Preparation method of copolymerization condensation resin

A condensed resin and copolymerization technology is applied in the field of preparation of co-condensed resin for rubber, which can solve the problems of long viscosity retention time, insufficient retention and high cost, and achieve the effects of simple production process, improved adhesion and easy industrial production.

Inactive Publication Date: 2013-06-26
徐川大
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Synthetic rubbers such as SBR, BR, NBR, IIR, and CR lack adhesiveness compared with natural rubber. In order to improve the self-adhesiveness or adhesiveness of synthetic rubber, some resins are often used in the rubber industry. As a tackifier, there are alkyl Phenol formaldehyde resin, alkylphenol acetylene resin, coumarone resin, xylene formaldehyde resin, petroleum resin, etc. These resins can be used alone or in combination in terms of price and performance. Different combinations can achieve different tackifying effects, especially in the rubber composition of automobile radial tires, p-tert-butylphenol acetylene resin is recognized as a high-quality tackifying resin, and the rubber composition containing p-tert-butylphenol acetylene resin Its natural rubber and synthetic rubber have high adhesiveness when they are not vulcanized, and the viscosity retention time is long, but the conditions for making p-tert-butylphenol acetylene resin are relatively harsh, and the cost is high, while conventional alkylphenol formaldehyde resin Adhesive, but not sufficient, and poor viscosity retention, for a long time, the industry has been researching and developing low-cost, easy-to-industrial production, affordable, tackifying resin with excellent viscosity, based on the current radial tire Rapid development, there is such a special demand in the tire industry

Method used

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  • Preparation method of copolymerization condensation resin
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  • Preparation method of copolymerization condensation resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Put 225g of p-tert-butylphenol, 28g of morpholine and 3.5g of the catalyst triethylamine into a 1000ml four-necked flask equipped with a stirring device, a reflux condenser, a liquid addition device, a receiving device and a thermometer. Start stirring. When the temperature is between 60°C and 75°C, slowly add 156.6g of 37% formaldehyde. At this time, it is an exothermic reaction. Control the temperature between 90°C and 100°C to maintain the reaction for 1 hour, and then add resorcinol 12g, react for another 1 hour, the reaction is over, the reflux condenser is switched to the receiving state, heated to increase the temperature, start dehydration recovery, when the temperature reaches 160℃, build a vacuum, continue dehydration and free phenol under reduced pressure, at 185~210 The reaction is maintained at °C until the softening point reaches the requirement, 15 g of paraffin wax is added and stirred uniformly to obtain the resin of the present invention. The softening ...

Embodiment 2

[0031] Put 225g of p-tert-butylphenol, 28g of morpholine and 3.5g of the catalyst triethylamine into a 1000ml four-necked flask equipped with a stirring device, a reflux condenser, a liquid addition device, a receiving device and a thermometer. Start stirring. When the temperature is between 60°C and 75°C, slowly add 156.6g of 37% formaldehyde. At this time, it is an exothermic reaction. Control the temperature at 90°C to 100°C to maintain the reaction for 1 hour, then add 12g of m-cresol and react again. After 1 hour, the reaction is over, the reflux condenser is switched to the receiving state, the temperature is increased, and the dehydration recovery is started. When the temperature reaches 160°C, a vacuum is established, and the dehydration and free phenol are continued under reduced pressure, and the reaction is maintained at 185-210°C. Until the softening point reaches the requirement, 15 g of paraffin wax is added and stirred evenly to obtain the resin of the present inv...

Embodiment 3

[0033] Put 309 g of p-tert-octylphenol, 28.8 g of morpholine and 6.5 g of the catalyst triethylamine into a 1000 ml four-necked flask equipped with a stirring device, a reflux condenser, a liquid addition device, a receiving device and a thermometer, and heat to dissolve, Then start stirring. When the temperature is 80℃~85℃, 160.5g 37% formaldehyde is slowly added dropwise. At this time, it is an exothermic reaction. Control the temperature at 90℃~100℃ to maintain the reaction for 1 hour, and then add 16.5g resorcinol After reacting for another 1 hour, the reaction is over, the reflux condenser is switched to the receiving state, the heating is increased, and the dehydration recovery is started. When the temperature reaches 160°C, a vacuum is established, and the dehydration and free phenol are continued under reduced pressure at 160~195°C. The reaction is maintained until the softening point reaches the requirement, and 19 g of paraffin wax is added and stirred evenly to obtain...

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Abstract

The invention discloses a preparation method of copolymerization condensation resin. The preparation method is characterized by comprising the following steps of: 1) putting para-position alkylphenol and other phenols, aldehydes, amines and catalysts, and carrying out reaction for 1-5 hours at the temperature of 60-160 DEG C; and 2) after the reaction is finished, carrying out distillation and concentration, and maintaining the temperature to be 140-220 DEG C until the temperature of a softening point is 90-145 DEG C. The preparation method disclosed by the invention has the beneficial effects that firstly the copolymerization condensation resin prepared by adopting the preparation method disclosed by the invention has improved adhesiveness and the viscosity retention rate is excellent, the copolymerization condensation resin also has the effect of enhancing a bonding force between rubber and a framework material, and the tackifying effect of the copolymerization condensation resin is equivalent to that of p-tert-butylphenol acetylene resin and is better than that of the existing alkylphenol formaldehyde tackifying resin; and secondly a production process is simple, and industrial production is easy to achieve.

Description

technical field [0001] The invention relates to an organic resin and a preparation method thereof, in particular to a preparation method of co-condensation resin for rubber. Specifically, the present invention relates to the preparation of co-condensation resins by one or more phenols, aldehydes, and amines under alkaline or acidic catalyst conditions. From the perspectives of price and performance, the co-polymerization resins can be used alone or further The modified resin is compounded or mixed with a modifier to obtain a modified resin. Due to its unique resin structure, the polarity is increased, the compatibility with rubber is improved, and it has remarkable heat resistance, moisture resistance and oxidation resistance. Not only It can endow the rubber with good adhesion and viscosity retention rate, and has the characteristics of improving the adhesion between rubber and skeleton materials. Its viscosity-increasing effect is equivalent to that of p-tert-butylphenol ace...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/12C08G14/09C08G14/073C08L21/00C08L9/06C08L61/34
Inventor 徐川大
Owner 徐川大
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