Modified m-cresol-phenol-formaldehyde resin, preparation method and rubber composition modified from modified m-cresol-phenol-formaldehyde resin

A technology of rubber composition and formaldehyde resin, which is applied in the field of rubber processing aids, can solve complex and other problems, and achieve the effects of improving storage performance, improving water resistance, and low content

Active Publication Date: 2019-01-08
JIANGSU QIXIANG HIGH NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its synthesis method is divided into two stages of polymerization, and formaldehyde is add

Method used

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  • Modified m-cresol-phenol-formaldehyde resin, preparation method and rubber composition modified from modified m-cresol-phenol-formaldehyde resin
  • Modified m-cresol-phenol-formaldehyde resin, preparation method and rubber composition modified from modified m-cresol-phenol-formaldehyde resin
  • Modified m-cresol-phenol-formaldehyde resin, preparation method and rubber composition modified from modified m-cresol-phenol-formaldehyde resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Add m-cresol 88g (0.8mol) and p-toluenesulfonic acid 2.9g to a 1L four-necked round-bottom flask equipped with stirring, temperature control, reflux condenser and constant pressure dropping funnel, and heat to 130°C, drop by drop Styrene 74.9 (0.72mol), after adding dropwise, keep warm for 90min, then add 94g (1mol) of phenol, then cool down to 100°C, add 103.0g of 37% formaldehyde (1.22mol) dropwise, keep warm for 90min after dropping, heat up to normal pressure Distill to 160°C, and distill at -0.08mpa for 60min under reduced pressure to obtain 258g of modified m-cresol-phenol-formaldehyde resin with a softening point of 105°C.

Embodiment 2

[0061] Add cresol 176g (1.6mol) in the 1L four-neck round-bottomed flask that is equipped with stirring, temperature control, reflux condenser and constant pressure dropping funnel, wherein m-cresol content is 70% and p-toluenesulfonic acid 1.1g, 1.1g of oxalic acid, heated to 130°C, added dropwise 108.2 (1.04mol) of styrene, kept warm for 90 minutes after the dropwise addition, then added 94g (1mol) of phenol, cooled to 100°C, then added dropwise 155.3g of 37% formaldehyde ( 1.87mol), after the dropwise addition, keep warm for 90min, heat up and distill at normal pressure to 160°C, and distill under reduced pressure at -0.08mpa for 60min to obtain 370g of modified m-cresol-phenol-formaldehyde resin with a softening point of 95°C.

Embodiment 3

[0063] Add m-cresol 132g (1.2mol) in a 1L four-neck round bottom flask equipped with stirring, temperature control, reflux condenser and constant pressure dropping funnel, wherein m-cresol content is 99.5% and p-toluenesulfonic acid 1.36g Heat to 130°C, add styrene 114.4 (1.1mol) dropwise, keep the temperature for 90 minutes after the dropwise addition, then add 94g (1mol) phenol, cool down to 100°C, then add 127.8g of 37% formaldehyde (1.54mol) dropwise, After the dropwise addition, keep the temperature for 90 minutes, raise the temperature and distill to 160°C under normal pressure, and then distill under reduced pressure at -0.08mpa for 60 minutes to obtain 342g of modified m-cresol-phenol-formaldehyde resin with a softening point of 98°C.

[0064] The specific relevant performance tests are as follows:

[0065] (1) The results of free phenol content are shown in Table 1.

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Abstract

The invention provides modified m-cresol-phenol-formaldehyde resin, a preparation method and a rubber composition modified from modified m-cresol-phenol-formaldehyde resin. The resin is prepared by reacting the materials which comprise cresol, a modifying agent X, phenol and at least one aldehyde in the presence of an acid catalyst; the softening point of the prepared modified m-cresol-phenol-formaldehyde resin is 90 to 110 DEG C; the content of free phenol in the resin is 0.3 to 1 percent of that of the resin; the content of alkyl free phenol in the resin is 0.3 to 1 percent of that of the resin; and the glass-transition temperature of the resin is 55 to 65 DEG C. The preparation method disclosed by the invention is simple and is low in cost; the content of the free phenol and the alkyl free phenol of the prepared modified m-cresol-phenol-formaldehyde resin is greatly reduced; moreover, the m-cresol-phenol-formaldehyde resin has comparative adhesion property with that of resorcinol adhesive resin; in addition, the water resistance of the phenolic aldehyde adhesive resin is improved; and the storage performance of a product is improved.

Description

technical field [0001] The invention relates to the field of rubber processing aids, in particular to a modified m-cresol-phenol-formaldehyde resin, a preparation method and a rubber composition thereof Background technique [0002] In reinforced rubber products, fiber, nylon, steel wire, etc. are used as the supporting skeleton structure, and a meta-formula-white bonding reinforcement system is used between the supporting skeleton structure and the rubber to improve the adhesion between the rubber and the skeleton. At present, resorcinol-hexamethylenetetramine-silica is commonly used. In the vulcanization process, silica catalyzes methylene to give hexamethylenetetramine to release formaldehyde, and formaldehyde reacts with resorcinol to form a network structure, which can improve the mechanical and adhesive properties of vulcanized rubber. [0003] Due to the low smoke point and high toxicity of resorcinol, the resorcinol used in the rubber mixing process is being gradual...

Claims

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Application Information

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IPC IPC(8): C08G8/24C08G8/12C08G8/10C08L9/00C08L11/00C08L9/02C08L9/06C08L61/08
CPCC08G8/10C08G8/12C08G8/24C08L9/00C08L9/02C08L9/06C08L11/00C08L61/06
Inventor 彭华龙高峰王莹莹姚翔尹兴昌
Owner JIANGSU QIXIANG HIGH NEW MATERIAL
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