preparing phosphorus (boric) ester melamine salt-based flame retardants. Background technique [0002] With the increasing awareness of environmental protection, halogen-free flame retardant technology has attracted much attention because it can endow polymer materials with flame retardant properties without producing secondary pollution. Halogen-free flame retardants are mainly divided into two categories: one is based on Mg(OH) 2 , Al(OH) 3 The representative inorganic flame retardant; the other is the intumescent flame retardant (IFR). Among them, the intumescent flame retardant can form a dense carbon layer when heated, which can hinder the thermal decomposition and combustion of the inner matrix through its thermal insulation and oxygen barrier function, so it has less smoke, no dripping, and no toxic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/09C07F5/04C08K5/3492
Inventor 张翔唐勇李风兰彬张帆
Owner 应急管理部四川消防研究所
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