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Fluorine-containing novolac resin and preparation method and application of fluorine-containing novolac resin

A technology of novolac resin and hexafluorobisphenol, which is applied in the field of low-molecular-weight fluorine-containing phenolic resin and its preparation, can solve the problems of low fluorine element content and insufficient improvement of comprehensive performance, and achieve comprehensive performance improvement, free The effect of low phenol residue and no three-hazard discharge

Inactive Publication Date: 2011-08-17
ETERNAL CHEM (CHINA) CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In these patents, the content of the fluorine element introduced is not high, which leads to the insufficient improvement of the comprehensive performance of the epoxy resin by the fluorine element

Method used

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  • Fluorine-containing novolac resin and preparation method and application of fluorine-containing novolac resin
  • Fluorine-containing novolac resin and preparation method and application of fluorine-containing novolac resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 350ml of n-butanol and 336g of hexafluorobisphenol A into a 500ml reaction kettle equipped with a thermometer, a stirrer and a reflux condenser, and stir at 60°C to fully dissolve the hexafluorobisphenol A. Then 5 g of oxalic acid was added and the temperature was raised to 80°C. Add a total of 60g of paraformaldehyde in batches, about 10g for the first feeding, and about 8g for each subsequent feeding. Control the feeding time within 45 minutes. After feeding, the temperature was raised to 95°C, and the reaction was stirred vigorously for about 5 hours. Raise the temperature to 160°C, distill under reduced pressure at a vacuum of -0.8 MPa, condense and recover the solvent through a condenser tube, and finally obtain a black viscous product, namely 345 g of fluorine-containing novolak resin.

[0037] The properties of the obtained fluorine-containing phenolic resin are: softening point 50°C (test standard: GB / T1633-2000), hydroxyl equivalent 137g / mol (test method:...

Embodiment 2

[0039] Add 300ml of toluene and 50ml of methyl ethyl ketone into a 500ml reaction kettle equipped with a thermometer, agitator and reflux condenser, add 380g of hexafluorobisphenol A and 7.6g of benzoic acid at the same time, stir at 50°C to fully dissolve and then heat up to 75°C . Then 50 g of paraformaldehyde was dissolved in methanol at a ratio of 1:6, and added to the hexafluorobisphenol A solution at a rate of 1 drop per second. After all the paraformaldehyde solution was dropped, the reaction temperature was raised to 95° C., and the reaction was stirred vigorously for about 7 hours. Finally, vacuum distillation was performed at 180° C. to distill off the solvent and unreacted substances to obtain about 403 g of fluorine-containing novolak resin.

[0040] The properties of the fluorine-containing phenolic resin are: softening point 60°C (test standard: GB / T 1633-2000), hydroxyl equivalent 145g / mol (test method: acetyl chloride titration hydroxyl value), and its average...

Embodiment 3

[0042] Add 400ml of benzene, 500g of hexafluorobisphenol A and 4g of salicylic acid into a 500ml reaction kettle equipped with a thermometer, stirrer and reflux condenser, stir at 60°C to fully dissolve and then heat up to 75°C. Then 49g of paraformaldehyde was added into the hexafluorobisphenol A solution three times. After the feeding was completed, the reaction temperature was raised to 95° C., and the reaction was vigorously stirred for about 7 hours. Finally, distill under reduced pressure at 200° C. to distill off the solvent and unreacted substances to obtain about 460 g of fluorine-containing novolak resin.

[0043] The properties of the fluorine-containing phenolic resin are: softening point 90°C (test standard: GB / T 1633-2000), hydroxyl equivalent 182g / mol (test method: acetyl chloride titration hydroxyl value), and its average molecular weight measured by GPC is 3100.

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Abstract

The invention discloses a fluorine-containing novolac resin, a preparation method of the fluorine-containing novolac resin and application of the fluorine-containing novolac resin, serving as a curing agent. The preparation method of the fluorine-containing novolac resin comprises the following step of performing a reaction of hexafluoro bisphenol A and solid paraformaldehyde by using organic acid as a catalyst to obtain the fluorine-containing novolac resin. The fluorine-containing novolac resin can be used as the curing agent to be cured with epoxide resin. High-content fluorine is induced into the curing agent, so that the comprehensive performance of an epoxide resin cured product is greatly promoted. A production process is controlled by adopting an acid catalysis method and a method of feeding paraformaldehyde serving as the raw material in batch. In the production process, the three wastes are not discharged, wherein a reaction solvent can be recycled. The production process is environmental-friendly. The structure of the fluorine-containing novolac resin is shown in the following formula (1) or (2).

Description

technical field [0001] The invention relates to a low molecular weight fluorine-containing phenolic resin and a preparation method thereof, and a curing method for curing fluorine-containing epoxy resin by using the fluorine-containing phenolic resin as a curing agent. Background technique [0002] As one of the three general-purpose thermosetting resins, epoxy resin has been receiving continuous attention and has been widely used in various fields. Epoxy resin contains unique active groups and polar groups such as epoxy groups, hydroxyl groups, ether bonds, etc., so it has many excellent properties and is widely used as semiconductor packaging materials, coatings, adhesives, molding materials, The matrix resin of fiber-reinforced composite materials, etc., is currently the most widely used high-performance composite material matrix resin. [0003] With the development of science and technology, new application fields have been continuously developed. In order to meet the s...

Claims

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Application Information

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IPC IPC(8): C08G8/20C08G59/62
Inventor 李欣欣仇伟李晓艳钱军潘金城马俊雄张书华
Owner ETERNAL CHEM (CHINA) CO LTD
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