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
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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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