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A kind of light color high softening point terpene phenol resin and its preparation method and application

A kind of terpene phenol resin and light-colored technology, which is applied in the field of light-colored high-softening point terpene phenol resin and its preparation, can solve the problems of accelerating polymer chain transfer, reducing the degree of polymerization, and low polymerization efficiency, and achieves the solution of resin Deep color and low softening point, improved adhesion and strength, simple preparation method

Active Publication Date: 2021-10-29
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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  • A kind of light color high softening point terpene phenol resin and its preparation method and application
  • A kind of light color high softening point terpene phenol resin and its preparation method and application
  • A kind of light color high softening point terpene phenol resin and its preparation method and application

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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 a terpene phenol resin with light color and high softening point, the structural formula of which is shown in formula (I). The light-colored high softening point terpene phenolic resin of the present invention is a natural renewable resource of terpene, which is rich in sources, low in price, environmentally friendly and clean; it can improve the adhesiveness and strength of the adhesive, and can be widely used in styrene-butadiene rubber, In rubber products such as natural rubber and neoprene, it can have an excellent viscosity-increasing effect. The invention also discloses a preparation method of the light-colored high-softening point terpene phenol resin. The preparation method is simple and can be prepared through polymerization-water-washing-distillation; the amount of catalyst is small, and it is dissolved in a solvent, so the post-treatment is simple , basically no corrosion and environmental pollution; it can solve the problems of dark resin color and low softening point in the synthesis process of terpene phenols. The invention also discloses the use of the light-colored high-softening-point terpene phenol resin as a rubber tackifier or 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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Patent Type & Authority Patents(China)
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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