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Preparation method of linear or body fluorine modified organosilicon material

A fluorine-modified silicone and linear technology, which is applied in the field of preparation of linear and body-shaped fluorine-modified silicone materials, can solve the problem of difficulty in obtaining high-molecular-weight fluorine-modified silicone materials, negative high temperature stability, Low molecular weight and other problems, to achieve the effect of strong application and industrialization prospects, good solvent resistance, and simple preparation steps

Active Publication Date: 2014-02-05
SKSHU PAINT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molecular weight of the fluorine-modified silicone prepared by these two methods is generally low, usually only 20K-60K, it is difficult to obtain a high molecular weight fluorine-modified silicone material (A.A.Thorpe, V.Peters, J.R.Smith, et al. J.J.Fluorine Chem.2000,104,37-45;H.Suzuki,M.Takeishi,I.Narisawa.J.Appl.Polym.Sci.2000,78,1955-1963;H.Murase,K.Nanishi,H. Kogure, et al. J. Appl. Polym. Sci. 1994, 54, 2051-2062.)
In addition, these two methods need to be realized with the help of specific catalysts. The former generally uses platinum and other noble metals as catalysts, which are relatively expensive; The application performance of the product, especially the high temperature stability is negatively affected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Octamethylcyclotetrasiloxane (D 4 ) and tetramethylammonium hydroxide pentahydrate (TMAH), mixed and stirred evenly, wherein the mass fraction of TMAH is 2wt.%. The resulting mixture was warmed to 70°C, and N 2 And keep vacuuming to remove the water in the system, react for 30 minutes to get tetramethylammonium hydroxide silicon alkoxide.

[0021] Trifluoropropylmethylcyclotrisiloxane (D 3 F) and octamethylcyclotetrasiloxane (D 4 ) into a 250ml four-neck flask, the molar ratio of the two is 1.0:1. Nitrogen is blown, and a certain amount of tetramethylammonium hydroxide silicon alkoxide is added under stirring, and the tetramethyl ammonium hydroxide silicon alkoxide accounts for 0.2wt.% of the total mass. The mixture was heated to 110°C for 2h. Finally, the temperature of the system was raised to 150° C. for 30 minutes, and tetramethylammonium hydroxide silicon alkoxide in the system was removed to obtain a linear fluorine-modified organosilicon material.

[0022] ...

Embodiment 2

[0025] Decamethylcyclopentasiloxane (D 5 ) and tetrabutylphosphorus hydroxide solution (TBPH), mixed and stirred evenly, wherein the mass fraction of TBPH is 2wt.%. The resulting mixture was warmed to 90°C, and the 2 And keep vacuuming to remove the water in the system, after 30 minutes of reaction, tetrabutylphosphosilicate hydroxide can be obtained.

[0026] Trifluoropropylmethylcyclotrisiloxane (D 3 F) and decamethylcyclopentasiloxane (D 5 ) into the four-neck flask, the molar ratio of the two is 1.0:1. Under the protection of nitrogen gas, a certain amount of tetrabutyl phosphorus hydroxide silicon alkoxide is added under the premise of medium-speed stirring, and the silicon alkoxide catalyst accounts for 0.2wt.% of the total mass. The mixture was heated to 110°C for 2 hours to obtain a high viscosity copolymer. Finally, the temperature of the system was raised to 150° C. for 30 minutes to decompose the tetrabutylphosphorus silicon alkoxide in the system to obtain a l...

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Abstract

The invention discloses linear or body fluorine modified polysiloxane and a preparation method thereof. The preparation method disclosed by the invention mainly comprises the following steps of: by taking quaternary ammonium base (such as tetramethylammonium hydroxide (TMAH)) siloxanolate or quaternary phosphorus alkali (such as tetrabutyl phosphorus hydroxide (TBPH)) siloxanolate as the catalyst, taking fluorine-containing cyclosiloxane (such as trifluoropropylmethyl cyclotrisiloxane (D3F)), alkyl cyclosiloxane (such as hexamethyl cyclotrisiloxane (D3), octamethyl cyclotetrasiloxane (D4) or decamethyl cyclopentasiloxane (D5)) or alkyl polycyclosiloxane (bi(heptamethyl cyclotetramethoxy)-ethane(bis-D4)) as the raw material, carrying out ring opening polymerization, and obtaining the linear or body fluorine modified organosilicon material. The preparation method of the linear or body fluorine modified organosilicon material disclosed by the invention is simple in preparation process and low in cost; furthermore, the molecular weight of the prepared product can be adjusted according to requirements; the linear or body fluorine modified organosilicon material has excellent antifouling property, solvent resistance, weather fastness and heat stability and has strong industrialization ability and application prospect.

Description

technical field [0001] The invention relates to a fluorine-modified organic silicon material, in particular to a preparation method of a linear and body-shaped fluorine-modified organic silicon material. Background technique [0002] Due to its unique -Si-O-Si- chain configuration, polyorganosiloxane has excellent thermal stability, high gas permeability, chemical inertness and other advantages. Until now, polyorganosiloxanes have been widely used in many industrial production fields, such as textiles, cosmetics, building waterproofing, pesticides, and coatings. However, the performance of polyorganosiloxane in terms of solvent resistance and oil resistance is not ideal, which greatly limits its practical application. [0003] Fluorine-containing organic compounds have the advantages of extremely low surface energy, unique amphiphobic properties, good weather resistance, excellent water resistance and solvent resistance (S.Krishnan, Y.-J.Kwark, C.K.Ober.Chem.Record2004,4,31...

Claims

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Application Information

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IPC IPC(8): C08G77/24C08G77/08
Inventor 洪杰林金斌林伟
Owner SKSHU PAINT
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