US-12624155-B2 - Preparation method of low-chlorine epoxy resin and use thereof

Abstract

The present disclosure relates to the technical field of the epoxy resin, specifically, relates to a preparation method a low-chlorine epoxy resin and use thereof, which can solve the problem of a high total chlorine content in the epoxy resin to a certain extent. The preparation method of a low-chloride epoxy resin comprises: loading a metal oxide as a stationary phase on a grid inside a reaction kettle; the reaction kettle being externally connected to an alternating-current power supply, and under a first pre-set condition, diluted epoxy resin containing a chlorine impurity, as a mobile phase, flowing through the grid loaded with the metal oxide; the epoxy resin containing a chlorine impurity contacting and reacting with the metal oxide to obtain a purified epoxy resin.

Inventors

• Biao Du

Assignees

• ZILLION NEW MATERIAL TECHNOLOGY (XI'AN) CO., LTD.

Dates

Publication Date

20260512

Application Date

20230222

Priority Date

20220720

Claims (7)

1. 1 . A preparation method of a low-chlorine epoxy resin, comprising: loading a metal oxide on a grid inside a reaction kettle, the metal oxide representing a stationary phase; supplying power to the reaction kettle from an externally connected alternating-current power supply, providing an epoxy resin that has been diluted with a solvent, the epoxy resin containing a chlorine impurity, and flowing the diluted epoxy resin, as a mobile phase, through the stationary phase under a first pre-set condition; wherein the epoxy resin containing a chlorine impurity contacts and reacts with the metal oxide to provide a purified epoxy resin.
2. 2 . The preparation method of a low-chlorine epoxy resin according to claim 1 , wherein the metal oxide is CaO, FeO, MgO, or CuO.
3. 3 . The preparation method of a low-chlorine epoxy resin according to claim 2 , wherein a molar ratio of the metal oxide to the epoxy resin containing a chlorine impurity is (0.5˜1.5): 1.
4. 4 . The preparation method of a low-chlorine epoxy resin according to claim 1 , wherein the solvent is xylene, acetone, methyl ethyl ketone, cyclohexanone, benzene, n-butanol or styrene.
5. 5 . The preparation method of a low-chlorine epoxy resin according to claim 1 , wherein the alternating-current power source has a frequency of 45 Hz˜75 Hz and a voltage of 220 V˜380 V.
6. 6 . The preparation method of a low-chlorine epoxy resin according to claim 5 , wherein the first pre-set condition comprises: a reaction time of 3 h˜5 h for reacting the epoxy resin containing a chlorine impurity with the metal oxide, and a reaction temperature of 50° C.˜90° C. in the reaction kettle during the reaction.
7. 7 . The preparation method of a low-chlorine epoxy resin according to claim 1 , wherein a reaction principle of the reaction is: wherein MO is the metal oxide.

Description

CROSS-REFERENCE TO RELATED APPLICATION This application claims priority to Chinese Application No. 202210859348.0, filed Jul. 20, 2022 with the China National Intellectual Property Administration, the entirety of which is incorporated herein by reference. FIELD OF THE PRESENT DISCLOSURE The present disclosure relates to the technical field of epoxy resins, and in particular to a preparation method of a low-chlorine epoxy resin and use thereof. BACKGROUND OF THE PRESENT DISCLOSURE Epoxy resin has good mechanical properties, high temperature resistance, good insulation performance, and is widely used in coatings, adhesives, flooring adhesives, electronic products and other fields. However, chlorine residue in epoxy resin has a lot of adverse effects on the application performance of products, which limits the application of epoxy resin in the fields of photoresists, electronic packaging, chip adhesive and other electronic products. In the field of epoxy resin applications of photoresists, the total chlorine content in the epoxy resin is required to be less than 800 ppm. At present, the most common method for removing chlorine in epoxy resin in industry is molecular distillation method, but it requires huge energy consumption and high production cost by this method for achieving the total chlorine content below 800 ppm, which is not advantageous for industrial production. SUMMARY OF THE PRESENT DISCLOSURE In order to solve the problem of high total chlorine content in the epoxy resin, the present disclosure provides a preparation method of a low-chlorine epoxy resin and the use thereof. The embodiments of the present disclosure are carried out as follows. Embodiments of the present disclosure provide a preparation method of a low-chlorine epoxy resin, comprising: loading a metal oxide as a stationary phase on a grid inside a reaction kettle;the reaction kettle being externally connected to an alternating-current power supply, and under a first pre-set condition, a diluted epoxy resin containing a chlorine impurity, as a mobile phase, flowing through the grid loaded with the metal oxide; andthe epoxy resin containing a chlorine impurity contacting and reacting with the metal oxide to form a purified epoxy resin. In some embodiments, the metal oxide is CaO, FeO, MgO, or CuO. In some embodiments, a molar ratio of the metal oxide to the epoxy resin containing a chlorine impurity is (0.5˜1.5): 1. In some embodiments, the epoxy resin is diluted with xylene, acetone, methyl ethyl ketone, cyclohexanone, benzene, n-butanol or styrene as a solvent to obtain the diluted epoxy resin containing a chlorine impurity. In some embodiments, the alternating-current power source has a frequency of 45 Hz˜75 Hz and a voltage of 220 V˜380 V. In some embodiments, the first pre-set condition comprises: a reaction time of being 3 h˜5 h for reacting the epoxy resin containing a chlorine impurity with the metal oxide, and during the reaction, the reaction temperature of 50° C.˜90° C. in the reaction kettle. In some embodiments, a reaction principle of reacting the epoxy resin containing a chlorine impurity with the metal oxide to form a purified epoxy resin is: wherein MO is the metal oxide. Yet another embodiment of the present disclosure provides use of a low-chlorine epoxy resin, comprising applying a purified epoxy resin prepared with the preparation method of a low-chlorine epoxy resin described above to a photoresist. Advantageous effects of the present disclosure: the epoxy resin containing a chlorine impurity, which is diluted by a solvent, flows through the metal oxide as a mobile phase; due to an external alternating electric field of the reaction device, the chlorine impurities and the metal oxide in the epoxy resin are easily polarized under the action of the alternating electric field, so that the chlorine impurities and the metal oxide in the epoxy resin have a high reaction activity, and then the epoxy resin containing a chlorine impurity and the metal oxide are reacted to obtain a purified epoxy resin and a by-product of metal chloride; the by-product of metal chloride produced thereby has the property of being insoluble in the organic solvent, and thus the purified epoxy resin also does not contain the metal chloride. In the present disclosure, the removal mechanism of the chlorine impurities in the epoxy resin is clear, the total chlorine content of the product is controllable, the reaction conditions are easy to control, and the reaction process is simple. BRIEF DESCRIPTION OF THE DRAWINGS In order to explain the technical solutions in the embodiments of the present disclosure or the prior art more clearly, the following briefly illustrates the embodiments or the drawings required to be used in the description of the prior art. Obviously, the drawings in the description below are some embodiments of the present disclosure, and it would have been obvious for a person of ordinary skill in the art to obtain other drawings