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Fluoride POSS acrylic ester block multipolymer resin and its synthesis

A technology of block copolymer and acrylate, applied in the field of acrylate copolymer resin and its synthesis, can solve the problems of increased water absorption on the surface of the coating, environmental pollution, and high cost, and achieves improved production efficiency, improved hydrophobicity, and improved The effect of utilization efficiency

Inactive Publication Date: 2007-09-05
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods mainly have the following disadvantages: 1. Fluorine-containing acrylate monomers are generally insoluble in commonly used organic solvents, and need to use some solvents that are expensive and pollute the environment to carry out solution polymerization; 2. Fluorine-containing acrylate monomers are in use In China, it is often emulsified with an emulsifier and then polymerized to form an emulsion. Although the water solvent does not pollute the environment when the water-based emulsion is used, the water absorption of the coating surface is increased due to the presence of the emulsifier; 3. Fluorine-containing acrylate emulsion In order to improve the utilization rate of monomers and reduce the surface energy of coatings during preparation, fluorine-containing surfactants are often used, so the cost is high and there is environmental pollution; 4. The hardness of fluorine-containing acrylate coatings is not very ideal.

Method used

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  • Fluoride POSS acrylic ester block multipolymer resin and its synthesis
  • Fluoride POSS acrylic ester block multipolymer resin and its synthesis
  • Fluoride POSS acrylic ester block multipolymer resin and its synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1. Put the weighed 0.144g of CuBr and 0.346g of PMDETA into a two-neck bottle, seal it, vacuumize it, and blow nitrogen gas. This replacement process is carried out 3 times.

[0033]Step 2. Dissolve 0.195g of initiator EBriB in 100g of monomer MMA, introduce nitrogen gas under the liquid surface of the monomer to bubble and deoxygenate, add it to the two-necked bottle together after 1 minute, vacuumize and ventilate nitrogen, and the replacement process is carried out 3 times. The ratio of the amount of substances in the system is EbriB:CuBr:PMDETA:MMA=1:1:2:1000. Then put the two-necked bottle in a silicone oil bath at 85°C and react for 24 hours.

[0034] Step 3, dilute the reacted solution with 100g of tetrahydrofuran, remove excess catalyst and initiator by alumina adsorption, then precipitate with methanol, filter, and vacuum dry at room temperature to constant weight to obtain pre Polymer;

[0035] Step 4, take another two-necked bottle, add 10g tetrahydro...

Embodiment 2

[0040] Step 1. Put the weighed 0.288g of CuBr and 0.692g of PMDETA into a two-neck bottle, seal it, vacuumize it, and ventilate it with nitrogen. The replacement process is carried out 3 times.

[0041] Step 2. Dissolve 0.195g of initiator EbriB in 100g of monomer MMA, introduce nitrogen gas under the liquid surface of the monomer to bubble and deoxygenate, add it to the two-necked bottle together after 1 minute, vacuumize and ventilate nitrogen, and the replacement process is carried out 3 times. The ratio of the amount of substances in the system is EbriB:CuBr:PMDETA:MMA=1:2:6:1500. Then put the two-necked bottle in a silicone oil bath at 80°C and react for 20 hours.

[0042] Step 3, dilute the reacted solution with 100g of tetrahydrofuran, remove excess catalyst and initiator by alumina adsorption, then precipitate with methanol, filter, vacuum dry at room temperature to constant weight, and obtain methyl methacrylate with Br-terminated Ester prepolymer;

[0043] Step 4,...

Embodiment 3

[0048] Step 1. Weigh 0.288g of CuBr and 0.692g of PMDETA, put them into a two-necked bottle, put them into a two-necked bottle, seal it, vacuumize it, and ventilate nitrogen. The replacement process is carried out 3 times.

[0049] Step 2. Dissolve 0.195g of initiator EbriB in 100g of monomer MMA, introduce nitrogen gas under the liquid surface of the monomer to bubble and deoxygenate, add it to the two-necked bottle together after 1 minute, vacuumize and ventilate nitrogen, and the replacement process is carried out 3 times. The ratio of the amount of substances in the system is EbriB:CuBr:PMDETA:MMA=1:3:8:1000. Put the two-neck bottle in a microwave oven, set the power to 300W, and react for 4h.

[0050] Step 3, dilute the reacted solution with 100g of tetrahydrofuran, remove excess catalyst and initiator by alumina adsorption, then precipitate with methanol, filter, vacuum dry at room temperature to constant weight, and obtain methyl methacrylate with Br-terminated Ester ...

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PUM

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Abstract

A fluoride POSS acrylic resin block copolymer resin and its synthesis are disclosed. The molecular-weight of copolymer Mn is 20000-60000, Mn / Mw is 1.1-1.5, contact angle between coating and water is 85-120degree. The process is carried out by adding components into reactor to obtain methyl acrylate performed polymer with Br end capping, reacting with CuBr, PMDETA and F-POSS, removing catalyst from reactant, depositing while filtering by methanol, vacuum drying to constant weight to obtain the final product. The polymer powders can be dissolved into acetic ether, acetone, 1,2-dichloroethane, dioxane and cyclohexanone or their mixtures, then it can be used for coating or filming.

Description

technical field [0001] The invention relates to an acrylate copolymer resin and a synthesis method thereof, in particular to an organic-inorganic hybrid nano-cluster fluorine-containing polyhedron oligomeric silsesquioxane (POSS) substituted (meth)acrylate block copolymer. Background technique [0002] Fluorine is the most electronegative element in the periodic table, has the strongest electronegativity, the lowest polarizability, and the atomic radius is second only to hydrogen. The bond length of the carbon-fluorine bond is short and the bond energy is large (up to 485kJ / mol , far greater than the bond energy of carbon-carbon bond 422kJ / mol) (Yang Tingting, et al. Polymer Bulletin, 2003, 6: 13-18). Due to the length of the carbon-fluorine bond in the fluoropolymer, the carbon-carbon main chain can be tightly wrapped, and at the same time, when the fluoropolymer is formed into a film, the fluorine-containing groups will spontaneously enrich the surface layer, making the fl...

Claims

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Application Information

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IPC IPC(8): C08G81/02
Inventor 戴李宗陈江枫许一婷邓远名彭小亮
Owner XIAMEN UNIV
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