Preparation method of titanium modified phenolic resin

A technology of phenolic resin and boron phenolic resin, which is applied in the field of preparation of titanium-modified phenolic resin, can solve the problems that it is difficult to form a uniform solution, must be sealed and stored, and the reaction is not easy to control, so as to save the preparation cost, suitable for storage, and easy to operate Effect

Active Publication Date: 2021-02-26
北京玻钢院复合材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the above-mentioned patent documents, nano-TiO 2 Particles are easy to agglomerate and unevenly dispersed in the above reaction system
[0006] In addition, in the prior art, titanate is generally used to directly modify boron phenolic resin, but titanate reacts rapidly with water to produce TiO 2 Precipitation, and the amount of addition is very small, the reaction is not easy to control, it is easy to gel, it is difficult to form a uniform solution, and must be sealed and stored to prevent the titanate bond from being hydrolyzed after water absorption to form a precipitate

Method used

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  • Preparation method of titanium modified phenolic resin

Examples

Experimental program
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Effect test

preparation example 1

[0026] The ethanol solution of preparation example 1-boron phenolic resin

[0027] First suck 956g of molten phenol into the reactor by vacuum, add 210g of boric acid while stirring, slowly raise the temperature to 140°C at a rate of 0.4°C / min, then gradually raise the temperature to 164°C at a rate of 0.1°C / min, and then Gradually raise the temperature to 181°C at a rate of 0.1°C / min, control the column head temperature to not exceed 98°C, collect fractions, stop heating when the weight of the fraction reaches 0.2 times that of phenol, discard the fraction, and the remaining product in the reactor is boric acid phenol ester. Lower the temperature of the boric acid phenol ester to below 60°C; add 303g of paraformaldehyde twice, control the heating rate to 0.5°C / min, and slowly raise the temperature to above 110°C until the reaction system starts to boil and reflux; after reflux for 30 to 40 minutes, it begins to decrease Pressure dehydration. When the gel time of the reactio...

Embodiment 1

[0029] (1) At 20°C, add 13g of butyl titanate into 120g of acetylacetone under stirring, and continue stirring until a uniform mixed solution A1 is formed.

[0030](2) At 20°C, under stirring, the above-mentioned mixed solution A1 was added dropwise at a constant speed and slowly to 700g of ethanol solution of boron phenolic resin with a glue content of 60wt%; the rate of addition was 4.5ml / min; the stirring speed was 200r / min.

[0031] (3) After the dropwise addition, continue stirring at 20° C. for half an hour at a stirring speed of 200 r / min to obtain titanium-modified boron phenolic resin B1, which is an orange-red, transparent solution.

[0032] The mass retention rate at 800°C of the titanium-modified boron phenolic resin B1 in Example 1 was 70%. See Table 1 for the performance of storage stability of the titanium-modified boron phenolic resin B1 in Example 1.

Embodiment 2

[0034] (1) At 20° C., add 22 g of isopropyl titanate into 140 g of acetylacetone under stirring, and continue stirring until a uniform mixed liquid A2 is formed.

[0035] (2) at 20 DEG C, under stirring, the above-mentioned mixed solution A2 is added dropwise at a constant speed and slowly to the ethanol solution of 60wt% barium phenolic resin with a glue content of 700g; the rate of addition is 5.5ml / min; the stirring speed is 200r / min.

[0036] (3) After the dropwise addition, continue to stir at 20° C. for half an hour at a stirring speed of 200 r / min to obtain a titanium-modified barium phenolic resin, which is an orange-red, transparent solution.

[0037] See Table 1 for the performance of the storage stability of the titanium-modified barium phenolic resin in Example 2.

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Abstract

The invention discloses a preparation method of titanium modified phenolic resin. The preparation method comprises the following steps: mixture solution A made from titanate ester and acetylacetone isstirred and slowly dripped into the ethanol solution of phenolic resin under 15-30 DEG C, and stirring is performed for 0.1-1 hour under 15-30 DEG C, so as to obtain the titanium modified phenolic resin, wherein the content of glue contained in the ethanol solution of the phenolic resin is 50-70 wt%, and the weight ratio of the ethanol solution of the phenolic resin to the acetylacetone to the titanate ester is 100:(7-40):(0.8-5). The titanium modified phenolic resin prepared by the invention has the advantages of being uniform in distribution system, good in stability and suitable for storage.

Description

technical field [0001] The invention relates to a preparation method of titanium modified phenolic resin, in particular to a preparation method of titanium modified phenolic resin with better dispersibility and better storage stability. Background technique [0002] The heat resistance of ordinary phenolic resin is not ideal, and its thermal decomposition phenomenon is quite serious when it exceeds 300°C, and the residual carbon rate is only about 40% at high temperature (above 800°C). In order to improve the heat resistance of phenolic resin, it needs to be modified. [0003] Boron modified phenolic resin (boron phenolic resin) is an effective way to improve the heat resistance of phenolic resin. Since the hydrogen in the phenolic hydroxyl group is replaced by boron, the B-O bond energy is much greater than the C-C bond energy, and the boron carbide honeycomb structure formed on the surface of the resin during high temperature pyrolysis can prevent the heat from diffusing ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/28
CPCC08G8/28
Inventor 张力田谋锋孙燚王雷姚亚琳魏旭刘晶涂晨辰宋金梅孙洪鑫
Owner 北京玻钢院复合材料有限公司
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