A kind of preparation method of resorcinol formaldehyde resin for alkylphenol modified rubber adhesive

A technology of resorcinol formaldehyde resin and modified rubber, which is applied in the direction of adhesives, adhesive types, aldehyde/ketone condensation polymer adhesives, etc., and can solve complex production processes, high water content of products, and easy water absorption Agglomeration and other problems, to achieve the effects of reduced risk, low reaction temperature, and low water absorption

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 400kg of p-octylphenol, 400kg of m-cresol, 800L of toluene, and 250kg of paraformaldehyde into the reaction kettle and stir for half an hour. After stirring for half an hour, the temperature was raised to 50°C, and 60.5kg of sodium hydroxide solution with a mass fraction of 25% was added dropwise. After the dropwise addition, keep the temperature at 50-55°C for 3 hours, raise the temperature to 95°C after the end of the heat preservation, and keep the temperature for 3 hours; cool down to below 80°C, add 15kg of oxalic acid, and stir for 30 minutes; put in 660kg of resorcinol, and heat up to 100 Reflux at ℃, react for 5 hours, remove toluene by distillation at atmospheric pressure until the temperature of the kettle is about 150℃, 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℃, take samples every hour to detect the softening point, When the...

Embodiment 2

[0025] Put 420kg of p-octylphenol, 420kg of p-cresol, 800L of toluene, and 250kg of paraformaldehyde into the reactor and stir for half an hour. After stirring for half an hour, the temperature was raised to 50°C, and 60.5kg of sodium hydroxide solution with a mass fraction of 25% was added dropwise. After the dropwise addition, keep the temperature at 50-55°C for 3 hours, raise the temperature to 95°C after the end of the heat preservation, and keep the temperature for 3 hours; cool down to below 80°C, add 15kg of oxalic acid, and stir for 30 minutes; put in 660kg of resorcinol, and heat up to 150 Reflux at ℃, react for 5 hours, remove toluene by atmospheric pressure distillation until the temperature of the kettle is about 150℃, 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℃, take samples every hour to detect the softening point, When the softening ...

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Abstract

The invention discloses a preparation method of a resorcinol formaldehyde resin for an alkylphenol modified rubber adhesive, which comprises the following steps: a) adding 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 oxalic acid 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 for alkylphenol 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 formaldeh...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/24C09J161/12
Inventor 罗刚张良张少刚李新
Owner SHANGHAI LUCKY BIOLOGICAL & CHEM TECH
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