Preparation method of boron modified phenolic resin

A phenolic resin, boron-modified technology, used in textiles and papermaking, one-component synthetic polymer rayon, chemical characteristics of fibers, etc. The effect of low cost and convenient operation

Active Publication Date: 2008-12-24
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The biggest disadvantage of the boron-modified phenolic resin prepared in this way is that it is very easy to hydrolyze. In melt spinning, the raw silk after spinning is very easy to hydrolyze and dissolve in the air.
Using the current common formaldehyde / hydrochloric acid aqueous curing system, once it is put into the curing liquid during the curing process, it will dissolve immediately, and the fiber cannot be cured and formed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1) In the first step, add 185g of 37% formaldehyde solution, 320g of phenol and 2g of oxalic acid in a 2500ml three-necked flask. After stirring well, heat the mixture. After reflux for 5 minutes, add 2 g of oxalic acid, continue to reflux for 1 hour, and add 1000 ml of deionized water. After the mixture is cooled, let it stand for 40 minutes, suck out the upper layer of water, and remove excess phenol and oxalic acid. Then, under the pressure of 8-12.6KPa, the temperature was raised to 110-120°C, and the reaction was carried out for 1-1.5h to obtain 280g of primary resin. 2) In the second step, dissolve 280g of the nascent resin with 1000ml of absolute ethanol, filter, steam distill, and repeat the operation twice, each time for 8h. Then add 10 g of triethanolamine borate ester, and carry out the third steam distillation for 8 hours. 3) In the third step, take out the resin in the lower layer and dissolve it with 1000ml of absolute ethanol, then add 18g of triethano...

Embodiment 2

[0025] 1) In the first step, add 185g of 37% formaldehyde solution, 235g of phenol and 2g of oxalic acid in a 2500ml three-necked flask. After stirring well, heat the mixture. After refluxing for 5 minutes, add 1.5 g of oxalic acid, continue refluxing for 1 hour, and add 1000 ml of deionized water. After the mixture is cooled, let it stand for 40 minutes, suck out the upper layer of water, and remove excess phenol and oxalic acid. Then, under the pressure of 8-12.6KPa, the temperature was raised to 110-120°C, and the reaction was carried out for 1-1.5h to obtain 270g of primary resin. 2) In the second step, dissolve 270g of the nascent resin in 1000ml of absolute ethanol, filter, steam distill, and repeat the operation twice, each time for 6h. Then add 10 g of triethanolamine borate ester, and carry out the third steam distillation for 6 hours. The preparation of boron-modified phenolic resin was the same as Example 1 except that the triethanolamine borate ester added in th...

Embodiment 3

[0027] 1) The first and second steps are the same as Example 1. 2) The third step is to dissolve the resin in the lower layer with 1000ml of absolute ethanol, then add 55g of triethanolamine borate, and disperse evenly with ultrasonic waves. Finally, heat up to 110° C. for 24 hours in a vacuum oven with a vacuum degree of 22.5 KPa to obtain a hydrolysis-resistant boron-modified phenolic resin for spinning. In the obtained modified phenolic resin, the boron content is 1.08%, the softening point temperature is 120-130 DEG C, and the spinnability evaluation is continuous and uniform. The phenolic fiber prepared after melt spinning can be solidified and formed by formaldehyde / hydrochloric acid aqueous solution system, the fiber is not swollen, insoluble and the B content in the obtained fiber is 0.48%.

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Abstract

This invention relates to a preparation method of boron modified phenol-formaldehyde resin used for imitation silk. The steps: mix formaldehyde and carbolic acid, whip uniformity, add oxalic acid for regurgitation, stand ing, heating-up underlayer solution to 110 - 120 deg under 8 to 12.6 kpa pressure, take reaction for 1 to 1.5 hours, then use absolute ethyl alcohol of 3 to 4 times quality for dissolution, wet distillation, then add borate, carry out wet distillation, take out lower resin and use absolute ethyl alcohol to dissolve, then use ultrasonic to disperse uniformity, finally at 20 to 25.3 KPa vacuum degree and 100 to 200 deg.C for 23 to 25 hours, gin waterproof boron modified phenol-formaldehyde resin used for imitation silk. This invention introduce a given mass of boron in bakelite, at the same time solve the problem of boron modified phenol-formaldehyde resin easily dissolve in water.

Description

technical field [0001] The invention belongs to a method for preparing a modified phenolic resin, in particular to a method for preparing a hydrolysis-resistant boron modified phenolic resin for melt spinning. Background technique [0002] Compared with ordinary phenolic resin, boron modified phenolic resin is a resin with better heat resistance and ablation resistance, and has excellent adhesion, dielectric properties, compression resistance and neutron absorption properties. Therefore, it is widely used in aerospace, aviation, rockets, missiles, space vehicles, nuclear power plants, nuclear submarines and automobile brake pads and other fields. The choice of boron to modify phenolic resin is based on: (1) The bond energy of B-O is higher. After the introduction of boron, the heat resistance and instantaneous high temperature resistance of the resin are greatly improved; (2) due to the introduction of B-O bond, the mechanical properties of the resin Performance and ablatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/28D01F6/58C08K5/55
Inventor 雷世文郭全贵宋进仁刘朗
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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