A kind of hyperbranched phosphorus-containing polysiloxane flame retardant and preparation method thereof

A polysiloxaborane and flame retardant technology, applied in the field of flame retardants, can solve the problems of low flame retardant efficiency, low flame retardant efficiency, poor matrix compatibility, etc., achieve high flame retardant efficiency and reduce volatility Production of substances, effects of improving flame retardancy and heat resistance

Active Publication Date: 2021-03-16
FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most single-element flame retardants have disadvantages such as low flame retardant efficiency and poor compatibility with the matrix, such as 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) Flame retardant is a phosphorus-based flame retardant widely used in polymer materials at present. It has disadvantages such as low flame retardant efficiency and poor compatibility with the matrix.

Method used

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  • A kind of hyperbranched phosphorus-containing polysiloxane flame retardant and preparation method thereof
  • A kind of hyperbranched phosphorus-containing polysiloxane flame retardant and preparation method thereof
  • A kind of hyperbranched phosphorus-containing polysiloxane flame retardant and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Under the protection of inert gas, DOPO (20mmol, 4.32g), dichloroethane solvent (30mL), TEA (22mmol, 3.1mL), APTS (20mmol, 4.67mL) were added successively to the three-necked flask, and stirred until Uniformly, then add CCl dropwise at 0°C 4 (22mmol, 2.13mL), after the dropwise addition, keep it at 30°C for 20h, and get the APTS-DOPO intermediate after suction filtration, washing and drying.

[0029] (2) Add dichloroethane (20mL) and phenylboronic acid (15mmol, 1.83g) into a three-necked flask and stir until dissolved, and dissolve the intermediate APTS-DOPO (10mmol, 4.35g) in dichloroethane (20mL) , into the three-necked flask drop by drop through the constant pressure dropping funnel, after the dropwise addition, the temperature was raised to 80°C for reflux reaction for 8 hours, after the reaction was completed, the hyperbranched phosphorus-containing polysiloxane boron was obtained after suction filtration, washing and drying alkanes flame retardants.

[0030]...

Embodiment 2

[0035] (1) Under the protection of inert gas, sequentially add DOPO (20mmol, 4.32g), 30mL dichloroethane solvent, TEA (22mmol, 3.1mL), APTS (20mmol, 4.67mL) into the three-necked flask, and stir until uniform, Then add CCl dropwise at -5°C 4 (22mmol, 2.13mL), after the dropwise addition, react at 40°C for 25h, and obtain the APTS-DOPO intermediate after suction filtration, washing and drying.

[0036] (2) Add dichloroethane (20mL) and methyl boric acid (30mmol, 1.8g) into a three-necked flask and stir until dissolved; dissolve the intermediate APTS-DOPO (20mmol, 8.71g) in dichloroethane (20mL) In the above-mentioned three-neck flask, the temperature was raised to 80° C. for reflux reaction for 10 hours through a constant-pressure dropping funnel. After the reaction is finished, the hyperbranched phosphorus-containing polysiloxaborane flame retardant is obtained after suction filtration, washing and drying.

[0037] The resulting hyperbranched phosphorus-containing polysiloxa...

Embodiment 3

[0042] (1) Under the protection of inert gas, DOPO (20mmol, 4.32g), dichloroethane (30mL) solvent, TEA (22mmol, 3.1mL), APTS (20mmol, 4.67mL) were added successively to the three-necked flask, and stirred until uniform. Then add CCl dropwise at 5°C 4 (22mmol, 2.13mL), after the dropwise addition, react at 20°C for 20h, and obtain the APTS-DOPO intermediate after suction filtration, washing and drying.

[0043](2) Add dichloroethane (20mL) and cyclopropylboronic acid (30mmol, 2.58g) into a three-necked flask and stir until dissolved; dissolve the intermediate APTS-DOPO (20mmol, 8.71g) in dichloroethane (20mL ), and transferred it to a constant pressure dropping funnel, and added dropwise to the above-mentioned three-necked flask. After the dropwise addition, the temperature was raised to 80° C., and the reaction was carried out under reflux for 15 hours. After the reaction is finished, the hyperbranched phosphorus-containing polysiloxaborane flame retardant is obtained after...

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Abstract

The invention provides a hyperbranched phosphorus-containing polysiloxyborane flame retardant and a preparation method thereof. The flame retardant is obtained by using 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), 3-aminopropyltriethoxysilane (APTS), and a boric acid compound as main raw materials through two steps. The first step, a DOPO-based intermediate (APTS-DOPO) is produced bya reaction of P-H of DOPO and -NH2 of APTS under certain conditions; and the second step, the hyperbranched phosphorus-containing polysiloxyborane flame retardant is obtained by a reaction of ethoxylof the DOPO-based intermediate obtained by the first step and -OH of the boric acid compound. A Si-O-B structure is designed in a structural unit of the flame retardant, and thus a modified materialis endowed with good mechanical properties and thermal stability; and flame retardant elements such as Si, B, N, P and the phosphaphenanthrene group in the structure can improve flame retardant and heat resistant properties of the material. A modified material prepared by adding the flame retardant has the advantages of low smoke and low toxicity, high flame retardant efficiency, and the like, canbe widely applied to polymer materials such as epoxy resin and unsaturated resin, and has broad application prospects.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a hyperbranched phosphorus-containing polysiloxane flame retardant and a preparation method thereof. Background technique [0002] Polymer materials have excellent characteristics such as light weight, good chemical stability, and easy processing, and are widely used in transportation, electrical and electronic, building materials and other fields. However, most polymer materials are extremely flammable, which increases safety hazards while providing convenience. Therefore, it is of great significance to develop efficient flame retardants. [0003] Flame retardants for polymer materials can be divided into two types: halogen-based and non-halogenated flame retardants, and halogen-based flame retardants will release a large amount of toxic fumes when burned. Therefore, the development of new halogen-free flame retardants with high efficiency, low smoke and low toxicity ...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G77/30C08L83/08
CPCC08G77/30C08L83/08C08L2201/02
Inventor陈明锋林修煌苏丽评李珊珊李治农刘灿培
OwnerFUJIAN NORMAL UNIV