Synthesis process of p-tert-butyl phenol formaldehyde resin

A technology of p-tert-butylphenol and formaldehyde resin, which is applied in the field of synthesis of p-tert-butylphenol-formaldehyde resin, can solve the problems of severe strong alkali catalyzed reaction, reduced washing times, poor product stability, etc.

Inactive Publication Date: 2019-10-15
河北泽田化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] "Journal of Contemporary Chemical Industry" Volume 31 No. 1 introduces a new synthesis method of p-tert-butylphenol formaldehyde resin, which uses calcium hydroxide and 201 # The co-catalyst is used as a catalyst, although compared with the process of using sodium hydroxide as a catalyst to produce p-tert-butylphenol formaldehyde resin, the number of washings is reduced and the production cycle is shortened, but this method also has strong alkali catalyzed reactions and poor product stability. The problem is that the appearance of the p-tert-butylphenol formaldehyde resin product produced at the same time is translucent and poor in transparency

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0022] Turn on the stirring, put 100Kg of 37% formaldehyde solution into the reaction kettle under normal pressure, then add 10Kg of 25% ammonia water into the reaction kettle, and then add 100Kg evenly within 100 minutes at a temperature of 50-55°C For p-tert-butylphenol, heat up to boiling in 60 minutes, keep boiling for 150 minutes, cool down to 60°C, add 4.5Kg of acetic acid to neutralize, stir for 5 minutes, add 180Kg of toluene for extraction, then stop stirring and let stand for 10 minutes, Drain the wastewater from the valve at the bottom of the reactor, add 1.0kg of oxalic acid, then start stirring and add 80Kg of tap water, stir for 5 minutes, then stop stirring and let it stand for 10 minutes, then discharge the wastewater from the valve at the bottom of the reactor, and check the pH ≈ 7-7.5 , desolvation under normal pressure, temperature rises to 150°C, vacuumizes to -0.080MPa, softening point reaches 95-100°C and discharges to obtain p-tert-butylphenol formaldehyd...

Embodiment 2

[0024] Turn on the stirring, put 110Kg of 37% formaldehyde solution into the reaction kettle under normal pressure, then add 8Kg of 25% ammonia water into the reaction kettle, and then add 100Kg evenly within 95 minutes at a temperature of 50-55°C For p-tert-butylphenol, heat up to boiling in 70 minutes, keep boiling for 160 minutes, cool down to 65°C, add 3.5Kg of acetic acid to neutralize, stir for 10 minutes, add 180Kg of toluene for extraction, then stop stirring and let it stand for 15 minutes. Drain the wastewater from the valve at the bottom of the reactor, add 1.5kg of oxalic acid, then start stirring and add 70Kg of tap water, stir for 8 minutes, then stop stirring and let it stand for 12 minutes, then discharge the wastewater from the valve at the bottom of the reactor, and check the pH ≈ 7-7.5 , desolvation under normal pressure, temperature rises to 145°C, vacuumizes to -0.085MPa, softening point reaches 95-100°C and discharges to obtain p-tert-butylphenol formaldeh...

Embodiment 3

[0026] Turn on the stirring, put 100Kg of 37% formaldehyde solution into the reaction kettle under normal pressure, then add 9Kg of 25% ammonia water into the reaction kettle, and then add 100Kg evenly within 90 minutes at a temperature of 50-55°C For p-tert-butylphenol, heat up to boiling in 65 minutes, keep boiling for 160 minutes, cool down to 62°C, add 4.0Kg of acetic acid to neutralize, stir for 5 minutes, add 180Kg of toluene for extraction, then stop stirring and let stand for 20 minutes, Drain the wastewater from the valve at the bottom of the reactor, add 2.0kg of oxalic acid, then start stirring and add 70Kg of tap water, stir for 5 minutes, then stop stirring and let it stand for 16 minutes, then discharge the wastewater from the valve at the bottom of the reactor, and check the pH ≈ 7-7.5 , desolvation under normal pressure, temperature rises to 155°C, vacuumizes to -0.083MPa, softening point reaches 95-100°C and discharges to obtain p-tert-butylphenol formaldehyde ...

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Abstract

The invention belongs to the technical field of synthesis of p-tert-butylphenol formaldehyde resin, and discloses a synthesis process of p-tert-butylphenol formaldehyde resin. The synthesis process comprises the following steps: adding a formaldehyde solution and ammonia water into a reaction kettle; uniformly adding p-tert-butylphenol, then heating to boiling, and maintaining for 150-180 minutes;cooling, adding acetic acid, neutralizing and stirring, and adding toluene for extraction; after standing for layering, draining wastewater; adding oxalic acid and tap water, stirring, standing for layering, and then draining wastewater; detecting pH which approximates 7-7.5, desolventizing the toluene under normal pressure, vacuumizing, and discharging under vacuum to obtain tert-butyl phenol formaldehyde resin. According to the process, the ammonia water is alkalescent, so that reaction is relatively mild, and the p-tert-butyl phenol formaldehyde resin prepared by the method is stable in product index and stable in use performance.

Description

technical field [0001] The invention belongs to the technical field of p-tert-butylphenol formaldehyde resin, and specifically discloses a synthesis process of p-tert-butylphenol formaldehyde resin. Background technique [0002] The content of impurities determines the quality of p-tert-butylphenol formaldehyde resin, the less the content of impurities, the more stable the performance and the higher the transparency of the appearance. [0003] At present, sodium hydroxide or calcium hydroxide is used as a catalyst for the synthesis of p-tert-butylphenol formaldehyde resin. In the production process, it must be washed 3-5 times in order to obtain p-tert-butylphenol formaldehyde resin products with a transparent appearance; In addition, the two catalysts of sodium hydroxide or calcium hydroxide are strong basic catalysts, and the reactions are relatively violent. The molecular weight distribution of the generated p-tert-butylphenol formaldehyde resin is wide, which makes the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/12
CPCC08G8/12
Inventor 李晓贺胡春红李世聪孙国秀杨永信
Owner 河北泽田化工有限公司
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