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Method for preparing novolac epoxy resin by utilizing vanillin production waste liquid

A technology of novolac epoxy resin and vanillin, which is applied in the fields of chemical industry and polymer materials, can solve the problems of secondary pollution, high cost, and low production efficiency of enterprises, and achieve the effect of solving difficult problems and realizing comprehensive utilization

Inactive Publication Date: 2018-01-05
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the difficulty in the treatment of phenol-containing wastewater from the production of vanillin is that after the adsorption and saturation of the macroporous adsorption resin, it is necessary to use an organic solvent or alkaline solution to desorb the phenol-containing organic matter. The cost remains high, there is a risk of secondary pollution, and the production efficiency of the enterprise is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add 600 g of vanillin production waste liquid containing phenolic organic matter with a mass concentration of 25% into the reaction flask, adjust the pH of the solution to 1.5-2 with a 10% aqueous solution of hydrochloric acid, and add formaldehyde solution with a mass concentration of 37% under stirring 81g, polymerized at 70°C for 2h to generate thermoplastic novolak polymer. To the reaction solution, 33g of aqueous sodium hydroxide solution, 4g of dodecyltrimethylammonium chloride surfactant and 45g of epichlorohydrin were further added with a concentration of 30% by mass, and the condensation reaction was carried out at 70°C for 2h. Alkoxylate about 50% of the phenolic hydroxyl groups in the novolak polymer molecule, add 33 g of 30% sodium hydroxide aqueous solution and continue the reaction for 2 hours, so that the chlorohydrins in the polymer molecule are cyclized to form epoxy groups. Vacuum distillation recovers the residual epichlorohydrin and evaporated solven...

Embodiment 2

[0019] Add 600 g of vanillin production waste liquid containing phenolic organic matter with a mass concentration of 25% into the reaction flask, adjust the pH of the solution to 1.5-2 with a 10% aqueous solution of hydrochloric acid, and add formaldehyde solution with a mass concentration of 37% under stirring 40g, polymerized at 50°C for 2h to generate novolac polymer. Further adding 16g of aqueous sodium hydroxide solution with a mass percent concentration of 30%, 2g of dodecyltrimethylammonium chloride surfactant and 23g of epichlorohydrin into the reaction solution, carried out condensation reaction at 60°C for 2h, Alkoxylate about 25% of the phenolic hydroxyl groups in the novolac polymer molecule, add 16 g of 30% sodium hydroxide aqueous solution and continue the reaction for 2 hours, so that the chlorohydrins in the polymer molecule are cyclized to form epoxy groups. Vacuum distillation recovers residual epichlorohydrin and evaporated solvent water, dissolves the disti...

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Abstract

The invention relates to a method for preparing novolac epoxy resin by utilizing vanillin production waste liquid. A polymerization reaction is performed on the waste liquid containing 20% to 30% of o-vanillin, 10% to 15% of isovanillin, 10% to 15% of vanillin, 10% to 15% of dimerized vanillin, 15% to 20% of vanillic acid, 5% to 10% of mandelic acid and 5% to 10% of dimerized mandelic acid and formaldehyde solution to generate a linear phenolic polymer. Under the condition of existence of sodium hydroxide and a surfactant, a condensation reaction is further performed on the linear phenolic polymer and epichlorohydrin to obtain the novolac epoxy resin of which an epoxy value is 0.1 to 0.27mol / 100g and a viscosity is 1.5 to 3.0mPa.s. According to the invention, the novolac epoxy resin is prepared by the vanillin production waste liquid, so that the difficult problem of treating the vanillin production waste liquid is solved, comprehensive utilization of waste is implemented, production cost of the novolac epoxy resin is greatly reduced, and product performance of the novolac epoxy resin is improved.

Description

technical field [0001] The invention relates to a method for preparing novolac epoxy resin by using vanillin production waste liquid, especially a method for preparing novolac epoxy resin by using vanillin high-concentration phenol-containing waste liquid of glyoxylic acid method as a raw material, and belongs to the field of chemical industry and polymer materials . Background technique [0002] Vanillin (English name Vanillin) is a white needle-like crystal, the chemical name is 3-methoxy-4-hydroxybenzaldehyde, and the chemical formula is C 8 h 8 o 3 , molecular weight 152.2, melting point 81-83°C, boiling point 284°C, slightly soluble in water, soluble in ethanol and chloroform, with vanilla aroma and strong milky aroma. There are many industrial production routes of vanillin. Considering the production cost and environmental protection, the glyoxylic acid method is widely used at home and abroad. Inventor once in "Jiangsu Chemical Industry" 1993, the 3rd period, the ...

Claims

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Application Information

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IPC IPC(8): C08G59/08
Inventor 李建生李霞张腾葸彦娇
Owner TIANJIN VOCATIONAL INST
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