Method for preparing polyol ester resin of terpene and rosin diene addition product based on rosin

A technology of rosin diene and polyol ester, which is applied in the field of polyol ester resin for preparing terpene and rosin diene adducts from rosin, can solve the problems such as no research report on polyol ester resin, and achieve the preparation method Energy saving, easy production operation, and simple process flow

Active Publication Date: 2015-06-17
广东省邦得利新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, people have done a lot of work on the research and application of pine resin and rosin, but there is no research report on the preparation of polyol ester resins of terpene and rosin diene adducts with rosin

Method used

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  • Method for preparing polyol ester resin of terpene and rosin diene addition product based on rosin
  • Method for preparing polyol ester resin of terpene and rosin diene addition product based on rosin

Examples

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Embodiment 1

[0040]In a 500ml four-necked flask with stirring, reflux, and distillation device functions, take 100 parts of net rosin liquid with a mass ratio of turpentine and rosin of 2:8, 60 parts of turpentine, and prepare a weight ratio of turpentine and rosin of 50 parts. : The reaction raw material A of 50. Add 55 parts of maleic anhydride and 1.6 parts of phosphoric acid, stir and heat to reflux reaction, control the reaction temperature, and gradually increase the temperature from 120°C to 190°C. When reflux occurs in the reaction, time the reaction for 2 hours, then steam the unreacted turpentine under normal pressure, then increase the reaction temperature to 210°C and continue the reaction for 1 hour, add 0.032 parts of zinc oxide, drop 50 parts of glycerin, and increase the reaction temperature to 220°C. -230°C, and control the reaction at 245-250°C for 3 hours, take a sample to measure the acid value, after passing the test (acid value is less than 40mgKOH / g), vacuum (20mmHg)...

Embodiment 2

[0042] In a 500ml four-neck flask with stirring, reflux, and distillation device functions, 120 parts of net turpentine liquid and 40 parts of turpentine were weighed, and the weight ratio of turpentine and rosin was prepared as reaction raw material A of 64:96. Add 60 parts of maleic acid and 1.2 parts of phosphoric acid, stir and heat to reflux reaction, control the reaction temperature, and gradually increase the temperature from 120°C to 200°C. When reflux occurs, time the reaction for 2 hours, then steam the unreacted turpentine under normal pressure, then increase the reaction temperature to 210°C and continue the reaction for 1 hour, add 0.04 parts of zinc oxide, drop 50 parts of glycerin, and increase the reaction temperature to 220- 230°C, and control the reaction at 250-260°C for 4 hours, take a sample to measure the acid value, after passing the test (acid value is less than 40mgKOH / g), vacuum (20mmHg) decompression, the temperature of the reaction bottle is controll...

Embodiment 3

[0044] In a 500ml four-necked flask with stirring, reflux, and distillation device functions, 150 parts of net turpentine liquid and 10 parts of turpentine were weighed, and the weight ratio of turpentine and rosin was prepared as reaction raw material A of 40:120. Add 40 parts of maleic anhydride and 0.8 parts of phosphoric acid, stir and heat to reflux reaction, control the reaction temperature, and gradually increase the temperature from 120°C to 210°C. When reflux occurs, the reaction time is 2 hours, and then the unreacted turpentine is steamed out under normal pressure, and then the reaction is continued at 210°C for 1 hour, 0.048 parts of zinc oxide is added, 60 parts of glycerin is added dropwise, and the reaction temperature is increased to 220-230°C. And control the reaction at 245-250°C for 3 hours, take a sample to measure the acid value, after passing the test (acid value is less than 40mgKOH / g), vacuum (20mmHg) depressurization, control the temperature of the reac...

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Abstract

The invention discloses a method for preparing the polyol ester resin of terpene and rosin diene addition product based on rosin. The method disclosed by the invention comprises the following preparation steps of: (1) mixing turpentine with rosin, removing impurities by means of heating and stirring to dissolve, filtering, washing and the like, clarifying to separate water, then performing atmospheric distillation, distilling out water and a part of turpentine left in rosin by virtue of an oil-water azeotropic principle, so as to obtain a pure rosin liquid, analysing the contents of turpentine and rosin in the rosin liquid, and preparing to achieve a certain ratio; (2) metering the pure rosin liquid, preparing the pure rosin liquid with turpentine to obtain a reaction raw material A, and reacting the reaction raw material A with a dienophile addition agent under the action of catalysis, so as to generate a turpentine-rosin diene addition product; (3) performing esterification on polyols and the turpentine-rosin diene addition product; (4) performing vacuum reduced pressure distillation to remove water generated during the esterification, unreacted alcohols, and the low-molecular substances generated by side reactions, so as to obtain the polyol ester resin of terpene-rosin diene addition product. The method disclosed by the invention is simple in process flow and achieves energy-saving and environment-friendly effects.

Description

technical field [0001] The invention relates to a deep processing method of rosin, rosin and turpentine, in particular to a method for preparing polyol ester resin of terpene and rosin diene adducts from rosin. Background technique [0002] Pine resin is a natural resin that is harvested from pinus pine trees. The main pine species harvested in my country are Masson pine, Slash pine, Simao pine and so on. Pine resin is a renewable resource. Our country's annual output is nearly 1 million tons, accounting for more than 70% of the world's average annual output of rosin. Rosin processed products are widely used in adhesives, synthetic rubber, paper, ink, electronics, food and many other industries. [0003] The main components in turpentine are rosin and turpentine. Rosin is a solid diterpene resin acid, and its molecule contains a tricyclic phenanthrene skeleton structure, a carboxyl group, and a conjugated double bond. Carboxyl groups and double bonds in rosin can be used...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09F1/04
Inventor 许卫平王振洪陈竟旭
Owner 广东省邦得利新材料技术有限公司
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