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Acrylic acid liquid crystal photosensitive resin and preparation method thereof

A technology of photosensitive resin and acrylic acid, which is applied in the direction of liquid crystal materials, chemical instruments and methods, etc., can solve the problems of not being suitable for parts with large thickness, and achieve the effects of poor heat resistance, high modulus, and low dimensional shrinkage

Pending Publication Date: 2021-12-14
QUANZHOU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is more suitable for preparing thin films, not for thicker parts.

Method used

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  • Acrylic acid liquid crystal photosensitive resin and preparation method thereof
  • Acrylic acid liquid crystal photosensitive resin and preparation method thereof
  • Acrylic acid liquid crystal photosensitive resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Mix with 23.0g4-hydroxyphenyl 4-hydroxybenzoic acid ester, 230ml part epichlorohydrin (EHC) and 0.5g Tetramethylammonium chloride, pass into N 2 protection, and then reacted at 60°C for 12 hours to obtain solution A;

[0027] (2) then slowly drip NaOH solution (0.25mol, concentration 45%) in the solution A, the water generated by the reaction is removed under reduced pressure by a vacuum pump, and the product is poured into the separatory funnel after continuing the reaction for 0.5 hours, and the NaCl is removed by filtration, Gained filtrate utilizes rotary evaporator to remove redundant EHC, obtains solution B;

[0028] (3) Mix solution B with methanol / acetone solution (ratio 1.0:1.0), put it in the refrigerator to cool down and crystallize, the obtained crystals are washed with methanol and filtered with suction, and the product is dried in an oven at 60°C to obtain a milky white solid that is liquid crystal Epoxy resin C;

[0029] (4) Take 19.3g (0.05mol) of ...

Embodiment 2

[0036] (1) Mix 0.1mol 4,4'-diphenol, 360ml parts epichlorohydrin (EHC) and 0.003mol tetrabutylammonium bromide as raw materials, feed N 2 protection, and then reacted at 50°C for 18 hours to obtain solution A;

[0037] (2) then slowly drip NaOH solution (0.30mol, concentration 40%) in the solution A, the water generated by the reaction is removed under reduced pressure by a vacuum pump; after continuing to react for 2.5 hours, the product is poured into the separatory funnel, and the NaCl is removed by filtration. Gained filtrate utilizes rotary evaporator to remove redundant EHC, obtains solution B;

[0038] (3) Mix solution B with methanol / acetone solution (ratio 1.0:3.0), put it in the refrigerator to cool down and crystallize, the obtained crystals are washed with methanol and filtered with suction, and the product is dried in an oven at 80°C to obtain a milky white solid that is liquid crystal Epoxy resin C;

[0039] (4) Take 14.9g (0.05mol) of liquid crystal epoxy resi...

Embodiment 3

[0042] (1) Mix 0.1mol 3,3',5,5'-tetramethylbiphenol, 120ml of epichlorohydrin (EHC) and 0.006mol of tetrabutylammonium chloride as raw materials, pass into N 2 protection, and then reacted at 80°C for 6 hours to obtain solution A;

[0043] (2) then slowly drip NaOH solution (0.20mol, concentration 60%) in the solution A, the water generated by the reaction is removed under reduced pressure by a vacuum pump, after continuing to react for 4.0 hours, the product is poured into the separatory funnel, and NaCl is removed by filtration, Gained filtrate utilizes rotary evaporator to remove redundant EHC, obtains solution B;

[0044] (3) Mix solution B with methanol / acetone solution (ratio 1.0:0.5), put it in the refrigerator to cool down and crystallize, the obtained crystals are washed with methanol and filtered with suction, and the product is dried in an oven at 100°C to obtain a milky white solid that is liquid crystal Epoxy resin C;

[0045] (4) Take 17.5g (0.05mol) liquid cr...

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Abstract

The invention discloses acrylic liquid crystal photosensitive resin and a preparation method thereof. The method comprises the following steps: mixing a compound which contains mesogenic elements and has -OH at an end part, EHC and a catalyst 1, and conducting reacting to obtain a solution A; dropwise adding NaOH into the solution A, removing water generated by the reaction, continuing the reaction, filtering a product to remove NaCl, and removing redundant EHC from an obtained filtrate to obtain a solution B; mixing the solution B with a methanol / acetone solution, carrying out cooling and crystallizing, washing an obtained crystal substance with methanol, and carrying out suction filtration and drying to obtain liquid crystal epoxy resin C; and subjecting the liquid crystal epoxy resin C with a polymerization inhibitor to mixing and a reaction, dropwise adding acrylic acid and a catalyst 2 after the epoxy resin C is completely melted, and conducting reacting to obtain the acrylic liquid crystal photosensitive resin. The acrylic liquid crystal photosensitive resin has the advantages of ordered liquid crystals and network crosslinking, is excellent in mechanical property, heat resistance, size stability and forming manufacturability, is cured through ultraviolet irradiation, and has the advantages of high curing speed, small pollution, energy conservation and the like.

Description

technical field [0001] The invention relates to the technical field of ultraviolet curing materials, in particular to an acrylic liquid crystal photosensitive resin and a preparation method thereof. Background technique [0002] Compared with other molding technologies, light-curing molding technology has the advantages of fast speed, short curing molding time, energy saving, and basically no pollution. The hardness, chemical resistance, and wear resistance of molding materials are all excellent. . The development of any molding technology must have materials with excellent performance as the basis. Therefore, the development of new photosensitive resin materials has gradually become the key to the innovation and breakthrough of photochemical polymerization technology, and it is also the only way to expand the application field of photochemical polymerization technology. [0003] Thermosetting liquid crystal resin is an extremely important branch of liquid crystal polymers...

Claims

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Application Information

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IPC IPC(8): C08G59/17
CPCC08G59/1466C08G59/063C08G59/022C09K19/3852
Inventor 陈少云卓东贤华文强陈明雪孙晓露瞿波王睿郑燕玉刘小英李文杰
Owner QUANZHOU NORMAL UNIV
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