Method for preparing microcapsule red phosphorus inflaming retarding polylactic acid

A technology of microencapsulated red phosphorus and polylactic acid is applied in the directions of dyeing physical treatment, fibrous filler, dyeing polymer organic compound treatment, etc. , the preparation process is simple and environmentally friendly

Active Publication Date: 2010-04-21
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

J Zhan et al. (Polymer Degradation and Stability, 2009, 94: 291-296) used pentaerythritol diphosphoryl chloride and melamine, with dimethylformamide as solvent, and reflux reaction at 160°C for 6 hours to obtain the flame retardant pentaerythritol diphosphate Melamine salt is mixed with polylactic acid by double-roller milling (temperature: 165°C, speed: 35 rpm, time: 10 minutes) and then hot-pressed. The experiment found that when the amount of flame retardant added is 25%, , the flame retardant performance of the composite material reaches UL94-V0 level, and the limiting oxygen index is 38, but the disadvantage of this method is that a large amount of organic solvent is needed in the reaction process, which is not conducive to industrial production

Method used

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  • Method for preparing microcapsule red phosphorus inflaming retarding polylactic acid
  • Method for preparing microcapsule red phosphorus inflaming retarding polylactic acid
  • Method for preparing microcapsule red phosphorus inflaming retarding polylactic acid

Examples

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Effect test

Embodiment 1

[0039] (1) 25.0 grams of pretreated red phosphorus, 0.375 grams of sodium lauryl sulfate and 400 milliliters of distilled water are made into a suspension, and 137.0 grams of aluminum sulfate solution with a mass concentration of 10% are slowly added under magnetic stirring, and the system is heated After reaching 75°C, use 25% ammonia water to adjust the pH value to 8-9, stir and keep warm for 2 hours to obtain aluminum hydroxide-coated red phosphorus suspension.

[0040](2) Add 3.2 grams of melamine and 6.2 grams of 37% formaldehyde solution into the reaction vessel, adjust the pH value of the system to 8-9 with 25% ammonia water, stir and heat to 90°C, and keep it for 50 minutes to obtain colorless and transparent melamine formaldehyde resin prepolymer solution. Add all the above prepolymer solution into the aluminum hydroxide-coated red phosphorus suspension, adjust the pH value of the system to 4-5 with glacial acetic acid, and keep stirring for 2 hours. After the reacti...

Embodiment 2

[0045] (1) 30.0 grams of pretreated red phosphorus, 0.3 gram of sodium hexametaphosphate and 300 milliliters of distilled water are made into a suspension, slowly add 164.5 grams of aluminum sulfate solution with a mass concentration of 10% under magnetic stirring, and the system is heated to 90 ℃, adjust the pH value to 8-9 with 25% ammonia water, stir and keep warm for 5 hours to obtain aluminum hydroxide-coated red phosphorus suspension.

[0046] (2) Add 16.5 grams of melamine and 31.8 grams of 37% formaldehyde solution into the reaction vessel, adjust the pH value of the system to 8-9 with 25% ammonia water, stir and heat to 85°C, and keep warm for 1 hour to obtain colorless and transparent melamine formaldehyde resin prepolymer solution. Add all the above prepolymer solution into the aluminum hydroxide-coated red phosphorus suspension, adjust the pH value of the system to 4-5 with glacial acetic acid, and keep stirring for 1 hour. After the reaction, the suspension was c...

Embodiment 3

[0051] (1) 20.0 grams of pretreated red phosphorus, 0.4 grams of OP-10 and 250 milliliters of distilled water are made into a suspension, slowly add 78.0 grams of aluminum chloride solution with a mass concentration of 10% under magnetic stirring, and the system is heated to 60 After ℃, use 25% ammonia water to adjust the pH value to 8-9, stir and keep warm for 4 hours to obtain aluminum hydroxide-coated red phosphorus suspension.

[0052] (2) Add 7.2 grams of melamine and 13.8 grams of 37% formaldehyde solution into the reaction vessel, adjust the pH value of the system to 8-9 with 25% ammonia water, stir and heat to 80°C, and keep warm for 70 minutes to obtain a colorless and transparent melamine formaldehyde resin prepolymer solution. Add all the above prepolymer solution into the aluminum hydroxide-coated red phosphorus suspension, adjust the pH value of the system to 4-5 with glacial acetic acid, and keep stirring for 3 hours. After the reaction, the suspension was coole...

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Abstract

The invention belongs to the technical field of inflaming retarding modification of high polymer materials, and specifically relates to a method for preparing microcapsule red phosphorus inflaming retarding polylactic acid. The method comprises the following steps of: pre-treating red phosphorus, and preparing melamine formaldehyde resin prepolymer solution; adding the pretreated red phosphorus, distilled water which is 2 to 20 times of the quantity of the red phosphorus and a dispersing agent which is 0.5 to 2 percent of the quantity of the red phosphorus into a reaction vessel; stirring the mixture and heating the mixture to a temperature of between 60 and 90 DEG C to obtain a red phosphorus suspension; then adding metal salt solution into the suspension; adjusting the pH value of the system by using ammonia water; keeping the temperature and stirring the mixture; adding the mixture into the melamine formaldehyde resin prepolymer solution so that the resin content in the solution is 22 to 94 percent of quantity of the red phosphorus; adjusting the pH value of the system to between 4 and 5 by using glacial acetic acid, keeping the temperature and stirring the mixture; after the reaction is finished, cooling and filtering the suspension, washing the suspension to be neutral, and drying the suspension to obtain inorganic-organic double-layer coated microcapsule red phosphorus; grinding the obtained microcapsule red phosphorus, and drying polylactic acid to remove the moisture; and adding the obtained microcapsule red phosphorus and the polylactic acid into a drying container, mixing the obtained microcapsule red phosphorus and the polylactic acid evenly, and melting and blending the mixture to obtain the required product. In the product, the polylactic acid accounts for 65 to 75 percent and the microcapsule red phosphorus accounts for 25 to 35 percent. The method has a low cost and a simple and environment-friendly preparation process.

Description

technical field [0001] The invention belongs to the technical field of flame-retardant modification of polymer materials, and in particular relates to a preparation method of microcapsule red phosphorus flame-retardant polylactic acid. Background technique [0002] The growing awareness of environmental protection and energy shortage have aroused people's attention to the research, development and application of biodegradable materials. Polylactic acid is a type of polymer chemically synthesized from microbial fermentation product lactic acid as a monomer. It is a non-toxic, non-irritating, good biocompatibility, biodegradable and absorbable polyester linear biodegradable polymer. Material. So far, polylactic acid has been able to carry out various molding processes like ordinary polymers. The various films, sheets, and fibers prepared by it have undergone secondary processing such as thermoforming and spinning in clothing, textiles, non-woven fabrics, packaging, Agricultu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/04C08K9/10C09C1/00C09C3/04C09C3/10
Inventor 任杰常少坤陈大凯李菁
Owner TONGJI UNIV
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