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Method for producing ultra-high solid content hydroxy acrylic resin

A hydroxyacrylic acid, ultra-high solid content technology, applied in the direction of coating, can solve the problems of large motion resistance, serious intermolecular entanglement, difficult application and so on

Active Publication Date: 2012-01-25
中山大桥化工集团有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional acrylic resin is a linear polymer obtained by free radical polymerization of vinyl monomers. At a high concentration, the intermolecular entanglement is serious, and it has a large movement resistance, which is manifested as a high flow viscosity, thus giving it a direct application of
In addition, some active functional groups in the molecular structure are covered by long chains, resulting in reduced reactivity due to steric hindrance.
The high solid content hydroxyl acrylic resin currently promoted in the market generally has a solid content of 60%-70%, and mercaptan chain transfer agents are widely used in the synthesis process to reduce the molecular weight of the resin, and the mercaptan odor in the product is difficult to remove

Method used

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  • Method for producing ultra-high solid content hydroxy acrylic resin
  • Method for producing ultra-high solid content hydroxy acrylic resin
  • Method for producing ultra-high solid content hydroxy acrylic resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0088] Preparation of methyl methacrylate (MMA) / butyl methacrylate (BMA) / hydroxyethyl methacrylate (HEMA) macromonomer (Macromonomer-1): MMA 100g / HEMA 130g / BMA 160g with 167g acetic acid Butyl ester, 1.95g AIBN, 78.5mg COPhBF (dihydrate bis(difluoride benzodiketoxime) cobaltate (II) salt) were mixed evenly, then added to the reaction bottle, heated and stirred at 75°C under nitrogen atmosphere, and reacted for 5h . The solid content of the product is 65%, and the conversion rate is 93%. GPC results Mn = 3097, Mw / Mn = 1.75.

[0089] Add 60g of butyl acetate and 1.5g of AIBN into the three-necked flask, wait until the initiator is completely dissolved and heat up to 75°C, then mix 300g of the obtained Macromonomer-1 solution with 31.5g of styrene (St), 31.5g of hydroxyethyl acrylate (HEA), 36.75 g methyl acrylate (MA) and 5.25 g acrylic acid (AA) were mixed evenly and then slowly added dropwise into the flask through a constant pressure dropping funnel for 4 h, and then 15 g o...

Embodiment 2

[0091] Preparation of MMA / BMA / HEMA macromonomer (Macromonomer-2): MMA100g / HEMA 130g / BMA 160g mixed with 167g butyl acetate, 1.95g AIBN, 100mgCOPhBF and added to the reaction flask, heated at 75°C under nitrogen atmosphere Stirring, reaction 5h. The solid content of the product is 62%, and the conversion rate is 89%. GPC results Mn = 1581, Mw / Mn = 1.56.

[0092] Add 60g of butyl acetate and 1.5g of AIBN into the three-neck flask, wait until the initiator is completely dissolved and heat up to 75°C, then mix 300g of the obtained Macromonomer-2 solution with 31.5g St, 31.5g HEA, 36.75g MA, 5.25g AA Slowly drop it into the flask through a constant pressure dropping funnel for 4 hours, add 15 g of butyl acetate and 0.25 g of AIBN after insulated for 1 hour, and incubate for 2 hours. After natural cooling, it was mixed with 3 times the volume of butyl acetate and passed through a 5 cm high silica gel column for decolorization, and then the solvent was distilled off under reduced p...

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Abstract

The invention relates to a preparation method of hydroxy acrylic acid resin with super high fixed content, and belongs to the paint manufacturing industry. The invention adopts methacrylate macromolecule monomer with the end provided with polymerizable double keys and ethylene type monomer copolymerized to get graft structure hydroxy acrylic acid resin. The resin has good performance and small viscosity with fixed content reaching more than 80 percent, thereby saving organic solvent, reducing environment pollution and avoiding bringing sulfur alcohol odor. The invention comprises the following steps: (A) methacrylate type macromolecule monomer is added to copolymerization ethylene type monomer of the synthetic resin, and the use quantity is 1 to 20 percent; (B) the copolymerization ethylene type monomer comprises alkyl methacrylate of 10 to 35 percent, hydroxyethyl methacrylate alkyl easter of 10 to 40 percent, unsaturation carboxylic acid of 1 to 10 percent and other ethane type monomer of 0 to 50 percent; (C) solvent is added in the reaction container, and nitrogen is brought to be heated to back flow temperature, and is mixed with the solvent of 3 times through keeping temperature, adding initiator and solvent, and the finished produce can be finally obtained through decolorizing and vacuum distillation.

Description

【Technical field】: [0001] The invention adopts macromonomer method to prepare graft type ultra-high solid content hydroxy acrylic resin, which is obtained by adding free radical initiator in the presence of solvent, and belongs to the manufacturing industry of organic macromolecular paint. 【Background technique】: [0002] In the paint industry, acrylic resin has many excellent properties (weather resistance, good chemical stability, etc.) and is widely used. The market share of traditional solvent-based acrylic resins is gradually decreasing due to competition from water-based, high-solids, powder, light-curing, and environmentally friendly varieties. The high-solid acrylic resins developed on the basis of traditional solvent-based resins have developed rapidly. Compared with traditional solvent-based coatings, high-solid acrylic resin greatly reduces the content of organic volatiles in the coating system and saves curing energy consumption. At the same time, it has light c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F265/04C09D151/06
Inventor 夏必来曾广鹏凌建雄洪昕林张新宇
Owner 中山大桥化工集团有限公司
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