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POSS (polysilsesquioxane)-containing polymerizable surfactant and preparation method thereof

A surfactant and polymerization technology, applied in the field of polymerizable surfactants and its preparation, can solve the problems of latex instability, lower water resistance of products, etc., and achieve remarkable results in water pollution problems

Inactive Publication Date: 2013-05-01
泉州鲁新新型建材有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But at the same time, the surfactants in the prior art also have disadvantages, that is, they are not bonded with a strong covalent bond but are only adsorbed on the polymer material in a physical adsorption mode.
In some occasions (such as freeze-thaw cycles, high shear force, etc.), these surfactants are easy to desorb from the surface of latex particles, making the latex unstable, and the surfactants are easy to migrate in the film. Form aggregates and reduce the water resistance of the product

Method used

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  • POSS (polysilsesquioxane)-containing polymerizable surfactant and preparation method thereof
  • POSS (polysilsesquioxane)-containing polymerizable surfactant and preparation method thereof
  • POSS (polysilsesquioxane)-containing polymerizable surfactant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) 10g of aminopropyl isobutyl POSS (its nuclear magnetic resonance spectrum is shown in figure 1 As shown in the spectral line a), 0.96g maleic anhydride (MA) and 0.028g p-diphenol were dissolved in 40mL of benzene, nitrogen was passed through to remove oxygen, and after reacting at 80°C for 12 hours, the benzene ring was evaporated with a rotary evaporator After resembling a solvent, use a volume ratio of 1:1 petroleum ether / diethyl ether mixed solution to extract and then separate and precipitate with a centrifuge to obtain POSS-MA (its nuclear magnetic resonance spectrum is as follows: figure 1 The spectral line b is shown).

[0028] (2) Dissolve 3g POSS-MA, 4.10g polyethylene glycol (PEG-2000), 0.015g p-toluenesulfonic acid and 0.0255g hydroquinone in 40mL benzene, blow nitrogen to remove oxygen, and react at 125°C After 24 hours, use a rotary evaporator to remove the benzene ring solvent, use a mixed solution of petroleum ether / diethyl ether with a volume ratio ...

Embodiment 2

[0035] (1) Dissolve 10.0g of aminopropyl isobutyl POSS, 0.96g of maleic anhydride and 0.1~1% of the total mass of aminopropyl isobutyl POSS and maleic anhydride in 40mL of benzene, and pass Deoxygenate with nitrogen, react at 90°C for 24 hours, evaporate the benzene ring solvent with a rotary evaporator, extract with a mixed solution of petroleum ether / ether with a volume ratio of 1:1, and then separate and precipitate with a centrifuge to obtain POSS-MA.

[0036] (2) Add 3g POSS-MA, 3.91g polyethylene glycol (PEG-400), 0.1~1% p-diphenol, 0.021g p-toluenesulfonate to the total mass of aminopropyl isobutyl POSS and maleic anhydride Dissolve the acid in 40mL of benzene, pass nitrogen gas to remove oxygen, react at 140°C for 24 hours, use a rotary evaporator to remove the benzene ring solvent, use a mixed solution of petroleum ether / diethyl ether with a volume ratio of 1:1 to extract and then Separate the precipitate with a centrifuge to obtain POSS-MA-PEG600 with a yield of 94%...

Embodiment 3

[0039] (1) Dissolve 8.0g of aminopropyl isobutyl POSS, 0.82g of maleic anhydride and 0.1~1% of the total mass of aminopropyl isobutyl POSS and maleic anhydride in 40mL of benzene, and pass Deoxygenate with nitrogen, react at 100°C for 15 hours, evaporate the benzene ring solvent with a rotary evaporator, extract with a mixed solution of petroleum ether / ether with a volume ratio of 1:1, and then separate and precipitate with a centrifuge to obtain POSS-MA.

[0040](2) Add 3g POSS-MA, 3.36g polyethylene glycol (PEG-600), 0.1~1% p-diphenol, 0.024g p-toluenesulfonate to the total mass of aminopropyl isobutyl POSS and maleic anhydride Dissolve the acid in 40mL of benzene, pass nitrogen gas to remove oxygen, react at 130°C for 18 hours, evaporate the benzene ring solvent with a rotary evaporator, use a mixed solution of petroleum ether / diethyl ether with a volume ratio of 1:1 to extract and then Separate the precipitate with a centrifuge to obtain POSS-MA-PEG600 with a yield of 93%...

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Abstract

The invention discloses a POSS (polysilsesquioxane)-containing polymerizable surfactant and a preparation method thereof. The POSS-containing polymerizable surfactant takes POSS as a hydrophobic terminal, a polyethylene glycol molecule as a hydrophilic chain terminal and maleate as a double-bond intermediate chain, so that desorption of the POSS-containing polymerizable surfactant and migration thereof in a film can be effectively avoided, and the POSS-containing polymerizable surfactant has a very significant application value in improving the rheological property and the stability of an emulsion and the glossiness and the water resistance of a coating film, solving a water pollution problem caused by the residual surfactant in gel preparation of a solid product and the like. The preparation method of the POSS-containing polymerizable surfactant comprises one-step amidation and one-step esterification based on maleic anhydride, and is simple in process, mild in reaction condition and high in yield.

Description

technical field [0001] The invention belongs to surfactants, in particular to a POSS-containing polymerizable surfactant and a preparation method thereof. Background technique [0002] In emulsion polymerization, surfactants play a very critical role for the nucleation of latex particles, the emulsification of monomer droplets or prepolymers, the stability of polymer particles during polymerization and the stability of products during storage are very important. But at the same time, the surfactants in the prior art also have disadvantages, that is, they are not bound by strong covalent bonds, but only adsorbed on polymer materials by physical adsorption. In some occasions (such as freeze-thaw cycles, high shear force, etc.), these surfactants are easy to desorb from the surface of latex particles, making the latex unstable, and the surfactants are easy to migrate in the film, Form aggregates and reduce the water resistance of the product. Contents of the invention [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01F17/54B01F17/42C08G81/00C08F2/24C09D7/12C09K23/54C09K23/42
Inventor 张瑞表庄碧双张心媚
Owner 泉州鲁新新型建材有限公司
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