Light-colored terpene phenol resin with high softening point as well as preparation method and application of light-colored terpene phenol resin

A point terpene phenol resin, light color technology, applied in the field of light color high softening point terpene phenol resin and its preparation, can solve the problems of limiting the scope of use and value, speeding up the transfer of polymer chains, affecting catalyst treatment, etc. Excellent viscosity-increasing effect, high softening point and compatibility, and the effect of improving dynamic storage modulus

Active Publication Date: 2019-07-12
江西金安林产实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on this, my country began to study it in the middle and late 20th century, but little progress was made. At present, it is mainly obtained by cationic polymerization of terpenes and phenols under the action of catalysts such as Lewis acids. It is unstable in medium and prone to termination reaction, which leads to low polymerization efficiency. In order to improve polymerization efficiency, the amount of catalyst is generally increased, which will not only lead to waste of catalyst, affect the later catalyst treatment, pollute the environment, but also cause the color of the resin to deepen. In order to reduce the resin The color does not affect the yield. Generally, low temperature is used for polymerization. However, because phenolic substances and α-pinene need to overcome high energy during polymerization, they are difficult to activate and effectively polymerize at lower temperatures, resulting in resin production. The rate is low, so the terpene phenol reaction process generally requires a higher temperature to increase the polymerization efficiency, but under high temperature conditions, the color of the resin will deepen and the transfer of the polymer chain will be accelerated, resulting in a decrease in the degree of polymerization and a smaller molecular weight. Eventually lead to a low softening point of the resin
Because of these problems, the color of the terpene phenolic resins currently researched is generally greater than the No. 6 color, and the softening point is less than 140°C, which limits its scope of use and value.

Method used

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  • Light-colored terpene phenol resin with high softening point as well as preparation method and application of light-colored terpene phenol resin
  • Light-colored terpene phenol resin with high softening point as well as preparation method and application of light-colored terpene phenol resin
  • Light-colored terpene phenol resin with high softening point as well as preparation method and application of light-colored terpene phenol resin

Examples

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Effect test

Embodiment 1

[0047] A kind of embodiment of the preparation method of light color high softening point terpene phenol resin of the present invention, comprises the following steps:

[0048] (1) Add 1.50g of BF 3 , 45g phenol, 300mL dry toluene and 0.80g phosphorus-containing inorganic acid light color agent, inject 0.05g ethyl benzoate with a micro syringe at the same time, place it in a low-temperature circulation pump, and pass N 2 Exhaust the air, start stirring, and slowly add 255g of refined masson turpentine into the flask through the constant pressure dropping funnel, and control the reaction temperature at 30°C. After 1 / 3 of the refined masson turpentine is added dropwise, add 1.50g of BF 3 and 0.05g ethyl benzoate, add 1.50g BF after adding 2 / 3 of the refined masson turpentine 3 and 0.05g ethyl benzoate, continue to drop the remaining refined masson turpentine, after the dropwise addition, continue the insulation reaction for 3h;

[0049] (2) After the reaction is completed, rem...

Embodiment 2

[0051] A kind of embodiment of the preparation method of light color high softening point terpene phenol resin of the present invention, comprises the following steps:

[0052] (1) Add 2.50g of BF 3 , 150g phenol, 300mL dry toluene and 0.60g phosphorus-containing inorganic acid light color agent, inject 0.10g ethyl benzoate with a micro syringe at the same time, place it in a low-temperature circulation pump, and pass N 2 Exhaust the air, start stirring, slowly add 150g of refined masson turpentine into the flask through the constant pressure dropping funnel, control the reaction temperature at 40°C, add 2.50g of BF after adding 1 / 3 of the refined masson turpentine into the flask 3 and 0.10g ethyl benzoate, add 2.50g BF after adding 2 / 3 of the refined masson turpentine 3 and 0.10g ethyl benzoate, continue to drop the remaining refined masson turpentine, after the dropwise addition, continue the insulation reaction for 3.5h;

[0053] (2) After the reaction is completed, remov...

Embodiment 3

[0055] A kind of embodiment of the preparation method of light color high softening point terpene phenol resin of the present invention, comprises the following steps:

[0056] (1) In a 1000mL dry four-necked flask equipped with a stirrer, thermometer, calcium chloride drying tube and constant pressure dropping funnel, add 3.50g BF 3 , 135g phenol, 300mL dry toluene and 0.40g phosphorus-containing inorganic acid light color agent, inject 0.14g ethyl benzoate with a micro syringe at the same time, place it in a low-temperature circulation pump, and pass N 2 Exhaust the air, start stirring, slowly add 165g of refined masson turpentine into the flask through the constant pressure dropping funnel, control the reaction temperature at 40°C, add 3.50g of BF after adding 1 / 3 of the refined masson turpentine into the flask 3 and 0.14g of ethyl benzoate, add 3.50g of BF after adding 2 / 3 of the refined masson turpentine 3 and 0.14g ethyl benzoate, continue to drop the remaining refined ...

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Abstract

The invention discloses light-colored terpene phenol resin with a high softening point. The structural formula of resin is shown in formula (I). The raw material terpene of the light-colored terpene phenol resin with the high softening point is a natural renewable resource, is abundantly sourced, cheap, environmentally friendly and clean; the light-colored terpene phenol resin with the high softening point can improved adhesiveness and strength of an adhesive, can be widely applied to rubber products such as styrene butadiene rubber, natural rubber and neoprene, and can play an excellent tackifying effect. The invention also discloses a preparation method of the light-colored terpene phenol resin with the high softening point. The preparation method is simple, and preparation can be achieved by polymerization-washing-distillation; a small quantity of catalyst is used and dissolved in a solvent, and thus, post-treatment is simple, and basically no corrosion or environmental pollution occurs; the problems of dark color and relatively low softening point of resin in the synthesis process of terpene phenol can be solved. The invention also discloses an application of the light-coloredterpene phenol resin with the high softening point as a rubber tackifier or a tire additive.

Description

technical field [0001] The invention relates to a terpene phenol resin and its preparation method and application, in particular to a light-colored high softening point terpene phenol resin and its preparation method and application. Background technique [0002] The annual output of turpentine in my country ranks first in the world. Using turpentine as raw material to produce high value-added fine chemical products is in line with the strategy of sustainable development and has important economic value and research significance. Among them, the terpene phenolic resin prepared by co-condensation of turpentine or pinene and phenolic substances is a typical representative thereof. This type of resin has good light resistance and heat resistance, and contains phenolic structural units, making its intramolecular interactions more complex than ordinary polyterpene resins, resulting in different properties and applications from the latter. Terpene phenol resin has good compatibil...

Claims

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Application Information

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IPC IPC(8): C08G61/02C08L65/00
CPCC08G61/02C08G2261/124C08G2261/1422C08G2261/312C08G2261/3323C08L65/00
Inventor 翁亮徐社阳林莉
Owner 江西金安林产实业有限公司
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