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Preparation method of branched poly (p-hydroxystyrene)

A technology of hydroxystyrene and acetoxystyrene is applied in the field of preparation of branched poly(p-hydroxystyrene) to achieve the effects of simple preparation operation, controllable structure and performance, and mild polymerization conditions

Inactive Publication Date: 2014-04-30
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the poly(p-hydroxystyrene) used in 248nm photoresist is mostly linear, and the application of branched poly(p-hydroxystyrene) in 248nm photoresist is rarely reported

Method used

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  • Preparation method of branched poly (p-hydroxystyrene)
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  • Preparation method of branched poly (p-hydroxystyrene)

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Synthesis of branched poly(p-acetoxystyrene): add (22mmol) 3.58g p-acetoxystyrene, ( (0.44mmol) 0.08g p-vinylbenzylmercaptan, (0.44mol) 0.072g AIBN, and then add 40ml of tetrahydrofuran as a polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 40°C, and then seal it with nitrogen gas for 10 minutes system, the temperature was raised to 65°C, the reaction was stirred at constant temperature for 24 hours, and then cooled to room temperature. Add the obtained polymer solution dropwise to methanol for sedimentation and suction filtration. After suction filtration, the obtained solid is repeatedly dissolved, precipitated and purified, and the obtained solid is vacuum-dried to obtain a branched poly(p-acetoxystyrene) product.

[0026] (2) Deacetoxylation of branched poly(p-acetoxystyrene): add 1.5g branched poly(p-acetoxystyrene) and 35ml methanol to a 100ml three-necked flask, 7.45g of ammonia water (containing 3g of ammonium hydr...

Embodiment 2

[0028] (1) Synthesis of branched poly(p-acetoxystyrene): add (22mmol) 3.58g p-acetoxystyrene, ( (0.88mmol) 0.16g p-vinylbenzylmercaptan, (0.44mol) 0.072g AIBN, and then add 40ml of tetrahydrofuran as a polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 40°C, and then seal it after nitrogen gas for 10min system, the temperature was raised to 65°C, the reaction was stirred at constant temperature for 24 hours, and then cooled to room temperature. Add the obtained polymer solution dropwise to methanol for sedimentation and suction filtration. After suction filtration, the obtained solid is repeatedly dissolved, precipitated and purified, and the obtained solid is vacuum-dried to obtain a branched poly(p-acetoxystyrene) product.

[0029] (2) Deacetoxylation of branched poly(p-acetoxystyrene): add 1.5g branched poly(p-acetoxystyrene) and 35ml methanol to a 100ml three-necked flask, 7.45g of ammonia water (containing 3g of ammonium hydroxid...

Embodiment 3

[0031] (1) Synthesis of branched poly(p-acetoxystyrene): add (22mmol) 3.58g p-acetoxystyrene, ( (1.32mmol) 0.24g p-vinylbenzylmercaptan, (0.44mol) 0.072g AIBN, and then add 40ml tetrahydrofuran as a polymerization solvent, place the flask in a constant temperature oil bath, heat and stir to 40°C, and then seal it with nitrogen gas for 10 minutes system, the temperature was raised to 65°C, the reaction was stirred at constant temperature for 24 hours, and then cooled to room temperature. Add the obtained polymer solution dropwise to methanol for sedimentation and suction filtration. After suction filtration, the obtained solid is repeatedly dissolved, precipitated and purified, and the obtained solid is vacuum-dried to obtain a branched poly(p-acetoxystyrene) product.

[0032] (2) Deacetoxylation of branched poly(p-acetoxystyrene): add 1.5g branched poly(p-acetoxystyrene) and 35ml methanol to a 100ml three-necked flask, 7.45g of ammonia water (containing 3g of ammonium hydroxi...

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Abstract

The invention discloses a preparation method of branched poly (p-hydroxystyrene). The preparation method comprises the steps: firstly, through simple free radical polymerization, with ethenylphenol acetate as a polymerization unit and vinyl benzyl mercaptane as a chain transfer monomer, preparing branched poly(p-ethenylphenol acetate) in a tetrahydrofuran solution, and then performing deacetoxylation on the branched poly(p-ethenylphenol acetate) to prepare the branched poly (p-hydroxystyrene). The polymerization process is easy to control and is capable of controlling the molecular weight of a polymer through adjusting the reaction time and the content of the chain transfer monomer.

Description

technical field [0001] The invention relates to a preparation method of branched poly-p-hydroxystyrene, which belongs to the field of polymer materials. Background technique [0002] Poly(p-hydroxystyrene) is widely used in homogeneous synthesis, phase transfer catalysis and HPLC homophasing, epoxy resin assimilation agent, organic waste liquid adsorbent, selective permeable membrane, free radical scavenger and antioxidant, etc. Polyp-hydroxystyrene is optically transparent at 248nm, and has good alkali solubility and excellent dry corrosion resistance, making it the first choice for 248nm photoresist film-forming resin. [0003] Compared with traditional linear polymers, branched polymers have low viscosity, high density, good solubility and film-forming properties. [0004] At present, the poly(p-hydroxystyrene) used in 248nm photoresist is mostly linear, and the application of branched poly(p-hydroxystyrene) in 248nm photoresist is rarely reported. Contents of the inv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/14C08F228/02C08F8/00
Inventor 刘晓亚林立成刘敬成李虎刘仁
Owner JIANGNAN UNIV
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