Organic phosphorus active flame-proof epoxy resin curing agent amine group phosphonate and preparation method thereof

An epoxy resin curing and amino phosphonate technology, which is applied in the field of organophosphorus active flame retardant epoxy resin curing agent amino phosphonate and its preparation, can solve the problem of unsatisfactory flame retardant effect of epoxy resin cured products, etc. problem, to achieve the effect of simple method and easy operation

Inactive Publication Date: 2008-01-02
HEILONGJIANG INST OF PETROCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the flame retardant effect of cured epoxy resin is not ideal at pr

Method used

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  • Organic phosphorus active flame-proof epoxy resin curing agent amine group phosphonate and preparation method thereof
  • Organic phosphorus active flame-proof epoxy resin curing agent amine group phosphonate and preparation method thereof
  • Organic phosphorus active flame-proof epoxy resin curing agent amine group phosphonate and preparation method thereof

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specific Embodiment approach 1

[0015] Specific embodiment one: the present embodiment amino phosphonate is made of dehydrated alcohol, phosphorus trichloride, organic amine (structural formula is H 2 N-R-NH 2 ) and acetone at a molar ratio of 3:1:1:1; the organic amine is diethylenetriamine, triethylenetetramine, tetraethylenepentamine or 4,4-diaminodiphenylmethane.

specific Embodiment approach 2

[0016] Specific embodiment two: the preparation method steps of organophosphorus active flame retardant epoxy resin curing agent amino phosphonate in the present embodiment are as follows: 1, synthetic diethyl phosphite: add 3mol anhydrous in every 100ml anhydrous benzene Proportion of ethanol Mix anhydrous ethanol and anhydrous benzene until uniform, then cool to 5-15°C, start the agitator, stir at a speed of 300-600r / min, and add dropwise at a speed of 3-5 drops per second The mixture of phosphorus trichloride and anhydrous benzene, wherein the mixture of phosphorus trichloride and anhydrous benzene is mixed according to the ratio of adding 1mol of distilled phosphorus trichloride per 100ml of anhydrous benzene, and absolute ethanol and three The molar ratio of phosphorus chloride is 3:1, the reaction temperature is kept between 5-15°C, and the reaction time is 0.8-1h; the reaction product is quickly moved into a vacuum distillation device, and under the condition of a water ...

specific Embodiment approach 3

[0018] Embodiment 3: In this embodiment, in step 1, the mixture of absolute ethanol and anhydrous benzene is cooled to 5-10°C. Others are the same as in the second embodiment.

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Abstract

The invention discloses an organophosphorus active flame-proof epoxide resin solidifying agent amino phosphonate ester and the preparing method. The amino phosphonate ester comprises the following parts: 3:1:1:1 absolute ethyl alcohol, phsophorus trichloride, organic amine (the structural formula is H2N-R-NH2)and acetone. The organic amine is diethylenetriamine, triethylene tetraamine, tetraethylene pentamine or 4, 4-diaminodiphenylmethane. The method comprises the following steps: 1, synthesizing diethyl phosphate with alcohol and phsophorus trichloride; 2, generating ketoimine with acetone and the organic amine by adding the anhydrating agent; 3, generating amino phosphonate with diethyl phosphate and ketoimine. The oxygen index of the product is more than 20 and less than 34.6. The invention is provided with the simple method and the simple operation.

Description

technical field [0001] The invention relates to an organic amine epoxy resin curing agent and a preparation method thereof, in particular to an organic phosphorus active flame-retardant epoxy resin curing agent aminophosphonate and a preparation method thereof. Background technique [0002] Since the commercialization of epoxy resin, its output and application have occupied an important position in the field of thermosetting plastics, and its consumption has been rising steadily. However, epoxy resin is a flammable resin, and its oxygen index is generally around 19.8. In recent years, various application fields have put forward higher requirements for the flame retardancy of epoxy resins. Phosphorus-based flame retardants have a good flame-retardant effect, but additive phosphorus-based flame retardants often have certain adverse effects on the physical and mechanical properties of cured epoxy resins, while reactive phosphorus-based flame retardants can To a considerable ex...

Claims

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Application Information

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IPC IPC(8): C08K5/5353C08L63/00
Inventor 曲春艳王德志张杨冯浩
Owner HEILONGJIANG INST OF PETROCHEM
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