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Preparation method of resorcinol formaldehyde resin for modified rubber adhesive

A technology of resorcinol formaldehyde resin and modified rubber, which is applied in the field of chemical adhesives, can solve the problems of complex production process, high water content in products, easy to absorb water and agglomerate, and achieve reduced risk and low reaction temperature. , the effect of low water absorption

Inactive Publication Date: 2014-07-23
SHANGHAI LUCKY BIOLOGICAL & CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The application range of resorcinol formaldehyde resin includes: production of sandpaper, grinding wheel, clutch material, plywood adhesive, etc., the usual production is to use resorcinol and formaldehyde aqueous solution as raw materials, add resorcinol, Inorganic salt and organic solvent, then add formaldehyde aqueous solution dropwise under the action of acid catalyst, synthesize by liquid-liquid heterogeneous reaction, then remove the water layer, then extract with organic solvent, wash with water, and finally distill off the organic solvent to obtain m-benzene Diphenol formaldehyde resin, such a production process is complicated; the product has high water content; resorcinol is easily released during use, which is not environmentally friendly; it is highly volatile and easy to absorb water and agglomerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde were put into the reactor, stirred for half an hour, warmed up to 40°C, dripped 60.5kg of sodium hydroxide solution, and was incubated at 50°C for 2 hours after the dripping finished, and after the insulation finished Be warming up to 80 ℃, be incubated 3 hours; Be cooled to below 80 ℃, add 15kg of oxalic acid, stir for 30 minutes; Throw in 642kg of resorcinol, be warming up to 110 ℃ of reflux, react 5 hours, remove toluene by atmospheric distillation, to still temperature 150 ℃ At about ℃, start to distill toluene under reduced pressure, control the vacuum degree to be higher than 0.08MPa during decompression, and the temperature of the kettle is about 160℃, take samples every hour to check the softening point, when the softening point reaches 99℃, start the granulator, turn on the feed pump, adjust Speed ​​until the particles are semi-circular, and the finished product is about 1600kg.

Embodiment 2

[0025] 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde were dropped into the reactor, stirred for half an hour, heated to 50°C, dripped with potassium hydroxide solution 60.5kg, and was incubated at 55°C for 2 hours after the dripping finished, and after the insulation finished Be warming up to 95 ℃, be incubated 3 hours; Be cooled to below 80 ℃, add 15kg of oxalic acid, stir for 30 minutes; Throw in 642kg of resorcinol, be warming up to 120 ℃ of reflux, react 5 hours, remove toluene to still temperature 150 ℃ by atmospheric distillation Start to distill toluene under reduced pressure, control the vacuum degree to be higher than 0.08MPa during decompression, the temperature of the kettle is about 160 ℃, take samples every hour to check the softening point, when the softening point reaches 105 ℃, start the granulator, turn on the material pump, adjust the rotation speed, When the particles are semicircular, the finished product is about 1600kg.

Embodiment 3

[0027] 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde were put into the reaction kettle, stirred for half an hour, and heated to 60 ℃, dripped potassium hydroxide 60.5kg, and was incubated at 55 ℃ for 2 hours after the dripping finished, and after the insulation finished Be warming up to 100 DEG C, keep warm for 3 hours; Be cooled to below 80 DEG C, add 15kg of oxalic acid, stir for 30 minutes; Throw in 642kg of resorcinol, be warming up to 100 DEG C reflux, react for 5 hours, remove toluene to still temperature 150 DEG C by atmospheric distillation Around, start to distill toluene under reduced pressure, control the vacuum degree to be higher than 0.08MPa during decompression, the temperature of the kettle is about 160 ℃, take samples every hour to check the softening point, when the softening point reaches 109 ℃, start the granulator, turn on the material pump, and adjust the rotational speed , until the particles are semi-circular, and the finished product...

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Abstract

The invention discloses a preparation method of a resorcinol formaldehyde resin for a modified rubber adhesive, which comprises the following steps: a) adding p-alkylphenol and polyformaldehyde into an organic solvent, and stirring uniformly at 40-70 DEG C; b) dropwisely adding an alkali solution, and keeping the temperature for 1-4 hours; c) heating the product obtained in the step b) to 80-100 DEG C, keeping the temperature for 2-4 hours, and cooling to 90 DEG C below; d) adding an acidity regulator into the product obtained in the step c), stirring, adding resorcinol, heating to 100-150 DEG C, and reacting under reflux for 2-5 hours; and e) removing the organic solvent from the product obtained in the step b), and starting granulation when the softening point of the product is 99-109 DEG C to obtain the granular resorcinol formaldehyde resin. The method uses polyformaldehyde instead of the formalin, and has the advantages of simple material feeding and lower risk.

Description

technical field [0001] The invention relates to a preparation method of resorcinol formaldehyde resin used for modified rubber adhesive, and belongs to the technical field of chemical adhesives. Background technique [0002] Resorcinol formaldehyde resins can be used as methylene acceptor binders in m-methyl-white systems to replace resorcinol monomers (resorcinol monomers or resorcinol complexes are used in The dust is too large in the process, which is not environmentally friendly). Resorcinol formaldehyde resin can produce adhesion by reacting with methylene donors, used for the adhesion of rubber and skeleton materials (such as metal skeleton and cord in tires), and can also be used as an additive for phenolic resins. In order to reduce processing time and reduce processing temperature. The application scope of resorcinol formaldehyde resin includes: production of sandpaper, grinding wheel, clutch material, plywood adhesive, etc. The usual production is to use resorcin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/24
Inventor 罗刚张良张少刚李新
Owner SHANGHAI LUCKY BIOLOGICAL & CHEM TECH
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