Maleic anhydride modified p-tert-butylphenol formaldehyde resin and synthesis method thereof

A technology with properties of p-tert-butylphenol and maleic anhydride, applied in the field of maleic anhydride-modified p-tert-butylphenol-formaldehyde resin and its synthesis, can solve problems such as limited improvement in tackifying properties, and achieve improved lasting viscosity and reduced The effect of heat generation and improvement of anti-aging ability

Active Publication Date: 2020-06-26
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen from the structure of the resin that compared with the traditional alkylphenol-formaldehyde resin, the resin obtained in this patent only has a vinyl structure connected at the end point, and the improvement in tackifying performance is limited.

Method used

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  • Maleic anhydride modified p-tert-butylphenol formaldehyde resin and synthesis method thereof
  • Maleic anhydride modified p-tert-butylphenol formaldehyde resin and synthesis method thereof
  • Maleic anhydride modified p-tert-butylphenol formaldehyde resin and synthesis method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A kind of synthetic method of maleic anhydride modified p-tert-butylphenol formaldehyde resin, comprises the following steps:

[0035] Step 1: Take by weighing p-tert-butylphenol 100g (0.67mol), concentrated sulfuric acid 0.17g, add in the 250ml four-necked round bottom reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are housed, be warmed up to 90 ℃, add dropwise 43.5g formaldehyde aqueous solution (phenol-formaldehyde ratio 1:0.8), and continue to react for 1 hour; after the reaction, raise the temperature to 100℃ to distill the water in the system. Subsequently, the temperature was raised to 160°C for polycondensation and kept for 2 hours;

[0036] Step 2: After the polycondensation reaction in step 1 is completed, add 0.2 g of acetic acid and maleic anhydride and grind it into powder before adding, add 3.0 g to carry out the modification reaction, and continue the reaction for 1.0 hour.

[0037] Step 3: After the reaction, a...

Embodiment 2

[0040] A kind of synthetic method of maleic anhydride modified p-tert-butylphenol formaldehyde resin, comprises the following steps:

[0041] Step 1: Weigh 100g (0.67mol) of p-tert-butylphenol and 0.17g of oxalic acid, add them to a 250ml four-necked round-bottom reaction flask equipped with a mechanical stirrer, a thermometer, a reflux condenser and a dropping funnel, and heat up to 80°C , Add dropwise 38.1g aqueous formaldehyde solution, continue to react for 2 hours. After the reaction, the temperature was raised to 100° C. to distill the water in the system. Subsequently, the temperature was raised to 165°C for polycondensation and kept for 1h;

[0042] Step 2: After the polycondensation reaction in step 1 is completed, 0.2 g of acetic acid and 6.0 g of maleic anhydride powder are added to carry out the modification reaction, and the reaction is continued for 0.5 hours.

[0043] Step 3: After the reaction is finished, add 2.0 g of sodium hydroxide lye (5%) to adjust the ...

Embodiment 3

[0046] A kind of synthetic method of maleic anhydride modified p-tert-butylphenol formaldehyde resin, comprises the following steps:

[0047] Step 1: Take by weighing p-tert-butylphenol 100g (0.67mol), p-toluenesulfonic acid 0.17g, add in the 250ml four-neck round bottom reaction flask that mechanical stirrer, thermometer, reflux condenser and dropping funnel are housed, heat up To 90°C, 48.9g of formaldehyde aqueous solution (phenol-formaldehyde ratio 1:0.9) was added dropwise, and the reaction continued for 3 hours. After the reaction, the temperature was raised to 100° C. to distill the water in the system. Subsequently, the temperature was raised to 170°C for polycondensation and kept for 1.5h;

[0048] Step 2: After the polycondensation reaction in step 1 is completed, add 0.2 g of acetic acid and 4.0 g of maleic anhydride powder to carry out the modification reaction, and continue the reaction for 0.5 hours;

[0049] Step 3: After the reaction is finished, add 2.0 g of...

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Abstract

The invention provides a maleic anhydride p-tert-butylphenol formaldehyde resin and a synthesis method thereof. The synthesis method comprises the following steps: 1, putting p-tert-butylphenol and formaldehyde into a reaction container provided with a stirrer, carrying out a condensation reaction under the action of a catalyst I, evaporating the water in the system at a temperature of 100 DEG C after the reaction is finished, heating, and carrying out a condensation polymerization reaction; 2, adding a catalyst II and maleic anhydride into the reaction container, and continuously carrying outa modification reaction under the action of the catalyst II; and 3, adding an alkali liquor into the reaction container, heating, and distilling off water and unreacted monomers to obtain the maleicanhydride modified p-tert-butylphenol formaldehyde resin. According to the invention, the double bonds contained in the obtained resin can react with double bonds in a rubber, so that migration of theresin in the rubber is reduced, heat generation is reduced, and the ageing resistance of the rubber is improved; and carboxyl and hydrogen bond interaction of modified group end points is strong, sothat the interaction force between molecules can be effectively improved, and the lasting viscosity is improved.

Description

technical field [0001] The invention belongs to the technical field of tackifying resins, in particular to a maleic anhydride-modified p-tert-butylphenol formaldehyde resin and a synthesis method thereof. Background technique [0002] In the tire production process, the lamination molding method is usually adopted, that is, the films of each part are made into unvulcanized rubber according to different performance requirements, and then laminating and molding; this process requires the unvulcanized rubber material to have a high molding viscosity. In order to improve the lack of adhesion between the various parts of the film, it is usually necessary to add a tackifier when mixing the rubber. [0003] At present, the widely used tackifying agent is common tackifying resin, that is, alkylphenol-formaldehyde resin. This type of resin has the advantages of simple process and low price, but after the tackifying resin is added to the rubber compound, the It is in a free state an...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C08G8/28C08L23/28C08L7/00C08L61/14C08K13/02C08K3/04C08K3/22C08K5/09C08K3/06
CPCC08G8/28C08L23/283C08L2205/035C08K2003/2296C08L7/00C08L61/14C08K13/02C08K3/04C08K3/22C08K5/09C08K3/06
Inventor马德龙李庆朝董瑞国李剑波黄存影
OwnerSHANDONG YANGGU HUATAI CHEM