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Novel phosphorus series compound as well as preparation method and application thereof

A technology of phosphorus compounds and compounds, which is applied in the field of preparing flame-retardant epoxy resin hardeners, and can solve the problems of rosic acid being expensive and uneconomical

Inactive Publication Date: 2013-01-09
CHANG CHUN PLASTICS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw material rosolic acid (rosolic acid) for synthesizing dopotriol in the literature is very expensive, and it is not economical for industrial applications

Method used

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  • Novel phosphorus series compound as well as preparation method and application thereof
  • Novel phosphorus series compound as well as preparation method and application thereof
  • Novel phosphorus series compound as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0092] The implementation of the above related inventions can be represented by flow process 1, and we will illustrate with the following specific examples.

[0093]

[0094] Process 1

example 1

[0096] Synthesis of Compound A

[0097] Compound A is obtained by reacting DHBP, DOPO and phenol under the catalysis of an acidic catalyst. The synthesis steps are as follows: in a 1-liter three-necked reactor with a temperature indicating device, add 26.75 grams (0.125 moles) of DHBP (4, 4′-dihydroxybenzophenone), 27.00 grams (0.125 moles) of DOPO (9,10-dihydro-9-oxa-10-phosphophenanthrene 10-oxide), 100 grams of phenol and 1.10 grams of Sulfuric acid, raise the reaction temperature to 130°C, maintain the temperature of the reaction system at 130°C, react for 12 hours, drop into 500 ml of hot water and stir to precipitate, which is Compound A.

[0098] After suction and filtration, the filter cake was washed with a large amount of hot water, separated by filtration, and dried in a vacuum oven at 110°C to obtain 54.50 g of Compound A with a yield of 86% and a melting point of 294°C.

[0099] Compound A 1 H NMR with 13 CNMR spectrum, 31 P NMR spectra are shown in figure 1 ...

example 2

[0101] Synthesis of Compound B

[0102] Compound B is obtained by reacting DHBP, DOPO and 2-cresol under the catalysis of an acidic catalyst. The synthesis steps are as follows: In a 1-liter three-neck reactor with a temperature indicating device, add 21.40 grams (0.1 mole) of DHBP , 21.60 grams (0.1 moles) of DOPO, 100 grams of 2-cresol and 1.10 grams of sulfuric acid, raise the reaction temperature to 130 ° C, the temperature of the reaction system is maintained at 130 ° C, after 12 hours of reaction, drop 100 milliliters of toluene Stirring and precipitation in the medium, an orange-red sticky substance was obtained. After removing the toluene, the sticky substance was dissolved with ethanol and dropped into deionized water for precipitation.

[0103] After separation by filtration, the filter cake was vacuum-dried in a vacuum oven at 100°C to obtain 35.00 g of Compound B as an orange-red solid with a yield of 67% and a melting point of 284°C.

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PUM

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Abstract

The invention provides a phosphorus series compound disclosed in a general formula (1), wherein substitutional radicals of R1-R10, A, B, D, X, Y, R11-R12, and the like are defined in a specification. The invention provides a method for preparing a compound disclosed in the general formula (1). The invention also provides a hardener. The invention also provides flame-resistant epoxy resin and a preparation method thereof.

Description

technical field [0001] The invention discloses a phosphorus-containing compound, which can be used as an epoxy resin hardener and used for preparing flame-retardant epoxy resin hardened products. Background technique [0002] Epoxy resin has the advantages of excellent electrical properties, shape stability, high temperature resistance, solvent resistance, low cost and high adhesion, and is most suitable for printed circuit boards and integrated circuit packaging materials. However, epoxy resin is as easy to burn as general plastic materials and endangers life. Therefore, there are strict requirements for the flame retardancy of electronic and information materials used all over the world. Epoxy resins containing bromine atoms are especially suitable for circuit boards with flame retardant properties. However, these bromine-containing epoxy resins release corrosive and toxic substances such as tetrabromodibenzo-p-dioxin and tetrabromodibenzofuran during combustion. In addi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08G59/40C08L63/00C08K5/5373
Inventor 林庆炫林宗立张家玮黄坤源杜安邦苏芳贤
Owner CHANG CHUN PLASTICS CO LTD