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Preparation method of organic-inorganic hybrid with core-shell structure

A core-shell structure and hybrid technology, which is applied in the field of preparation of core-shell structure organic-inorganic hybrids, can solve the problems of difficult processing and recycling of flame-retardant polymers, damage to mechanical properties and processing properties, and low flame-retardant efficiency. Achieve good synergistic effect, improve mechanical properties and improve compatibility

Inactive Publication Date: 2018-11-30
NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the halogen-based flame retardant system based on gas phase flame retardant has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and has been gradually restricted. or prohibit the use of
Compared with halogenated flame retardants, inorganic flame retardants based on endothermic flame retardants and intumescent flame retardants based on condensed phase flame retardants are environmentally friendly "green" flame retardants recognized by the scientific and industrial circles. agent, but this type of flame retardant often requires a higher addition amount (inorganic type is usually not less than 40wt%, phosphorus-containing type is not less than 20wt%) to make the material achieve the expected flame retardant effect, and the flame retardant efficiency is low. The mechanical properties and processing properties of the material are greatly damaged. At the same time, the thermal stability is poor and the decomposition temperature is low, which causes difficulties in the processing and recycling of flame-retardant polymers.

Method used

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  • Preparation method of organic-inorganic hybrid with core-shell structure
  • Preparation method of organic-inorganic hybrid with core-shell structure
  • Preparation method of organic-inorganic hybrid with core-shell structure

Examples

Experimental program
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Effect test

Embodiment 1

[0042]Add 14.3 g of bisphenolic acid (DPA; 4,4-bis(4-hydroxyphenyl) valeric acid, CAS No. 126-00-1), 20.5 g of dimethylamine aqueous solution (33 wt%), and 20.5 g of formaldehyde in a 250 mL three-necked flask. 16.2g of aqueous solution (37wt%) and 100ml of ethanol were protected by nitrogen, and reacted at 25°C for 20 hours under mechanical stirring. Finally a clear solution was obtained. The solvent was removed by rotary evaporation to obtain a crude product.

[0043] The crude product was dissolved in 300 mL of deionized water to obtain a transparent light yellow solution, 20 g of activated cation exchange resin 732 was added, and stirred for 1 hour. Filtration, the resulting clear night rotary evaporation to remove water. 80C vacuum drying for 8 hours. Monomer (II) is obtained. (That 1 H NMR and 13 C NMR spectrum see attached figure 1 )

[0044] Synthesis of polyphosphate (III): Add 20 g of monomer (II), 5.1 g of triethylamine and 120 mL of acetonitrile into a 250 ...

Embodiment 2

[0052] Add 14.3 g of bisphenolic acid (DPA; 4,4-bis(4-hydroxyphenyl) valeric acid, CAS No. 126-00-1), 20.5 g of dimethylamine aqueous solution (33 wt%), and 20.5 g of formaldehyde in a 250 mL three-necked flask. 16.2g of aqueous solution (37wt%) and 100ml of ethanol were protected by nitrogen, and reacted at 25°C for 20 hours under mechanical stirring. Finally a clear solution was obtained. The solvent was removed by rotary evaporation to obtain a crude product.

[0053] The crude product was dissolved in 300 mL of deionized water to obtain a transparent light yellow solution, 20 g of activated cation exchange resin 732 was added, and stirred for 1 hour. Filtration, the resulting clear night rotary evaporation to remove water. 80C vacuum drying for 8 hours. Monomer (II) is obtained.

[0054] Synthesis of polyphosphate (III): Add 20 g of monomer (II), 5.1 g of triethylamine and 120 mL of acetonitrile into a 250 ml three-necked flask, and flush with nitrogen gas for 10 minut...

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Abstract

The invention relates to a preparation method of an organic and inorganic hybrid with a core-shell structure. The reaction formula of a process line is represented by the following formula (I) in which APP is ammonia polyphosphate, bPEI is branched polymine, and BPE is self-made biomass polyphosphoester electrolyte; an organic and inorganic hybrid flame retardant with 1 to 6 layers is prepared by a layer-by-layer self-assembling method; every two layers are connected via electrostatic or hydrogen bond action. Due to the molecularly structural design, a relative good flame retardant effect can be achieved when the adding amount of the prepared biomass organic and inorganic hybrid in polylactic acid (PLA) is less than 15 weight percent, and the adding amount is far lower than that of the conventional phosphorus based flame retardant. The organic and inorganic hybrid is an efficient and environment-friendly flame retardant: FORMULA.

Description

technical field [0001] The invention relates to a preparation method of an organic-inorganic hybrid with a core-shell structure. Such hybrids can be used as flame retardants in the field of flame retardancy. Background technique [0002] At present, the basic research and application development of flame retardant materials at home and abroad are very active. Although the halogen-based flame retardant system based on gas phase flame retardant has a good flame retardant effect, it releases toxic and corrosive gases during combustion, which poses great hidden dangers to humans and the environment, and has been gradually restricted. or prohibited. Compared with halogenated flame retardants, inorganic flame retardants based on endothermic flame retardants and intumescent flame retardants based on condensed phase flame retardants are environmentally friendly "green" flame retardants recognized by the scientific and industrial circles. agent, but this type of flame retardant of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00C08G79/04C08L87/00C08L67/04C08K9/10C08K3/32
CPCC08G79/04C08G83/001C08K3/32C08K9/10C08K2003/323C08L67/04C08L2201/02C08L87/005
Inventor 井健张艳方征平
Owner NINGBO INST OF TECH ZHEJIANG UNIV ZHEJIANG