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Phosphor-silicon-containing aggregated flame retardant and preparation method thereof

A polymerized, flame retardant technology, applied in the field of flame retardants and their preparation, can solve the problems of large amount of flame retardants, poor flame retardant efficiency, poor compatibility, etc., achieve mild conditions and improve flame retardant. Efficiency, overcoming the effect of easy precipitation

Active Publication Date: 2017-10-20
宁波塑之华塑化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented new compound described by this patents allows for better interaction between certain chemicals like alcohols or amines when reacted together without forming unwanted side products. It does this through specific structures called trialkanes, making them easier to handle compared to previous methods. Additionally, its use results in improved fire resistance performance over existing ones.

Problems solved by technology

This patented technical solution describes how different types of chemical substances called phosphonium compounds (PQ) with strong fire resistance ability help improve the performance of various products made from these compositions.

Method used

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  • Phosphor-silicon-containing aggregated flame retardant and preparation method thereof
  • Phosphor-silicon-containing aggregated flame retardant and preparation method thereof
  • Phosphor-silicon-containing aggregated flame retardant and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0035] A preparation method of a phosphorus-containing, silicon-polymerized flame retardant, the steps of which are:

[0036] Weigh 1.6g ODOPB (5mmol) and 1.0g triethylamine (10mmol) into a 100mL three-necked flask, and add 50ml N,N-dimethylformamide (DMF for short), ultrasonically dissolve it completely and put it into a magneton , device buret, condenser, nitrogen device, heat up to 40 ° C, and weigh 0.645g dimethyldichlorosilane (abbreviated as DCDMS, 5mmol) at the same time, add 7ml DMF to dilute, and add it to the burette, slowly add DCDMS / The DMF solution was dropped in about 2 hours, and kept at this temperature for 1 hour after the drop. After the reaction, the reaction system was added to about 5 times of methanol to precipitate the product, vacuum filtered, the filter cake was washed twice with methanol, and dried in a vacuum oven (90kPa) at 80°C for 10h to obtain 1.65g of a yellowish powder. Yield 88%.

Embodiment 2

[0038] A preparation method of a phosphorus-containing, silicon-polymerized flame retardant, the steps of which are:

[0039] Weigh 1.6g ODOPB (5mmol) and 1.9g pyridine (25mmol) into a 100mL three-neck flask, and add 50ml tetrahydrofuran (THF), ultrasonically dissolve it completely and put it into a magnet, install a burette, a condenser, a nitrogen device, and heat up To 60°C, weigh 0.705 methylvinyldichlorosilane (DCMVS, 5mmol) and add 12ml THF to dilute it, and add it to the burette, slowly add DCMVS / THF dropwise under magnetic stirring, and drop it for about 1 hour. Temperature reaction 4h. After the reaction, add the reaction system to water about 10 times the volume of the reaction solution to precipitate the product, vacuum filter, wash the filter cake twice with distilled water, put it in a 60°C oven for 8 hours under vacuum (86kPa), and obtain 1.51g of orange Powder, yield 78%.

Embodiment 3

[0041] A preparation method of a phosphorus-containing, silicon-polymerized flame retardant, the steps of which are:

[0042] Weigh 1.6g ODOPB (5mmol) and 1.7g imidazole (25mmol) into a 100mL three-necked flask, and add 50ml N, N-dimethylformamide (DMF for short), ultrasonically dissolve it completely and put it into a magnet, and install a burette , condenser tube, nitrogen device, heat up to 60°C, weigh 0.705g of methylvinyldichlorosilane (DCMVS for short, 5mmol) and add 10ml of DMF to dilute, and add it to the burette, and slowly add the DCMVS / DMF solution dropwise under magnetic stirring , After about 1 hour of dripping, keep this temperature for 6 hours after dripping. After the reaction, the reaction system was added into water about 10 times the volume of the reaction solution to precipitate the product, vacuum filtered, the filter cake was washed twice with distilled water, and dried in a vacuum oven at 60°C for 11 hours under vacuum (82kPa) to obtain 1.78g Yellow pow...

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Abstract

The invention discloses a phosphor-silicon-containing aggregated flame retardant and a preparation method thereof. The preparation method comprises the following steps: adding 10-(2,5-dihydroxy phenyl)-9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and an acid-binding agent into a reactor loaded with a burette, a condensing tube and a nitrogen protection device, heating to 40 to 100 DEG C; weighing R1, R2-dichlorosilane, adding a solvent, and adding the mixture into the burette; adding the mixture at the temperature of 40 to 100 DEG C dropwise, and performing a thermal reaction for 2 to 10 hours after finishing of dropping; adding a precipitant, performing suction filtration, washing filter cakes with the precipitant, and drying to obtain the phosphor-silicon-containing aggregated flame retardant. The phosphor-silicon-containing aggregated flame retardant has high phosphor content and silicon content, abundant carbon sources, high char forming characteristic, superior flame retardance and thermal stability, and can be applied to high-molecular materials such as flame-retardant polypropylene, polystyrene and epoxy resin.

Description

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Claims

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Application Information

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Owner 宁波塑之华塑化有限公司
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