Full-bio-based flame retardant, flame-retardant PLA composite material and preparation method thereof

A composite material and all-biological technology, applied in the field of design and synthesis of flame retardants, can solve the problems of non-environmental protection, large addition amount, low flame retardant efficiency, etc., and achieve the effect of cost reduction, low addition amount and excellent effect

Active Publication Date: 2020-07-24
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the problems of low flame retardant efficiency, large addition amount and non-environmental protection of traditional PLA flame retardants, the present invention provides a high-efficiency, environment-friendly, low-addition all-bio-based flame retardant for PLA

Method used

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  • Full-bio-based flame retardant, flame-retardant PLA composite material and preparation method thereof
  • Full-bio-based flame retardant, flame-retardant PLA composite material and preparation method thereof
  • Full-bio-based flame retardant, flame-retardant PLA composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] In a constant temperature water bath at 55°C, dissolve 37.7g of 70% phytic acid solution in 158.4mL of distilled water, and then slowly add ammonia water to adjust the pH to pH=4.5. Add it into the phytic acid solution and react for 5 hours; after the reaction, cool the reaction product to room temperature, add 600ml of ethanol to recrystallize and precipitate the reaction product, filter it with suction and dry it to obtain a full bio-based flame retardant with a yield of 76%. figure 1 It is an infrared comparison chart of the bio-based flame retardant prepared in Example 1 and raw materials phytic acid and sulfur-containing amino acid (taurine). From figure 1 It can be seen that the flame retardant contains all the characteristic peaks of phytic acid and taurine, while at 1490cm -1 A new characteristic peak appeared, belonging to -NH 3 + The stretching vibration peak of phytic acid and taurine can be proved that phytic acid and taurine have reacted successfully.

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Embodiment 2

[0044] In a constant temperature water bath at 60°C, dissolve 37.7g of 70% phytic acid solution in 208.4mL of distilled water, then slowly add ammonia water to adjust the pH to pH = 3, and dissolve 57.6g of cystine in the aqueous solution, and slowly dissolve the cystine solution Add it into the phytic acid solution and react for 6 hours; after the reaction, cool the reaction product to room temperature, add 750ml of methanol to recrystallize and precipitate the reaction product, filter it with suction and dry it to obtain a full bio-based flame retardant with a yield of 69%.

[0045] 2.5g (5.0wt% addition) of the full bio-based flame retardant prepared in Example 2 and 47.5g of dried PLA were mixed uniformly and then put into an internal mixer for melting processing. The processing temperature was 170° C., and the time for 8min. The measured LOI of the composite material is 32.5, the vertical burning grade is FV-0 grade (3mm) grade, and the tensile strength is 59.2MPa.

Embodiment 3

[0047] In a constant temperature water bath at 65°C, dissolve 37.7g of 70% phytic acid solution in 258.4mL of distilled water, then slowly add ammonia water to adjust the pH to pH = 5, and at the same time dissolve 71.5g of methionine in the aqueous solution and then dissolve the methionine The solution was slowly added to the phytic acid solution, and reacted for 4.5 hours; after the reaction, the reaction product was cooled to room temperature, and 800ml of ethanol was added to recrystallize to obtain the reaction product, which was filtered and dried to obtain a full bio-based flame retardant with a yield of 78%.

[0048] 1.25g (2.5wt% addition) of the full bio-based flame retardant prepared in Example 3 and 48.75g of dried PLA were mixed uniformly and put into an internal mixer for melting and processing. The processing temperature was 160° C., and the time 10min. The measured LOI of the composite material is 30.5, the vertical burning grade is FV-0 grade (3mm) grade, and...

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Abstract

The invention relates to the technical field of design and synthesis of flame retardants, aims at the problems that a traditional flame retardant for PLA is low in flame retardant efficiency, large inadditive amount and not environmentally friendly, and provides a full-bio-based flame retardant, a flame-retardant PLA composite material and a preparation method thereof. The full-bio-based flame retardant has the following structural general formula: in the formula, A < + > is amino protonated biomass sulfur-containing amino acid, and n=1-12. The raw materials used by the all-bio-based flame retardant are phytic acid and sulfur-containing amino acid from biological sources, i.e., the synthesized flame retardant is the all-bio-based flame retardant, and the all-bio-based flame retardant is green in source and conforms to the theme of sustainable development at present and can relieve petroleum shortage crisis and can protect the global environment.

Description

technical field [0001] The invention relates to the technical field of design and synthesis of flame retardants, in particular to an all-bio-based flame retardant, a flame-retardant PLA composite material and a preparation method thereof. Background technique [0002] Polylactic acid (PLA), also known as polylactide, can be prepared by ring-opening polymerization of lactide, and can also be produced from carbohydrates extracted from biomass resources such as wheat, corn and cassava through hydrolysis, fermentation and purification. resin. PLA not only has transparency, but also has good biocompatibility, mechanical properties, biodegradability and processing properties, and has full application potential. However, PLA is highly flammable, which greatly limits the use of PLA in applications with high flame retardancy requirements. The practical application in industry, so the flame retardant modification of polylactic acid is very important. [0003] The flame retardant mod...

Claims

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Application Information

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IPC IPC(8): C08K5/521C08K5/42C08K5/39C08L67/04C07F9/117
CPCC08K5/521C08K5/42C08K5/39C07F9/117C08L2201/02C08L2201/06C08L67/04
Inventor 陈思王旭吴飞洋俞陈诚马猛施燕琴何荟文
Owner ZHEJIANG UNIV OF TECH
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