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Silicon nitrogen containing flame retardant type polymer dye and preparation method thereof

A polymer and flame-retardant technology, applied in the field of silicon-nitrogen-containing flame-retardant polymer dyes and their preparation, can solve the problem of high requirements for synthesis equipment, high temperature and high pressure reaction, and difficulty in controlling the content of azobenzene flame retardant groups, etc. problems, to reduce migration, improve flame retardancy and anti-droplet properties, and achieve the effect of good adhesion

Active Publication Date: 2016-06-15
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is to introduce azobenzene groups through esterification to produce high-temperature self-crosslinking expansion, flame retardancy and anti-droplet performance, which requires high temperature and high pressure reactions, high requirements for synthesis equipment, and it is difficult to control the azobenzene resistance in the molecular structure. Combustion group content

Method used

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  • Silicon nitrogen containing flame retardant type polymer dye and preparation method thereof
  • Silicon nitrogen containing flame retardant type polymer dye and preparation method thereof
  • Silicon nitrogen containing flame retardant type polymer dye and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1) PPOSSMA m Synthesis of Macromolecular Chain Transfer Agents

[0022] Methacryloxypropyl heptaisobutyl polyhedral oligomeric silsesquioxane POSSMA (5.2808g), cumyl dithiobenzoate CDB (0.1524g) and azobisisobutyronitrile AIBN (0.0274g ) was dissolved in 8.0ml tetrahydrofuran, after continuous freeze-thaw degassing for 5 times, the RAFT polymerization reaction was carried out under the protection of argon, and then the reaction was quenched by liquid nitrogen, and methanol: ethyl acetate was 8: 1 as the precipitant repeatedly. Precipitate 3 times to get the product PPOSSMA m Macromolecular chain transfer agent;

[0023] 2) PPOSSMA m -b-PAZOMA n Synthesis of diblocks

[0024] Take step 1) synthesized PPOSSMA m Macromolecular chain transfer agent (1.1300g) and 4-{[(2-methacryloyloxy)ethyl]ethylamino} azobenzene AZOMA (1.0122g) and azobisisobutyronitrile (0.0050g) Dissolve in 3.0ml tetrahydrofuran, conduct RAFT polymerization reaction under the protection of argon a...

Embodiment 2

[0028] 1) PPOSSMA m Synthesis of Macromolecular Chain Transfer Agents

[0029] Methacryloxypropyl heptaisobutyl polyhedral oligomeric silsesquioxane POSSMA (2.8290g), cumyl dithiobenzoate CDB (0.0454g) and azobisisobutyronitrile AIBN (0.0082g ) was dissolved in 5.0ml tetrahydrofuran, after continuous freeze-thaw degassing for 5 times, RAFT polymerization was carried out under the protection of argon, and then quenched with liquid nitrogen to stop the reaction, and methanol:ethyl acetate was 7:1 as the precipitating agent repeatedly Precipitate 3 times to get the product PPOSSMA m Macromolecular chain transfer agent;

[0030] 2) PPOSSMA m -b-PAZOMA n Synthesis of diblocks

[0031] Take step 1) synthesized PPOSSMA m Macromolecular chain transfer agent (1.6950g) and 4-{[(2-methacryloyloxy)ethyl]ethylamino} azobenzene AZOMA (1.0122g) and azobisisobutyronitrile (0.0050g) Dissolve in 3.0ml tetrahydrofuran, conduct RAFT polymerization reaction under the protection of argon aft...

Embodiment 3

[0033] 1) PPOSSMA m Synthesis of Macromolecular Chain Transfer Agents

[0034] Methacryloxypropyl heptaisobutyl polyhedral oligomeric silsesquioxane POSSMA (2.6404g), cumyl dithiobenzoate CDB (0.0762g) and azobisisobutyronitrile AIBN (0.0137g ) was dissolved in 5.0ml tetrahydrofuran, and after continuous freeze-thaw degassing for 5 times, RAFT polymerization was carried out under the protection of argon, and then quenched with liquid nitrogen to stop the reaction, and methanol:ethyl acetate was 8:1 as the precipitant repeatedly. Precipitate 3 times to get the product PPOSSMA m Macromolecular chain transfer agent;

[0035] 2) PPOSSMA m -b-PAZOMA n Synthesis of diblocks

[0036] Take step 1) synthesized PPOSSMA m Macromolecular chain transfer agent (1.3560g) and 4-{[(2-methacryloyloxy)ethyl]ethylamino} azobenzene AZOMA (1.2164g) and azobisisobutyronitrile (0.0059g) Dissolve in 3.5ml tetrahydrofuran, conduct RAFT polymerization reaction under the protection of argon after ...

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Abstract

Relating to a block copolymer dye, the invention provides a silicon nitrogen containing flame retardant type polymer dye and a preparation method thereof. Polymethacryloxypropyl polyhedron oligomeric silsesquioxane is adopted as a first block, and polymethacrylate azobenzene is taken as a second blocker to prepare a halogen-free flame retardant block copolymer dye by means of reversible addition-fragmentation chain transfer. The self-assembly effect of a POSS group in the dye molecule can significantly improve the dye molecule fastness and reduce dye molecule migration, and through introduction of an azo group (-N=N-) and the POSS group, the material can be endowed with good flame-retardant and anti-dripping performance. By adjusting the feeding proportion of the two monomers, the content of silicon and nitrogen flame retardant elements in the polymer dye molecules can be controlled, and the method has the advantages of simple synthesis process, mild reaction conditions, easy control of reaction, and is suitable for mass production.

Description

technical field [0001] The invention relates to a block copolymer dye, in particular to a silicon-nitrogen-containing flame-retardant polymer dye with flame-retardant and droplet-resistant properties and a preparation method thereof. Background technique [0002] Azo dyes refer to dyes that contain an azo group (—N=N—) in their molecular structure and have at least one aromatic structure in their linking part. This type of dye has a complete color spectrum and good shade, and is widely used in dyeing and printing of textiles and leather products. Currently, about 60% of the synthetic dyes in the world market are based on azo chemistry. Although small molecule azo dyes are widely used, they also have disadvantages such as poor adhesion, washability and stability. Long-term contact with products containing small molecule azo dyes, especially when the color fastness is not good, small molecule azo dyes Dyes are prone to migration and mix with substances released during normal...

Claims

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Application Information

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IPC IPC(8): C09B69/10C08F293/00
CPCC08F293/00C09B69/106
Inventor 许一婷李奇戴李宗陈显明王美杰侯培鑫
Owner XIAMEN UNIV
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