CN104513136A - Synthesis method for reactive flame retardant tetrabromo-p-phenylenedimethanol - Google Patents

Abstract

The invention discloses a synthesis method for reactive flame retardant tetrabromo-p-phenylenedimethanol. The method includes the steps of: firstly using bromine, anhydrous aluminum trichloride and p-xylene to synthesize tetrabromo-p-xylene; then reacting carbon tetrachloride, bromine and the obtained tetrabromo-p-xylene to synthesize tetrabromo-p-phenyl dimethyl bromide; then subjecting anhydrous sodium acetate, glacial acetic acid and the obtained tetrabromo-p-phenyl dimethyl bromide to esterification reaction to synthesize tetrabromo-p-phenylenedimethanol diacetate; and finally subjecting dioxane, potassium hydroxide and the obtained tetrabromo-p-phenylenedimethanol diacetate to hydrolysis reaction so as to obtain tetrabromo-p-phenylenedimethanol. The synthesis method for the reactive flame retardant tetrabromo-p-phenylenedimethanol provided by the invention has the characteristics of easily available reaction raw materials, simple and rapid synthesis, few by-products, high yield, and obvious flame retardant effect.

Description

The synthetic method of reactive flame retardant tetrabromo terephthalyl alcohol

 

Technical field

The present invention relates to a kind of preparation method of fire retardant, be specifically related to a kind of preparation method of reactive flame retardant.

 

Background technology

Reactive flame retardant has the function base that fire retardant can be bonded in polymer molecule with other monomer reactions, as vinyl, carboxyl, hydroxyl, additive flame retardant is then added in macromolecular material with physical admixture, a lot of shortcoming can be brought, first be that fire retardant easily runs off, the consistency of fire retardant and superpolymer is difficult to resolve certainly, moreover be add in a mixed manner, can produce a very large impact the performance of material, the problems such as response type then easily runs off owing to solving fire retardant, poor compatibility, make material have good homogeneity and be paid close attention to widely.

 

Summary of the invention

The object of the invention is to, provide a kind of synthetic method of reactive flame retardant tetrabromo terephthalyl alcohol, reaction raw materials is easy to get, and technique is simple, and by product is few, and yield is high.

A synthetic method for reactive flame retardant tetrabromo terephthalyl alcohol, it comprises the following steps:

One, in four-hole boiling flask, add bromine, aluminum trichloride (anhydrous), stir at 5 DEG C of temperature, drip p-Xylol, dropwise, reaction produces to without hydrogen bromide, and logical nitrogen, adds methyl alcohol, and cooling is filtered;

Two, add in four-hole boiling flask by above-mentioned product and tetracol phenixin mixing, logical nitrogen, heating for dissolving, drips the mixing solutions of bromine and tetracol phenixin, dropwises, back flow reaction 6h under illumination, and cooling is filtered, washing, dry white solid;

Three, add in there-necked flask by above-mentioned gained white solid and sodium acetate, anhydrous, Glacial acetic acid, be heated to backflow, stirring reaction, to reaction solution clear, cools, suction filtration, dry, obtains white solid;

Four, add in there-necked flask by step 3 gained white solid and dioxane, be heated to backflow, drip potassium hydroxide solution, back flow reaction 2h, adds a small amount of water and makes product become semi-solid mashed prod, and cooling is filtered, washing, dry, obtains product.

The synthetic method of reactive flame retardant tetrabromo terephthalyl alcohol provided by the invention, its beneficial effect is, reaction raw materials is easy to get, simple synthetic method, quick, and by product is few, and yield is high, and its flame retardant effect is obvious.

 

Embodiment

Below in conjunction with an embodiment, the synthetic method of reactive flame retardant tetrabromo terephthalyl alcohol provided by the invention is described in detail.

 

Embodiment

One, in 250ml four-hole boiling flask, add 64g bromine, 1g aluminum trichloride (anhydrous), stir at 5 DEG C of temperature, drip 20ml p-Xylol, dropwise, reaction produces to without hydrogen bromide, steams bromine with water-bath, and bromine is caught up with to the greatest extent by logical nitrogen, adds methyl alcohol, and cooling is filtered;

Two, in the four-hole boiling flask that mechanical stirring, reflux condensing tube and constant pressure funnel are housed, add the above-mentioned product of 38g and 520ml tetracol phenixin, logical nitrogen, heating for dissolving, drips the mixing solutions of 10ml bromine and 50ml tetracol phenixin, dropwise, back flow reaction 6h under illumination, is cooled to 0-5 DEG C, filters, colourless to filtrate with the washing of cold tetracol phenixin, dry white solid;

Three, in there-necked flask, add the above-mentioned gained white solid of 42g and 42g sodium acetate, anhydrous, 670ml Glacial acetic acid, be heated to backflow, stirring reaction, to reaction solution clear, cools, suction filtration, dry, obtains white solid;

Four, in there-necked flask, add 20g step 3 gained white solid and 200ml dioxane, be heated to backflow, under agitation dropping is dissolved in the solution in 50ml water containing 20g potassium hydroxide, dropwise, back flow reaction 2h, adding a small amount of water makes product become semi-solid mashed prod, cooling, filters, washing, drying, obtains product.

Claims (1)

1. a synthetic method for reactive flame retardant tetrabromo terephthalyl alcohol, is characterized in that: it comprises the following steps:

One, in four-hole boiling flask, add bromine, aluminum trichloride (anhydrous), stir at 5 DEG C of temperature, drip p-Xylol, dropwise, reaction produces to without hydrogen bromide, and logical nitrogen, adds methyl alcohol, and cooling is filtered;

Two, add in four-hole boiling flask by above-mentioned product and tetracol phenixin mixing, logical nitrogen, heating for dissolving, drips the mixing solutions of bromine and tetracol phenixin, dropwises, back flow reaction 6h under illumination, and cooling is filtered, washing, dry white solid;

Three, add in there-necked flask by above-mentioned gained white solid and sodium acetate, anhydrous, Glacial acetic acid, be heated to backflow, stirring reaction, to reaction solution clear, cools, suction filtration, dry, obtains white solid;

Four, add in there-necked flask by step 3 gained white solid and dioxane, be heated to backflow, drip potassium hydroxide solution, back flow reaction 2h, adds a small amount of water and makes product become semi-solid mashed prod, and cooling is filtered, washing, dry, obtains product.