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A kind of phosphorus, silicon polymerized flame retardant and preparation method thereof

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

Active Publication Date: 2020-06-23
宁波塑之华塑化有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the existing flame retardants in the prior art, such as large amount of addition, poor compatibility, and poor flame retardant efficiency, and to provide a phosphorus-containing and silicon-polymerized flame retardant and a preparation method thereof
The flame retardant of the present invention has mild preparation conditions, contains phosphorus and silicon elements, and has good thermal stability and flame retardancy; meanwhile, the silicon element contained in the main chain and polymer materials such as non-polar polyolefins also have Good compatibility; therefore, the polymeric phosphorus and silicon flame retardant of the present invention can solve the disadvantages of poor compatibility between existing flame retardants and polymer materials, and has the advantages of low toxicity and environmental protection, and is stable in the polymer matrix. Not easy to migrate, has good durability

Method used

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  • A kind of phosphorus, silicon polymerized flame retardant and preparation method thereof
  • A kind of phosphorus, silicon polymerized flame retardant and preparation method thereof
  • A kind of phosphorus, silicon polymerized flame retardant and preparation method thereof

Examples

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Effect test

Embodiment 1

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

[0036] Weigh 1.6g ODOPB (5mmol) and 1.0g triethylamine (10mmol) into a 100mL three-necked flask, and add 50ml N,N-dimethylformamide (abbreviated as DMF), ultrasonically dissolve it completely and put in the magnet , The device burette, condenser, nitrogen device, heated to 40 ℃, while weighing 0.645g dimethyldichlorosilane (abbreviated as DCDMS, 5mmol) added 7ml DMF dilution, and added to the burette, slowly adding DCDMS / under magnetic stirring DMF solution, drip in about 2h, keep this temperature for 1h after dripping. After the reaction, the reaction system was added to about 5 times methanol to precipitate the product, vacuum filtered, the filter cake was washed twice with methanol, and dried in an oven at 80°C under vacuum (90kPa) for 10 hours to obtain 1.65g of slightly yellow powder. The yield was 88%.

Embodiment 2

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

[0039] Weigh 1.6g ODOPB (5mmol) and 1.9g pyridine (25mmol) into a 100mL three-necked flask, and add 50ml of tetrahydrofuran (THF), ultrasonically dissolve it completely and put it in a magnet, install a burette, condenser, and nitrogen device, and heat up To 60℃, weigh 0.705 methyl vinyl dichlorosilane (DCMVS, 5mmol) and add 12ml THF to dilute, and add it to the burette, slowly add DCMVS / THF dropwise under magnetic stirring, drop it for about 1h, keep it at this level after dropping The temperature reacts for 4h. After the reaction, the reaction system was added to 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 placed in an oven at 60°C and dried under vacuum (86kPa) for 8 hours to obtain 1.51g of orange Powder, the yield is 78%.

Embodiment 3

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

[0042] Weigh 1.6g ODOPB (5mmol) and 1.7g imidazole (25mmol) into a 100mL three-necked flask, and add 50ml of N,N-dimethylformamide (abbreviated as DMF), ultrasonically dissolve it completely and put it in a magnet, and install a burette , Condensing tube, nitrogen device, heating up to 60℃, while weighing 0.705g methyl vinyl dichlorosilane (DCMVS for short, 5mmol), adding 10ml DMF to dilute, and adding to the burette, slowly adding DCMVS / DMF solution dropwise under magnetic stirring After dripping in about 1h, keep this temperature for 6h after dripping. After the reaction, the reaction system was added to 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 (82kPa) at 60°C for 11h to obtain 1.78g micro Yellow powder, yield 92%.

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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

Technical field [0001] The invention belongs to a flame retardant and its preparation, and relates to a phosphorous and silicon polymerized flame retardant and a preparation method thereof. The phosphorus-containing, silicon polymerized flame retardant of the present invention is particularly suitable for flame retardant of polypropylene, polystyrene, epoxy resin and the like. Background technique [0002] Flame retardants have been widely used as additives for polymer materials, including plastic processing and new materials. In the 1980s, halogen flame retardants were widely used due to their high flame retardant efficiency. However, since the Dioxin incident in 1986, halogenated flame retardants have faced tremendous environmental pressure. At present, as environmentally friendly phosphorus and silicon flame retardants, more and more attention has been paid due to their simple processing technology, good thermal stability and flame retardant properties. [0003] Phosphorus and...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/00C07F9/6574C08L23/12C08L83/00C08L63/00C08L25/06C08K5/5425
CPCC07F9/657172C08G77/00C08K5/5425C08L23/12C08L25/06C08L63/00C08L2201/02C08L2201/08C08L83/00
Inventor 胡小平缪飞
Owner 宁波塑之华塑化有限公司
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