A kind of 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 of products, easy water absorption and caking, etc., and achieves reduced risk and low reaction temperature , Low water absorption effect

Inactive Publication Date: 2016-03-02
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] Put 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde into the reaction kettle, stir for half an hour, raise the temperature to 40°C, add 60.5kg of sodium hydroxide solution dropwise, and keep warm at 50°C for 2 hours after the addition. Raise the temperature to 80°C and keep it warm for 3 hours; lower the temperature to below 80°C, add 15kg of oxalic acid, and stir for 30 minutes; put in 642kg of resorcinol, raise the temperature to 110°C and reflux, react for 5 hours, remove toluene by atmospheric pressure distillation, and reach the temperature of the kettle at 150°C At about ℃, start toluene distillation under reduced pressure. During the decompression, control the vacuum degree to be higher than 0.08MPa, and the kettle temperature is about 160℃. Take samples every hour to detect the softening point. When the softening point reaches 99℃, start the granulator, turn on the material pump, and adjust Rotate the speed until the granules are semicircular, a...

Embodiment 2

[0025] Put 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde into the reaction kettle, stir for half an hour, raise the temperature to 50°C, add 60.5kg of potassium hydroxide solution dropwise, and keep the temperature at 55°C for 2 hours after the addition. Raise the temperature to 95°C and keep it warm for 3 hours; lower the temperature to below 80°C, add 15kg of oxalic acid, and stir for 30 minutes; put in 642kg of resorcinol, raise the temperature to 120°C and reflux, react for 5 hours, remove toluene by atmospheric pressure distillation until the kettle temperature is 150°C Start to distill toluene under reduced pressure, control the vacuum degree to be higher than 0.08MPa during decompression, and keep the temperature of the kettle at about 160°C. Take samples every hour to detect the softening point. When the softening point reaches 105°C, start the granulator, turn on the material pump, and adjust the speed. Until the particles are semicircular, the fini...

Embodiment 3

[0027] Put 840kg of p-cresol, 735L of toluene, and 249kg of paraformaldehyde into the reaction kettle, stir for half an hour, raise the temperature to 60°C, add 60.5kg of potassium hydroxide dropwise, and keep the temperature at 55°C for 2 hours after the addition. Raise the temperature to 100°C and keep it warm for 3 hours; lower the temperature to below 80°C, add 15kg of oxalic acid, and stir for 30 minutes; put in 642kg of resorcinol, raise the temperature to 100°C and reflux, react for 5 hours, remove toluene by atmospheric pressure distillation until the kettle temperature is 150°C Start to distill toluene under reduced pressure. During the decompression, control the vacuum degree to be higher than 0.08MPa, and the temperature of the kettle is about 160°C. Take samples every hour to detect the softening point. When the softening point reaches 109°C, start the granulator, turn on the material pump, and adjust the speed , until the particles are semicircular, the finished pr...

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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 method for preparing a resorcinol formaldehyde resin for modified rubber adhesives, belonging to the technical field of chemical adhesives. Background technique [0002] Resorcinol formaldehyde resin can be used as the methylene acceptor binder in m-methane-white system to replace resorcinol monomer (resorcinol monomer or resorcinol complex is used The dust in the process is too large and not environmentally friendly). Resorcinol formaldehyde resin can produce adhesion by reacting with methylene donors, and is used for bonding rubber and skeleton materials (such as metal skeleton and cord in tires), and can also be used as an additive for phenolic resins. To reduce processing time and lower processing temperature. 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...

Claims

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Application Information

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Patent Type & Authority Patents(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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