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A kind of modified boron phenolic resin and its preparation method and application

A boron phenolic resin and silicon modification technology, applied in the field of modified phenolic resin and its preparation, can solve the problems of dispersibility of modified phenolic resin, ammonia escape, environmental pollution, etc., and achieve improved ablation resistance and mechanical properties Performance, improved thermal stability and flame retardancy, simple preparation method

Active Publication Date: 2019-02-26
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

The mass retention rate of this material at 800°C is about 75%. However, ammonia water and zinc acetate are used as catalysts in this method, and ammonia will escape during the later molding process, which will damage the health of the operator; the alkali metal ion Zn 2+ It will also have an adverse effect on the electrical properties of the material; and as the reaction progresses, the viscosity of the reaction system is increasing, and it is difficult for boric acid to react completely, and there are still dispersion problems
[0007] In addition to the above defects, the above-mentioned modified phenolic resin needs to use a catalyst in the preparation process. The introduced catalyst is difficult to remove in the post-treatment process. The alkaline earth metal in the catalyst is likely to cause communication interruption in the warhead guidance part, resulting in a decline in the precision strike performance of the warhead. ; or make the rocket engine wake, reduce the oxidation resistance of the material
In addition, in order to reduce the presence of free phenol during the synthesis of the above modified phenolic resin, excessive boric acid will be added, and unreacted boric acid will precipitate, resulting in the separation of resin and unreacted boric acid, resulting in the dispersion of the final modified phenolic resin. There is a problem with the property; and a large amount of waste water will be generated during the synthesis, which will pollute the environment

Method used

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  • A kind of modified boron phenolic resin and its preparation method and application
  • A kind of modified boron phenolic resin and its preparation method and application
  • A kind of modified boron phenolic resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] The preparation of embodiment 1 silicon modified boron phenolic resin

[0064] Preparation of boron phenolic resin: first suck 956g of molten phenol into the reactor by vacuum, add 155g of boric acid while stirring, slowly raise the temperature to 140°C at a rate of 0.5°C / min, and then gradually increase the temperature to 140°C at a rate of 0.2°C / min 164°C, then gradually increase the temperature to 181°C at a rate of 0.1°C / min, control the column head temperature not to exceed 98°C, collect fractions, stop heating when the weight of the fraction reaches 0.2 times the weight of phenol, and discard the fraction. Cool down to 60°C; add a total of 344g of paraformaldehyde into the reactor twice, control the heating rate at 0.2°C / min, and slowly raise the temperature to above 110°C until the reaction system starts to boil and reflux; after reflux for 30-40min, it begins to decrease Pressure dehydration. When the gel time of the reaction system reaches 60s (200±1°C), the r...

Embodiment 2

[0070] The preparation of embodiment 2 silicon modified boron phenolic resins

[0071]Preparation of boron phenolic resin: first suck 956g of molten phenol into the reactor by vacuum, add 155g of boric acid while stirring, slowly raise the temperature to 140°C at a rate of 0.7°C / min, and then gradually increase the temperature to 140°C at a rate of 0.1°C / min. 164°C, then gradually increase the temperature to 181°C at a rate of 0.2°C / min, control the column head temperature not to exceed 98°C, collect fractions, and stop heating when the weight of the fraction reaches 0.2 times that of phenol. Cool the distillate to 60°C, add 344g of paraformaldehyde twice, control the heating rate to 0.1°C / min, and slowly raise the temperature to above 110°C until the reaction system starts to boil and reflux; after reflux for 30-40min, start dehydration under reduced pressure. When the gel time of the reaction system reaches 50s (200±1° C.), the reaction ends, and 536 g of ethanol is added to...

Embodiment 3

[0074] The preparation of embodiment 3 silicon modified boron phenolic resins

[0075] Preparation of boron phenolic resin: Same as in Example 2, when preparing boron phenolic resin, discharge immediately after the final reaction, without adding ethanol, to obtain boron phenolic resin block solid.

[0076] Preparation of silicon-modified boron phenolic resin: Take 70g of boron phenolic resin solid and add it to the reaction kettle, slowly raise the temperature to 50-60°C to melt it completely, add 10g of ethyl orthosilicate, 30g of isopropyl orthosilicate and methyl orthosilicate Add 10 g of the ester into the separatory funnel, dropwise complete within half an hour, and react for 4 hours to obtain the silicon-modified boron phenolic resin.

[0077] Infrared spectrogram, thermogravimetric (TGA) curve and derivative thermogravimetric (DTG) curve are all similar to the results of Example 1, and will not be repeated one by one.

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Abstract

The invention discloses titanium-modified boron-containing phenolic resin as well as a preparation method and application thereof. The titanium-modified boron-containing phenolic resin is prepared from the following raw materials in parts by weight: 65-70 parts of boron-containing phenolic resin and 0.5-2 parts of titanate. The preparation method comprises the following steps that the titanate isdropwise added into the boron-containing phenolic resin, uniform mixing is carried out, and reaction is carried out at room temperature for 2-5 hours so as to obtain the titanium-modified boron-containing phenolic resin. According to the titanium-modified boron-containing phenolic resin as well as the preparation method and application thereof, a modified boron-containing phenolic resin solution is still transparent and uniform after being placed at room temperature for three months, no boric acid and other solid substances are separated out, the quality retention rate is also obviously increased, and the modified boron-containing phenolic resin is used in a flame-retardant composite material, a functional coating, a curing agent for epoxy resin, a rubber modifier and the like, so that thethermal stability and the flame retardancy of a product can be improved; and the preparation method is simple, no catalyst is used, and the hidden danger caused by incomplete removal of the catalystcan be avoided.

Description

technical field [0001] The invention relates to the technical field of modified phenolic resin and its preparation method and application, in particular to a modified boron phenolic resin obtained by modifying boron phenolic resin with heteroatoms and its preparation method and application. Background technique [0002] Phenolic resin raw materials are easy to obtain, low in price, and excellent in heat resistance, showing great application potential in the field of ablation-resistant and heat-resistant materials. Compared with other organic resins, the main advantage of phenolic resin as ablation-resistant material matrix resin is high quality retention rate, but phenolic resin degrades seriously during high-temperature ablation, and excessive ablation pits and grooves often appear after ablation. Ablation and unstable ablation phenomena. For this reason, technicians have carried out a lot of research on the modification of phenolic resins. Usually, high-temperature-resist...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L61/14C08K5/5415C08K5/10C08G8/28
CPCC08G8/28C08K5/10C08K5/5415C08K2201/014C08L2201/08C08L61/14
Inventor 田谋锋张力姚亚琳王雷张丹谈娟娟涂晨辰宋金梅
Owner 北京玻钢院复合材料有限公司
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