Preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin

A technology of polymethyl methacrylate and polymethacrylic acid is applied in the fields of polymer chemistry and polymers, phosphorus-containing flame retardant resins and their preparation, and can solve problems such as flammability and thermal stability.

Inactive Publication Date: 2016-03-09
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Polymethyl methacrylate (PMMA) is a kind of general-purpose resin that is often used in production and life. However, as a kind of

Method used

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  • Preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin
  • Preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin
  • Preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin

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preparation example Construction

[0013] The preparation steps of phosphorus-containing flame-retardant polymethacrylic resin are:

[0014] In a reaction vessel equipped with a stirrer, a thermometer and a glass tube, add the formula amount of methyl methacrylate, tris((6-oxo-6H-dibenzo[c,e][1,2]oxophosphorus Heterohexacyclo-6-yl) methyl) phosphate and initiator benzoyl peroxide. Stir at 85.2°C for about 52 minutes. The system becomes viscous. Then pour the prepolymer into the mold and cool to about 40°C. The temperature is kept for 6 hours, and then the temperature is increased to 80°C for 12 hours to obtain a flame-retardant polymethacrylic resin.

[0015] According to the above-mentioned preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin, in terms of mass percentage, three ((6-oxo-6H-dibenzo[c,e][1,2] oxygen The formula of phosphahexyl-6-yl) methyl) phosphate is:

[0016] 6-(Hydroxymethyl)-6H-dibenzo[c,e][1,2]oxahexacyclo-6-oxide 9.87%~11.22%, phosphorus oxychloride 10.11%~...

Embodiment 1

[0043] In a reactor equipped with a stirrer, a thermometer, and a reflux condenser, 56.76 kg of xylene and 35.64 kg of DOPO are added and heated with stirring. DOPO is completely dissolved when the temperature is 85°C. Keep the same temperature, add 4.95kg paraformaldehyde in batches within 2h. After the feeding was completed, the temperature was raised to 120°C, the system refluxed, and the system turned from clear to turbid. Then keep the temperature for 6h and discharge. Wash the precipitate with a large amount of xylene while it is hot and filter with suction. Then place it at 120°C for 48h. A white powder HDOPO is obtained.

Embodiment 2

[0045] Add 5.57kg HDOPO and 32.48g dichloromethane solution to a reactor equipped with a thermometer and a gas pipe, and stir for 30min at 25°C. The temperature of the system was lowered to -8°C, 2.49g of triethylamine was added, stirred and kept for 30 minutes. Then began to drop a mixed solution of 5.78 kg of phosphorus oxychloride and 9.28 kg of methylene chloride. After the dripping is completed, keep the temperature at a low temperature for 2 hours, then heat to 25°C and stir for 6 hours. Discharge, evaporate the solvent and triethylamine in the system. The product was recrystallized to obtain the pure product TOPMP.

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Abstract

The invention relates to a preparation method of phosphorus-containing flame-retardant polymethyl methacrylate resin. A formula for preparing the phosphorus-containing flame-retardant polymethyl methacrylate resin comprises the following components by weight percent: 17.92 to 22.65 percent of tri((6-oxo-6H-dibenz [c,e][1,2] oxaphosphorin-6-yl)methyl) phosphate, 78.16 to 82.39 percent of methyl methacrylate and 0.16 to 0.76 percent of benzoperoxide. The preparation method comprises the following steps: adding a formula amount of methyl methacrylate, tri((6-oxo-6H-dibenz [c,e][1,2] oxaphosphorin-6-yl)methyl) phosphate and initiator benzoperoxide into a reaction container, stirring about 52 min at 85.2 DEG C, allowing the system to be viscous, then pouring a prepolymer into a mold, cooling to about 40 DEG C, performing the heat insulation for 6h, then heating to 80 DEG C, and performing the heat insulation for 12h to obtain the flame-retardant polymethyl methacrylate resin.

Description

Technical field [0001] The invention relates to a phosphorus-containing flame-retardant resin and a preparation method thereof, and belongs to the technical field of polymer chemistry and polymer technology. Background technique [0002] Polymethyl methacrylate (PMMA) is a general-purpose resin often used in production and life. However, as a kind of acrylic resin, it has the shortcomings of flammability and poor thermal stability, which makes it in the application process restricted. Adding flame retardant directly to the material is an effective means of flame retarding. Past studies have found that halogen flame retardants will release a large amount of smoke and toxic gases when they are thermally decomposed. Many countries have begun to ban the use of halogen-containing flame retardants. [0003] Phosphorus has many advantages as a flame-retardant element. It can exert flame-retardant effects in both the gas phase and the condensed phase. No toxic gases will be released dur...

Claims

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Application Information

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IPC IPC(8): C08F120/14C08K5/5313
Inventor 慕波郭永亮崔锦峰杨保平郭军红包雪梅张秀君周应萍郭宏伟胡清姜子燕倪恒健
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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