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A kind of non-volatile solubilizing diluent and its preparation method and application

A diluent and non-volatile technology, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve safety issues, personal health, environmental issues, etc., and achieve improved compatibility, high boiling point, The effect of reducing the viscosity of the system

Active Publication Date: 2020-11-10
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the continuous increase in the use of epoxy resin, it brings serious environmental problems, safety problems and personal health problems

Method used

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  • A kind of non-volatile solubilizing diluent and its preparation method and application
  • A kind of non-volatile solubilizing diluent and its preparation method and application
  • A kind of non-volatile solubilizing diluent and its preparation method and application

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Experimental program
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preparation example Construction

[0029] The preparation process of this solubilizing diluent comprises the following steps:

[0030] Dry the three-neck flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator before installing them. Get 0.2mol phthalic anhydride and add in a three-necked flask, add 0.2-0.3mol fatty alcohol with more than four carbons; the fatty alcohol with more than four carbons is any one of n-butanol, n-octanol or lauryl alcohol, Heating to 110-140°C, stirring while heating until completely dissolved to form mixture A. Cool mixture A to room temperature, add 100-300mL toluene, measure the acid value and record; then add 0.3-0.5mol of dihydric alcohol and 1.5-3g of p-toluenesulfonic acid to prepare mixture B; dibasic alcohol includes ethylene glycol, Diethylene glycol, hexanediol and propylene glycol, measure the initial acid value of mixture B and record it. Put the mixture B in the water separator, heat up to 110°C and reflux, use the wa...

Embodiment 1

[0033] Dry the three-necked flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator and install them; take 0.2mol of phthalic anhydride into the three-necked flask, add 0.22mol of n-butanol, heat to 140°C, and stir until completely dissolved. Cool to room temperature, add 100mL toluene, measure the acid value; then add 0.3mol diethylene glycol and 1.5g p-toluenesulfonic acid, measure the initial acid value; The water formed was separated off and the acid value was monitored during the reaction. Stop the reaction until the acid value is lower than 5; after the reaction, a yellow liquid is obtained, and the toluene is removed by rotary evaporation, then dissolved in dichloromethane, washed with 5% sodium bicarbonate until neutral, washed twice with saturated saline and evaporated The solvent was removed to obtain a pale yellow solubilizing diluent.

[0034] Utilize the solubilizing diluent prepared in this embodiment to prepar...

Embodiment 2

[0036] Dry the three-neck flask, condenser tube and other instruments at 120°C for 1.5h, take them out and cool them in a desiccator before installing them. Take 0.2mol of phthalic anhydride into a three-necked flask, add 0.22mol of n-octanol, heat to 110°C, and stir until completely dissolved. Cool to room temperature, add 200mL of toluene, measure the acid value; then add 0.3mol ethylene glycol and 1.5g p-toluenesulfonic acid, measure the initial acid value. Add a water separator, heat up to 110°C and reflux, use a water separator to continuously separate the generated water, monitor the acid value during the reaction, until the acid value is lower than 5, the reaction ends. A yellow liquid was obtained, and the toluene was distilled off under reduced pressure, then dissolved in dichloromethane, washed with 5% sodium bicarbonate until neutral, washed twice with saturated brine, and the solvent was distilled off to obtain a light yellow solubilizing diluent.

[0037] Utilize...

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Abstract

The invention discloses a non-volatile solubilizing diluent as well as a preparation method and an application thereof. The solubilizing diluent is prepared by an esterification reaction, contains a lipophilic ester group, can be soluble with epoxy resin, contains a hydrophilic hydroxyl group, is low in viscosity and high in boiling point, is less volatile, and can improve compatibility of the epoxy resin and a curing agent and reduce system viscosity; the solubilizing diluent is free of VOC (volatile organic compound) emission and pollution-free to the environment in a using process, the effect is obvious with addition of a small quantity of the solubilizing diluent, and the solubilizing diluent has quite low viscosity and also has functions of a diluent. When the diluent is applied to the epoxy resin, viscosity of the epoxy resin can be effectively reduced, and a traditional amine curing agent can be better compatible with bulk E type epoxy resin. Not only is consumption of a volatile solvent eliminated, but also the solubilizing diluent becomes a part of a resin system, so that cost of the resin is not increased, and impact resistance and low-temperature performance of the curedresin are greatly improved.

Description

【Technical field】 [0001] The invention belongs to the field of chemical and chemical synthesis, and in particular relates to a non-volatile solubilizing diluent and its preparation method and application. 【Background technique】 [0002] Epoxy resin is widely used in high-performance coatings, inks, adhesives and composite materials because of its advantages such as low shrinkage, good adhesion, high strength and good mechanical properties. These excellent properties can only be manifested when the epoxy resin undergoes a curing cross-linking reaction with the curing agent. Different curing agents have different properties of cured products. Commonly used room temperature curing agents are mainly amine curing agents. However, such curing agents such as 651, 650, T31, etc. have poor compatibility with commonly used E-type epoxy resins, cannot form a uniform system, and directly affect the performance after curing. The traditional method is to add a large amount of volatile ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C69/80C09D7/20
Inventor 曹瑞军王翠钰马莉娜
Owner XI AN JIAOTONG UNIV