CN102127198A - Method for preparing bisphenol A type boron phenolic resin - Google Patents

Abstract

The invention discloses a method for preparing a bisphenol A type boron phenolic resin. A component formula and the preparation method are provided. The component formula of bisphenol A, formaldehyde, boric acid, borax and a catalyst is adopted; the conventional equipment is utilized in coordination with the technical scheme of an easy and practicable process flow; and the problems that small private enterprise production are not suitable in the prior art are solved. In the method for preparing the bisphenol A type boron phenolic resin, the preparation of boron modified phenolic resin is suitable for small private enterprise production through the conventional equipment and a simple preparation process.

Description

The preparation method of bisphenol A-type boron bakelite resin

Technical field

The present invention relates to a kind of preparation method of boron modified phenolic resin, specifically be meant the employing conventional equipment, prepare the preparation method of a kind of bisphenol A-type boron bakelite resin of bisphenol A-type boron bakelite resin with dihydroxyphenyl propane, formaldehyde, boric acid, borax polymerization.

Background technology

Boron bakelite resin is a kind of boron modified phenolic resin, and solid-phase synthesis is adopted in the preparation of prior art boron modified phenolic resin, earlier esterification, generation triphenyl-boron is taken place for phenol and boron oxide 300 ℃ the time; With the reaction 150 ℃ time of triphenyl-boron and Paraformaldehyde 96, generate BPF again; Then with product respectively at 80,100 ℃ of thermal treatments 24 hours, obtain yellow solid boron modified phenolic resin goods.Solid-phase synthesis required equipment and processing condition are suitable for large and medium-sized enterprise's suitability for industrialized production, are not suitable for the enforcement of private small business, and therefore, there are the problems and shortcomings that are not suitable for the production of private small business in art methods.

Summary of the invention

Problems and shortcomings at above-mentioned prior art existence, the present invention adopts the component prescription of dihydroxyphenyl propane, formaldehyde, boric acid, borax, catalyzer, utilize conventional equipment, supporting technical scheme with simple technical process, a kind of preparation method of bisphenol A-type boron bakelite resin is provided, is intended to the preparation of boron modified phenolic resin to be reached and is suitable for the purpose that private small business produces by conventional equipment, simple and easy technology.

The object of the present invention is achieved like this: the preparation method of bisphenol A-type boron bakelite resin, comprise component prescription, preparation method, wherein,

Described component prescription is:

Dihydroxyphenyl propane, 44.7～58.8%;

Formaldehyde (37%), 29.32～37.27%;

Boric acid, 5.9～8.94%;

Borax, 5.9～8.94%;

Catalyzer: potassium hydroxide or sodium hydroxide, 10% the aqueous solution, 0.08～0.15%;

The prescription unit is weight percentage;

Described preparation method:

Step 1,

Formaldehyde in the component prescription and dihydroxyphenyl propane adding are had in the stainless steel cauldron of agitator and thermometer, add the catalyzer in the component prescription when heated and stirred, temperature reach 60 ℃, be warming up to 65 ℃, constant temperature begins the vacuum decompression distillation dehydration after 0.5 hour;

Step 2,

When temperature of reaction is gone up to 67～70 ℃, stop the vacuum decompression distillation, and in reactor, add borax and boric acid in the component prescription, be warming up to 100 ℃ once more, constant temperature vacuum decompression distillation dehydration once more after 1 hour;

Step 3,

The question response temperature rises to 120 ℃ gradually and stops the vacuum decompression distillation, and blowing cooling at once is cooled to room temperature and obtains the solid state material, through pulverizing, packs, and is the finished product of bisphenol A-type boron bakelite resin.

Above-mentioned, the present invention adopts the component prescription of dihydroxyphenyl propane, formaldehyde, boric acid, borax, catalyzer, utilize conventional equipment, supporting technical scheme with simple technical process, overcome art methods and had the problems and shortcomings that are not suitable for the production of private small business, the preparation method of a kind of bisphenol A-type boron bakelite resin that is provided has reached the preparation of boron modified phenolic resin by conventional equipment, simple and easy preparation technology and is suitable for the purpose that private small business produces.

The embodiment explanation

Below be described in further detail by the preparation method of specific embodiment bisphenol A-type boron bakelite resin of the present invention, the those skilled in the art can make the bisphenol A-type boron bakelite resin with reference to prescription and the preparation method of embodiment, but should not be construed as any limitation of the invention.

Embodiment

Embodiment

The name of an article: bisphenol A-type boron bakelite resin

Prescription: the prescription unit is weight percentage

Dihydroxyphenyl propane, 44.7%;

Formaldehyde (37%), 37.27%;

Boric acid, 8.94%;

Borax, 8.94%;

Catalyzer: potassium hydroxide, 10% the aqueous solution, 0.15%;

The prescription unit is weight percentage;

Preparation condition, equipment:

Ambient pressure a: normal atmosphere;

Envrionment temperature: room temperature;

Preparation equipment:

Stainless steel cauldron (having agitator, electric heater and thermometer), water-ring vacuum pump, jaw crusher, iron sheet container (long 2 meters * wide 1 meter * high 0.3 meter, some);

The preparation method:

Step 1,

Formaldehyde and dihydroxyphenyl propane are added in the stainless steel cauldron, add catalyzer when heated and stirred, temperature reach 60 ℃, be warming up to 65 ℃, constant temperature begins the vacuum decompression distillation dehydration after 0.5 hour;

Step 2,

When temperature of reaction is gone up to 67～70 ℃, stop the vacuum decompression distillation, and in reactor, add borax and boric acid, be warming up to 100 ℃ once more, constant temperature vacuum decompression distillation dehydration once more after 1 hour;

Step 3,

The question response temperature rises to 120 ℃ gradually and stops the vacuum decompression distillation, and blowing cooling at once is cooled to room temperature and obtains the solid state material, through pulverizing, packs, and is the finished product of bisphenol A-type boron bakelite resin.

Claims (1)

1. the preparation method of a bisphenol A-type boron bakelite resin, it is characterized in that: comprise component prescription, preparation method, described component prescription is: dihydroxyphenyl propane, 44.7～58.8%; Formaldehyde (37%), 29.32～37.27%; Boric acid, 5.9～8.94%; Borax, 5.9～8.94%; Catalyzer: potassium hydroxide, 10% the aqueous solution, 0.08～0.15%; The prescription unit is weight percentage;

Described preparation method:

Step 1,

Formaldehyde in the component prescription and dihydroxyphenyl propane adding are had in the stainless steel cauldron of agitator and thermometer, add the catalyzer in the component prescription when heated and stirred, temperature reach 60 ℃, be warming up to 65 ℃, constant temperature begins the vacuum decompression distillation dehydration after 0.5 hour;

Step 2,

When temperature of reaction is gone up to 67～70 ℃, stop the vacuum decompression distillation, and in reactor, add borax and boric acid in the component prescription, be warming up to 100 ℃ once more, constant temperature vacuum decompression distillation dehydration once more after 1 hour;

Step 3,

The question response temperature rises to 120 ℃ gradually and stops the vacuum decompression distillation, and blowing cooling at once is cooled to room temperature and obtains the solid state material, through pulverizing, packs, and is the finished product of bisphenol A-type boron bakelite resin.