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P/N/Si-multi-element-containing poly-phosphorus-silazane fire retardant for epoxy resin and preparing method thereof

A multi-element technology for epoxy resin, applied in the field of P/N/Si multi-element polyphosphosilazane flame retardant for epoxy resin and its preparation, can solve the problem of poor heat resistance of cured epoxy resin High, poor mechanical properties and other problems, to achieve the effect of easy to achieve large-scale production, high quality retention rate, and improve flame retardant effect

Active Publication Date: 2019-01-04
库贝化学(上海)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the reactive flame retardant epoxy monomer or curing agent can better maintain the physical properties of the material while achieving flame retardancy, there are also defects such as low heat resistance and poor mechanical properties of the cured epoxy resin.

Method used

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  • P/N/Si-multi-element-containing poly-phosphorus-silazane fire retardant for epoxy resin and preparing method thereof
  • P/N/Si-multi-element-containing poly-phosphorus-silazane fire retardant for epoxy resin and preparing method thereof
  • P/N/Si-multi-element-containing poly-phosphorus-silazane fire retardant for epoxy resin and preparing method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of P / N / Si Multi-element Polyphosphosilazane Flame Retardant

[0026] Under the protection of high-purity nitrogen, add DOPO and chloroform to the three-necked flask in turn, raise the temperature to 45°C, and after DOPO is completely dissolved, add the mixed solution of PVSZ and chloroform, and stir for a certain period of time. Then add the mixed solution of AIBN and chloroform through the constant pressure dropping funnel, continue to maintain the temperature at 45 ° C for 24 hours, after the reaction, filter with suction and collect the filtrate. P / N / Si multi-element polyphosphosilazane flame retardant for epoxy resin. In this example, the molar ratio of PVSZ to DOPO is 1:1, the amount of AIBN is 0.2% of DOPO moles, and the structure of the obtained flame retardant is:

[0027]

[0028] The structural characterization data are:

[0029] FTIR: 3312cm -1 (N-H), 3042cm -1 (Ph-H), 2984cm -1 (CH 3 ), 2137cm -1 (Si-H), 1460cm -1 (P-C), 1261cm -1 (Si...

Embodiment 2

[0033] Preparation of P / N / Si Multi-element Polyphosphosilazane Flame Retardant

[0034] Under the protection of high-purity nitrogen, add DOPO and toluene in turn to the three-necked flask, raise the temperature to 80°C, and after DOPO is completely dissolved, add the mixed solution of PVSZ and toluene, and stir for a certain period of time. Then add the mixed solution of AIBN and toluene through the constant pressure dropping funnel, continue to maintain the temperature at 80 ° C for 10 h, after the reaction, filter with suction and collect the filtrate, the filtrate is post-treated by washing, distillation, purification, etc., and vacuum-dried to obtain P / N / Si multi-element polyphosphosilazane flame retardant for epoxy resin. In this embodiment, the molar ratio of PVSZ to DOPO is 1:3, and the amount of AIBN is 0.5% of the molar number of DOPO.

[0035] The structural characterization data are:

[0036] FTIR: 3334cm -1 (N-H), 3036cm -1 (Ph-H), 2991cm -1 (CH 3 ), 2130cm ...

Embodiment 3

[0039] Application of P / N / Si Multi-element Polyphosphosilazane Flame Retardant in Epoxy Resin

[0040] The limiting oxygen index of the 4,5-epoxycyclohexane-1,2-diglycidyl carboxylate epoxy resin modified with the product obtained in Example 1 (addition mass fraction is 10%) is 38.0%, UL- 94 vertical combustion can reach V-0 level, which has good flame retardant effect; after modification, the epoxy resin is stable at N 2 TGA in the atmosphere (heating rate is 10°C / min) (such as figure 2 ) The results show that: weight loss 5% (T d5 ) and 10% weight loss (T d10 ) corresponding temperatures are 320°C and 356°C respectively, and the temperature corresponding to the maximum thermogravimetric rate (T dmax ) is 407°C, the mass retention rate at 600°C is 33.2%, and has good thermal stability.

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Abstract

The invention discloses a P / N / Si-multi-element-containing poly-phosphorus-silazane fire retardant for epoxy resin and a preparing method thereof. The fire retardant is obtained after a C=C key in a PVSZ structure and a P-H key in a DOPO structure are subjected to an addition reaction. The preparing method includes the following steps that under protection of inert gas, an AIBN serves as an initiating agent, and through the addition reaction between the PVSZ and the DOPO, the P / N / Si-multi-element-containing poly-phosphorus-silazane fire retardant for the epoxy resin is prepared with the one-step method, wherein the molar ratio of the PVSZ to DOPO is 1:(1-3). The method has the advantages that the raw materials are easy to obtain, the technology is simple, the method is fast, simple and convenient, and large-scale production is easy to achieve; the main chain of the fire retardant prepared with the method is a Si-NH repetition structure unit, and can be subjected to a cross-linking reaction with the epoxy resin, and the good heat stability and the high quality retention rate are provided for the fire retardant; a phosphaphenanthrene structure of a side chain can generate phosphoric-acid substances in the combustion process, fast dehydration and carbonization of the surface of a polymer are promoted, and a carbonized layer or a non-combustible layer is formed to cover a base material; meanwhile, P / N / Si multi-elements in the structure can also have the synergistic flame retardant effect, and the flame retardant effect is further improved.

Description

technical field [0001] The invention belongs to the technical field of synthesis of phosphorus-containing flame retardants, and in particular relates to a P / N / Si multi-element polyphosphosilazane flame retardant for epoxy resins and a preparation method thereof. Background technique [0002] Epoxy resin is a class of organic compounds containing two or more epoxy groups in its molecule. It is widely used in aviation because of its good adhesion, heat resistance, chemical stability and easy molding and processing. Aerospace, mechanical construction and electrical and electronic fields. However, general-purpose epoxy resins have poor thermal stability and are extremely flammable, posing a serious threat to life and property safety. Therefore, the development of new halogen-free, high-efficiency flame-retardant, and good thermal stability epoxy resin materials has become a hot spot in the current research field. [0003] At present, there are two main ways to improve and enha...

Claims

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Application Information

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IPC IPC(8): C08L63/00C08L83/16C08G77/62
CPCC08G77/62C08L63/00C08L2201/02C08L2201/08C08L83/16
Inventor 陈明锋范先谋李治农李珊珊刘灿培
Owner 库贝化学(上海)有限公司
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