Method for preparing boron modified phenolic resin

A phenolic resin, boron modification technology, applied in the field of polymer synthesis and modification, can solve the problems of easy curing and crosslinking, poor storage stability, limited boron content, etc., achieve excellent heat resistance, increase reactivity, and improve boron content. The effect of the content of

Active Publication Date: 2015-04-22
沙县宏盛塑料有限公司
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Problems solved by technology

In this method, due to the low reactivity of phenol and boric acid, most boric acid cannot participate in the reaction. In the synthesized phenolic resin, boric acid will still be dispersed in the phenolic resin in the form of solid boric acid, and will be chemically bonded to the boron in the molecular chain of the phenolic resin. limited content
Chinese patent 200610024515.0 reports the use of a two-step method. First, phenol and boric acid are catalyzed by bases in organic solvents to synthesize borate esters, and then react with paraformaldehyde to synthesize boron-modified phenolic resins. This method can increase the boron content in phenolic resins. , but the boron-modified phenolic resin synthesized in an alkaline environment has strong activity and poor storage stability. In addition, the reaction is not easy to control during the synthesis process, and it is easy to...

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  • Method for preparing boron modified phenolic resin
  • Method for preparing boron modified phenolic resin
  • Method for preparing boron modified phenolic resin

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preparation example Construction

[0026] Further, the preparation method of boron modified phenolic resin of the present invention, comprises the steps:

[0027] 1) Add the organoboron compound and aldehyde into the reaction kettle, stir evenly, adjust the pH of the reaction solution to 8-12 with alkali, raise the temperature to 80-120°C, and react for 1-6h;

[0028] 2) Add phenol to the reaction solution obtained in step 1), adjust the pH to 2-5 with an acid, react at a temperature of 70-100° C. for 1-5 hours, and adjust the pH of the solution to 1-2 with an acid;

[0029] 3) Take the aldehyde, adjust the pH to 1-2 with an acid, add it to the reaction solution obtained in step 2), and react for 1-8 hours at a temperature of 80-120° C. to obtain a boron-modified phenolic resin.

[0030] Taking triphenyl borate, formaldehyde and phenol as examples, the main reaction formula is as follows:

[0031]

[0032] Among them, R 1 , R 2 ...R 9 independently selected from H or CH 2 OH, and R 1 , R 2 ...R 9 At ...

Embodiment 1

[0050] 1) Add 15 parts of triphenyl borate and 17 parts of 37% formaldehyde solution into the reaction kettle, stir evenly, adjust the pH of the reaction solution to 8-10 with sodium hydroxide, heat up to 95°C, and react for 4 hours;

[0051] 2) Add 100 parts of phenol to the reaction mixture obtained in step 1), adjust the pH to 2-3 with oxalic acid, raise the temperature to 90° C., react for 3 hours, and adjust the pH of the solution to 1-2 with hydrochloric acid;

[0052] 3) Take 65 parts of 37% formaldehyde solution, adjust the pH to 1-2 with oxalic acid, add it to the reaction solution obtained in step 2), and react for 3 hours at a temperature of 100 ° C. After dehydration, branched with high boron content is obtained. Boron modified phenolic resin.

[0053] After testing, the obtained boron-modified phenolic resin has a molecular weight of 3553 and a boron content of 0.5%.

Embodiment 2

[0055] 1) Add 10 parts of L-norvalyl diphenyl borate and 18 parts of 37% formaldehyde solution into the reaction kettle, stir evenly, adjust the pH of the reaction solution to 8-10 with potassium hydroxide, and heat up to 100°C , reaction 4h;

[0056] 2) Add 100 parts of phenol to the reaction mixture obtained in step 1), adjust the pH to 2-3 with phosphonic acid, raise the temperature to 95° C., react for 3 hours, and adjust the pH of the solution to 1-2 with oxalic acid;

[0057] 3) Take 69 parts of 37% formaldehyde solution, adjust the pH to 1-2 with hydrochloric acid, add it to the reaction solution obtained in step 2), and react for 4 hours at a temperature of 100°C. After dehydration, a branched product with high boron content is obtained. Boron modified phenolic resin.

[0058] After testing, the weight-average molecular weight of the obtained boron-modified phenolic resin is 3764, and the content of boron connected to the resin by chemical bonds is 0.3%.

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Abstract

The invention discloses a method for preparing boron modified phenolic resin. A three-step method is adopted, and the three-step method comprises the following steps: firstly, reacting an organic boron compound with aldehyde under an alkaline condition to generate hydroxymethylated organic boron, then pre-polymerizing the hydroxymethylated organic boron with phenol under an acidic condition to form a short chain pre-polymer, and finally copolymerizing the short chain pre-polymer with aldehyde under the acidic condition to form branched boron modified phenolic resin with a high boron content. By adopting the method disclosed by the invention, the reaction activity of the boron compound is improved, the boron content in a molecular chain segment of the phenolic resin is improved, high molecular weight phenolic resin with a branch chain structure can be prepared, and the prepared boron modified phenolic resin is high in boron content and is excellent in heat resistance.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis and modification, in particular to a preparation method of boron-modified phenolic resin. Background technique [0002] Phenolic resin (PF) has rich sources of raw materials, low price, simple production process, excellent mechanical properties, heat resistance, electrical insulation, dimensional stability, molding processability and flame retardancy, good dimensional stability of products, electrical insulation With excellent performance and low smoke emission, it has become an indispensable material in the industrial sector, and has been widely used in related industries such as automobiles, home appliances, electrical appliances, steel and housing. [0003] However, with the development of industry, especially the development of aerospace and other cutting-edge defense technologies, new requirements have been put forward for phenolic resins, which cannot be met with pure phenolic resi...

Claims

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Application Information

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IPC IPC(8): C08G8/28
Inventor 罗建峰黄世俊陈银桂朱光明翟苏宇
Owner 沙县宏盛塑料有限公司
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