Hydrophobic/oleophobic fluorosilicone triblock polymer and preparation method thereof

A polymer and tri-block technology, applied in biocide-containing paints, antifouling/underwater coatings, coatings, etc., can solve high curing temperature, poor substrate adhesion, and poor film-forming properties of silicone resins and other problems, to achieve the effect of mild reaction conditions, low requirements, and mild reaction conditions

Active Publication Date: 2014-12-10
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the film-forming performance of silicone resin is poor, the curing temperature is relatively high, and the adhesion to the substrate is poor

Method used

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  • Hydrophobic/oleophobic fluorosilicone triblock polymer and preparation method thereof
  • Hydrophobic/oleophobic fluorosilicone triblock polymer and preparation method thereof
  • Hydrophobic/oleophobic fluorosilicone triblock polymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of chlorine atom-terminated polydimethylsiloxane chain initiator

[0025] 20.0g (0.01mol) double-terminated hydroxyl-polydimethylsiloxane with an average molecular weight of 2000, 4.42g (0.028mol) α-chloroisobutyl chloride, 4.86g (0.048mol) triethylamine, 100mL Add tetrahydrofuran into a 250mL three-neck flask, under nitrogen protection, stir and react at -10°C for 8 hours, filter after the reaction is completed, distill the filtrate under reduced pressure to remove tetrahydrofuran, dissolve it in dichloroethane, and wash it three times with a saturated aqueous solution of sodium bicarbonate , standing for stratification, after liquid separation, add anhydrous sodium sulfate to the organic phase to dry and remove water, and then filter, and the filtered filtrate is distilled off under reduced pressure to remove dichloroethane to obtain oily yellow chlorine atom-capped polydimethylsiloxane Oxyalkylene chain initiators.

[0026] 2. Preparation of hydrophob...

Embodiment 2

[0031] 1. Preparation of chlorine atom-terminated polydimethylsiloxane chain initiator

[0032] 20.0g (0.01mol) of double-terminated hydroxyl-polydimethylsiloxane with an average molecular weight of 2000, 5.06g (0.032mol) of α-chloroisobutyl chloride, 5.27g (0.052mol) of triethylamine, 100mL Tetrahydrofuran was added into a 250 mL three-necked flask, and stirred and reacted at -10° C. for 10 hours under nitrogen protection. Other steps in this step were the same as in Example 1 to obtain an oily yellow polydimethylsiloxane chain initiator terminated by chlorine atoms.

[0033] 2. Preparation of hydrophobic / oleophobic fluorosilicone triblock polymer

[0034] 2.24g (0.001mol) of chlorine atom-terminated polydimethylsiloxane chain initiator prepared in step 1, 12.5g (0.05mol) hexafluorobutyl methacrylate, 0.0099g (0.001mol) cuprous chloride , 0.094g (0.0006mol) 2,2'-bipyridine, 0.089g (0.0006mol) N-(2-pyridylmethylene)-1-propylamine, 100mL toluene were added to a 250mL three-nec...

Embodiment 3

[0038] 1. Preparation of chlorine atom-terminated polydimethylsiloxane chain initiator

[0039] 30.0g (0.01mol) of double-terminated hydroxyl-polydimethylsiloxane with an average molecular weight of 3000, 4.42g (0.028mol) of α-chloroisobutyl chloride, 4.86g (0.048mol) of triethylamine, 100mL Tetrahydrofuran was added into a 250 mL three-necked flask, and stirred and reacted at 10° C. for 10 hours under nitrogen protection. Other steps in this step were the same as in Example 1 to obtain an oily yellow polydimethylsiloxane chain initiator terminated by chlorine atoms.

[0040] 2. Preparation of hydrophobic / oleophobic fluorosilicone triblock polymer

[0041]With 3.24g (0.001mol) the polydimethylsiloxane chain initiator that the chlorine atom termination of step 1 prepares, 15.0g (0.06mol) hexafluorobutyl methacrylate, 0.0099g (0.001mol) cuprous chloride , 0.139g (0.0012mol) tetramethylethylenediamine, and 100mL toluene were added to a 250mL three-necked flask, and under nitroge...

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Abstract

The invention discloses a hydrophobic/oleophobic fluorosilicone triblock polymer and a preparation method thereof. The structural formula of the polymer is as shown in the specification, in the structural formula, m is an integer from 10 to 50, n is an integer from 20 to 50, and a target polymer, namely, hexafluorobutyl methacrylate-b-polydimethylsiloxane-b-polyhexafluorobutyl methacrylate is synthesized by taking chloro-polydimethylsiloxane as a chain initiator under the co-catalysis of a catalyst CuCl and catalyst ligands 2,2'-dipyridyl and N-(2-pyridine methylene)-1-propylamine or tetramethylethylenediamine by using an atom transfer radical polymerization method. According to the hydrophobic/oleophobic fluorosilicone triblock polymer, microwave radiation heating is adopted, the operation is simple and convenient, the reaction condition is gentle, the molecular weight and the distribution of a reaction product can be controlled, and the synthesized hydrophobic/oleophobic fluorosilicone triblock polymer is excellent in hydrophobic and oleophobic property and is wide in application prospect in anti-flouring coating.

Description

technical field [0001] The invention relates to a hydrophobic / oleophobic fluorosilicon tri-block polymer, and relates to an atom transfer radical polymerization method, using chlorinated polydimethylsiloxane as a chain initiator, and heating by microwave radiation. The target polymer polyhexafluorobutylmethacrylate-b-poly Dimethicone-b-polyhexafluorobutylmethacrylate method. Background technique [0002] The carbon-fluorine bond of the organic fluorine material has a large bond energy and is relatively stable. The fluorine atoms are not only firmly bonded to the carbon atoms, but also arranged very tightly on the outer layer of the carbon skeleton, effectively preventing the exposure of the carbon atoms and carbon chains, showing excellent Chemical stability, weather resistance, corrosion resistance, oxidation resistance and other properties. Silicone materials have the properties of both inorganic and organic substances, and have excellent high and low temperature resista...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08F220/22C08F2/46C09D153/00C09D5/16
Inventor 成西涛黄方方张存社王前进白燕周魁
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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