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Bio-based epoxy resin containing silicon phenylene structure, composition and preparation method thereof

A technology based on epoxy resin and biotechnology, applied in the direction of silicon organic compounds, compounds of group 4/14 elements of the periodic table, chemical instruments and methods, etc., can solve the problem of low yield of closed-loop products and difficult to meet high-quality application requirements , High content of hydrolyzable chlorine, etc., to achieve excellent intrinsic flame retardant properties, excellent catalytic performance, and high heat resistance

Active Publication Date: 2021-02-26
AVIC BEIJING AERONAUTICAL MFG TECH RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this reaction requires repeated extraction and washing, resulting in a large amount of waste liquid, and the yield of the closed-loop product is low, about 70%, and the content of hydrolyzable chlorine in the product is high, which is difficult to meet the needs of high-quality applications.

Method used

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  • Bio-based epoxy resin containing silicon phenylene structure, composition and preparation method thereof
  • Bio-based epoxy resin containing silicon phenylene structure, composition and preparation method thereof
  • Bio-based epoxy resin containing silicon phenylene structure, composition and preparation method thereof

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preparation example Construction

[0048] figure 1 It is a schematic flow diagram of a preparation method of a bio-based epoxy resin containing a silicon phenylene structure provided by the embodiment of the present invention, as figure 1 As shown, according to the first aspect of the embodiments of the present invention, the preparation method of the bio-based epoxy resin containing silicon phenylene structure, the preparation method comprises the following steps:

[0049] S1. Mix eugenol, epichlorohydrin, solid base and the first catalyst under normal pressure, stir at -20-0°C for 1-2 hours, then raise the temperature to 60-100°C for 1-10 hours, Filtration and rotary evaporation to remove impurities to obtain epoxidized eugenol; wherein, the first catalyst is a mesoporous molecular sieve solidly loaded with a mixture of tetramethylammonium bromide and benzyltriethylammonium chloride.

[0050] In this step, the content of tetramethylammonium bromide and benzyltriethylammonium chloride in the first catalyst is...

Embodiment approach

[0076] As a preferred embodiment, the preparation method includes the following steps:

[0077] In step (1), the molar ratio of eugenol, epichlorohydrin and solid base is 1: (5-10): (1-5), preferably, 1: (5-8): (2-5 ).

[0078] The content of tetramethylammonium chloride and tetramethylethylenediamine in the first catalyst is 1%-10% of the total mass of eugenol, epichlorohydrin and solid base, preferably 1%-9%.

[0079] figure 2 It is a schematic diagram of the hydrogen nuclear magnetic resonance spectrum of a bio-based epoxy resin with a silicon-phenylene structure having a structural formula I-1 provided by the embodiment of the present invention, such as figure 2 As shown, according to the second aspect of the embodiments of the present invention, there is provided a bio-based epoxy resin containing silicon phenylene structure prepared according to the above process, and the structural formula is as shown in (I-1):

[0080]

[0081] The above-mentioned bio-based epo...

Embodiment 1

[0092] (1) Add 2g of SBA-15 mesoporous molecular sieve and 2g of (N-(β-aminoethyl))-γ-aminopropyltrimethoxysilane into 150ml of absolute ethanol. Use a high-speed disperser to process the mixed suspension at a speed of 5000r / min for 0.5 hour; then use an ultrasonic oscillator to continue processing the suspension with an oscillation power of 600W, an oscillation frequency of 22kHz, and an oscillation time of 1 hour. The uniformly mixed suspension is evaporated in a water bath under electromagnetic stirring, and when the solvent is evaporated to dryness, the vacuum-dried particles are ground with a mortar to obtain a modified mesoporous molecular sieve.

[0093] (2) Mix tetramethylammonium bromide and benzyltriethylammonium chloride aqueous solution (concentration is 10g / L, 100ml) with the treated SBA-15 mesoporous molecular sieve (2g), and remove the water by evaporation , the remaining material was placed in an ultrasonic oscillator, and treated at 100° C. for 0.3 hours to ob...

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Abstract

The invention relates to bio-based epoxy resin containing a silicon phenylene structure, a composition and a preparation method thereof. The method comprises the steps of mixing eugenol, epichlorohydrin, solid alkali and a first catalyst at normal pressure, stirring for 1-2 hours at the low temperature of -20-0 DEG C, heating to 60-100 DEG C and reacting for 1-10 hours, filtering and rotary evaporation to remove impurities, acquiring epoxidized eugenol, mixing epoxidized eugenol, 1, 4-di(dimethylsilyl) benzene and a second catalyst, and carrying out a reaction to prepare bio-based epoxy resincontaining a silicon phenylene structure. The first catalyst is a mesoporous molecular sieve immobilized with a mixture of tetramethyl ammonium bromide and benzyltriethylammonium chloride. The bio-based epoxy resin containing the silicon phenylene structure and the preparation method thereof aim at solving the problem of how to prepare epoxy resin with high heat resistance.

Description

technical field [0001] The invention relates to the technical field of epoxy resins, in particular to a bio-based epoxy resin containing a silicon phenylene structure, a composition and a preparation method thereof. Background technique [0002] Due to its excellent chemical, electrical, heat resistance, adhesive and mechanical properties, epoxy resin is widely used in coatings, adhesives, auto parts and other fields, and is one of the three thermosetting polymer materials. At present, almost all commercial epoxy resins are derived from petroleum bases, and bisphenol A epoxy resins account for about 90% of the output. Bisphenol A is one of the most widely used industrial compounds in the world, but in recent years, with the in-depth understanding of the biological toxicity of bisphenol A, many countries have banned the use of bisphenol A in food plastic packaging and containers. Therefore, the preparation of epoxy resins from bio-based raw materials has gradually become a r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08B01J31/02B01J29/04B01J37/34B01J37/03C08G59/30C08L63/00
CPCC07F7/081C07F7/0829B01J31/0274B01J31/0275B01J31/0239B01J31/0254B01J29/041B01J37/343B01J37/033C08G59/306C08L63/00C08L2201/02C08L2201/08B01J2231/323B01J35/23
Inventor 李言张博窦鹏
Owner AVIC BEIJING AERONAUTICAL MFG TECH RES INST
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