Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of polymethacryloxysilsesquisilane

A polymethacryloyloxy, silsesquioxane technology, applied in the direction of silicon organic compounds, can solve problems such as low efficiency and difficult product purification process, and achieve high reaction efficiency, easy operation, and mild reaction conditions. Effect

Active Publication Date: 2020-11-03
HARBIN INST OF TECH
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing polymethacryloxysilsesquioxane in order to solve the problems of low efficiency and difficult product purification process in the existing polymethacryloxy POSS synthesis method , the method has the advantages of mild reaction conditions, low energy consumption, high synthesis efficiency, high product purity, simple process, etc.

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of preparation method of polymethacryloxysilsesquisilane
  • A kind of preparation method of polymethacryloxysilsesquisilane
  • A kind of preparation method of polymethacryloxysilsesquisilane

Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0018] Specific embodiment one: what this embodiment records is a kind of preparation method of polymethacryloxysilsesquioxane, and described method step is as follows:

[0019] Step 1: Weigh tetraethyl orthosilicate and tetramethylammonium hydroxide according to the molar ratio of 1:1, and then dissolve tetramethylammonium hydroxide in aqueous ethanol to obtain 0.08-0.2g / mL tetramethylammonium hydroxide base ammonium hydroxide solution, and then drop tetraethyl orthosilicate, wherein, the volume ratio of ethanol and water in the ethanol aqueous solution is 8:1;

[0020] Step 2: Under stirring conditions, place the mixed solution obtained in Step 1 at 25°C for 24 hours, then raise the temperature to 60°C for 6 hours, and cool to room temperature naturally after the reaction;

[0021] Step 3: Concentrate the product obtained in Step 2 to the remaining one-third of its volume by rotary evaporation, cool and crystallize at room temperature at 25°C, filter, precipitate with aceton...

Embodiment 1

[0025] The preparation of polymethacryloxysilsesquioxane, proceeds as follows:

[0026] 1. Mix 11.215g of tetramethylammonium hydroxide pentahydrate, 48mL of ethanol, and 6mL of water evenly, and add 13.8mL of tetraethyl orthosilicate dropwise;

[0027] 2. Stir the mixed system for 24 hours at 25°C, then rapidly raise the temperature to 60°C for 6 hours, and cool to room temperature naturally after the reaction;

[0028] 3. The reaction product is concentrated by rotary evaporation to the remaining one-third volume, cooled and crystallized and filtered, the product is precipitated with acetone, and the precipitate is dried at 45°C for 1 hour to obtain octamer tetramethylammonium POSS ammonium salt, and its infrared spectrum Such as figure 1 As shown, it can be clearly seen that the characteristic absorption peak of octapolytetramethylammonium POSS ammonium salt, 3500cm -1 The nearby broad absorption peak belongs to the hydroxyl vibration of water; 2940cm -1 Two nearby peaks...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a preparation method of polymethacryl silsesquioxane, and belongs to the technical field of POSS preparation. The method comprises the following steps: weighing tetraethyl orthosilicate and tetramethylammonium hydroxide and dissolving into an ethanol aqueous solution; putting in 25 DEG C environment and reacting for 24 hours, raising the temperature to 60 DEG C, reacting for 6 hours, and naturally cooling to room temperature after the reaction is ended; carrying out rotary evaporation and concentration on a product, cooling, crystallizing filtering, precipitating and drying to obtain octapolytetramethyl-ammonium POSS ammonium salt; weighing dimethyl sulfoxide and N-hexane as solvents and mixing; then weighing the octapolytetramethyl-ammonium POSS ammonium salt and methacryloyl chloride, mixing the solvents with the ammonium salt and the methacryloyl chloride; under a stirring condition, reacting at room temperature for 1 to 2 hours, separating liquid and carrying out suction filtration on an N-hexane phase, thus obtaining the polymethacryl silsesquioxane. The preparation method disclosed by the invention has the advantages of short synthesis reaction time, high reaction efficiency, easiness in operation and mild reaction conditions.

Description

technical field [0001] The invention belongs to the technical field of POSS preparation, and in particular relates to a preparation method of polymethacryloxysilsesquioxane. Background technique [0002] Multifaceted oligomeric silsesquioxane (POSS for short) is a compound with a nanoscale cage structure, also known as cubic silane, with the general molecular formula (RSiO 1.5 ) n , the basic structural unit is -Si-O-, the scale of the entire molecule is between 1 and 3nm, and it is the smallest silicon particle. Its molecule has a silicon-oxygen skeleton as the core, and the eight Si vertices are connected with organic substituent groups. The inorganic silicon-oxygen skeleton can endow the material with good heat resistance and mechanical properties, and the peripheral organic groups are designed as reactive groups such as olefin groups. , silanol group, acryloyloxy group, etc., through reactive groups, POSS and organic polymers can undergo surface bonding, grafting, copo...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 黄玉东王昱璎刘丽贺金梅张润泽吴帆
Owner HARBIN INST OF TECH