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A kind of bio-based phosphorus-containing starch and its preparation method and application

A bio-based, starch technology, applied in the field of modified starch, can solve the problems of poor compatibility between starch and matrix plastics, poor thermal stability of starch, and inability to meet application requirements, and achieves the ability to promote carbon formation, high phosphorus content, high yield effect

Active Publication Date: 2019-04-02
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many reports on the application of natural starch in plastics such as polylactic acid and polypropylene, but there are obvious defects: first, the thermal stability of starch is not good, it is easy to degrade during processing, and yellowing occurs, resulting in unsightly products. Beautiful; Secondly, the compatibility between starch and base plastic is very poor, which limits the filling amount of starch, and the mechanical properties of the material are very poor, which cannot meet the requirements of practical applications

Method used

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  • A kind of bio-based phosphorus-containing starch and its preparation method and application
  • A kind of bio-based phosphorus-containing starch and its preparation method and application
  • A kind of bio-based phosphorus-containing starch and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] In a 250mL three-necked flask, 20g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and 15g of maleic anhydride (MA) were dissolved in 50mL of toluene and 20mL of dioxygen Hexacyclic, heated to 40 ° C, nitrogen protection, reflux reaction for 12 hours. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0061] In a 250mL three-necked flask, 20g of starch (corn starch) and 40mL of pyridine were heated to 65°C and refluxed for 2h under nitrogen protection. After the temperature dropped to 50°C, 20g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed at 50°C for 12h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

Embodiment 2

[0063] In a 250mL three-necked flask, 20g DOPO and 18g maleic anhydride (MA) were respectively dissolved in 50mL xylene and 20mL THF (tetrahydrofuran), heated to 50°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0064] In a 250mL three-necked flask, 20g of starch (corn starch) and 60mL of pyridine were heated to 75°C and refluxed for 4h under nitrogen protection. After the temperature dropped to 50°C, 25g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

Embodiment 3

[0066] In a 250mL three-necked flask, 20g DOPO and 21g maleic anhydride (MA) were dissolved in 70mL xylene, heated to 60°C, under nitrogen protection, and refluxed for 24h. After the reaction, the solvent was removed by rotary evaporation, and the product 1 was obtained after vacuum drying, which was set aside.

[0067] In a 250mL three-necked flask, 20g of starch (corn starch) and 80mL of pyridine were heated to 85°C and refluxed for 8h under nitrogen protection. After the temperature dropped to 65°C, 35g of the product 1 (dissolved in DMSO) was added to the catalyst 4-dimethylaminopyridine, protected by nitrogen, and refluxed for 24h. After the reaction is finished, it is washed, purified, and vacuum-dried to obtain bio-based phosphorus-containing starch, ie, modified starch.

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Abstract

The invention discloses bio-based phosphoric starch and a preparation method and application thereof. The preparation method comprises the steps that 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, maleic anhydride and a first organic solvent are mixed, reflux reaction is performed at the temperature of 40-100 DEG C and under protective gas for 12-36 hours, reduced pressure distillation and drying are performed to obtain a product 1; starch, a catalyst and a second organic solvent are mixed, heating activation is performed at the temperature of 60-120 DEG C and under protective gas for 2-24 hours to obtain an activated starch solution; the product 1 is added to the cooled activated starch solution, reaction continues at the temperature of 30-90 DEG C and under protective gas for 12-64 hours, and washing and drying are performed to obtain the bio-based phosphoric starch. The bio-based phosphoric starch has high grafting rate and high phosphorus content, both the thermal stability of the obtained bio-based phosphoric starch and the compatibility with a matrix resin interface are significantly improved, and the practical application requirements can be met.

Description

technical field [0001] The invention relates to the technical field of modified starch, in particular to a bio-based phosphorus-containing starch and a preparation method and application thereof. Background technique [0002] With the increasingly severe environmental problems and the oil crisis, people's research on sustainable materials has gradually increased. Bio-based materials, as fully biodegradable green materials, fully meet the current development needs and have received widespread attention. Among them, polylactic acid (PLA), as the bioplastic with the most development potential, has excellent mechanical properties and good processing performance, and is widely used in the automotive industry, electrical facilities and other fields. However, its flammability has greatly limited its promotion in these fields. At present, due to the advantages of low toxicity, environmental protection and smoke suppression, intumescent flame retardant has replaced the traditional h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/04C08L67/04C08L3/06
CPCC08B31/04C08L67/04C08L2201/02C08L2201/08C08L3/06C08K2003/323C08K5/3492
Inventor 孙晋皓汤兆宾朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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