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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 1697032생성일: 2026년 10월 26일

Azobisisobutyronitrile → Propylene glycol methyl ether acetate

https://huagongshe.com/reaction/1697032

반응식

참여 물질

역할이름HCID투입량
반응물AzobisisobutyronitrileHCID 6547—
반응물Methyl Ethyl KetoneHCID 6569—
반응물2-Ethyl-2-methacryloyloxyadamantaneHCID 9813645—
용매MethanolHCID 887—
생성물Propylene glycol methyl ether acetateHCID 7946—

반응 조건

온도80 °C

반응 단계

A monomer solution was prepared by placing 4800 g of methyl ethyl ketone (hereinafter inscribed as “MEK”) in a tank kept at a nitrogen atmosphere, and dissolving 2080 g of 5-acryloyloxy-2,6-norbornanecarbolactone (hereinafter inscribed as “NLA”) as a repeat unit (B) having a polar group for enhancing adhesion to a semiconductor substrate {hereinafter (B) on a head of the compounds in the examples has the same meaning as this} and 2480 g of 2-ethyl-2-adamantyl methacrylate (hereinafter inscribed as “EAM”) as a repeat unit (A) which is decomposed by an acid to become alkali soluble (hereinafter (A) on a head in the compounds in the examples has the same meaning as this). A polymerization initiator was prepared by placing 700 g of MEK and 80 g of azobisisobutyronitrile (hereinafter inscribed as “AIBN”) in another container kept at a nitrogen atmosphere and dissolving. Into a polymerization tank kept at the nitrogen atmosphere, 3500 g of MEK was put and the temperature was raised to 80° C. with stirring. Subsequently, the monomer solution and the polymerization initiator solution kept at the temperature of 25 to 30° C. were fed into the polymerization tank kept at 80° C. over 4 hours, respectively. After the completion of feed, the polymerized solution was matured for 2 hours with keeping the polymerization temperature at 80° C., then cooled to room temperature and taken out. Polymer was precipitated from the resulting polymerized solution by dropping in 70 kg of aqueous methanol and filtrated. The resultant wet cake was washed with 70 kg of methanol, filtrated subsequently dissolved in MEK again, and passed through a filter 40QSH supplied from Cuno Incorporated to remove a trace amount of metals. Then, the solvent was replaced by PGMEA with removing MEK by heating under reduced pressure to prepare PGMEA solution containing 15% polymer. The features of the resultant polymer, the content of high polymer and the evaluation results of storage stability of PGMEA solution are shown in Table 1.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US08163852B2
출처 데이터셋uspto-grants-2012_04
ORD IDord-e2da5e63fc9d49aa8d9047ace4f7d78e
출처 메모uspto-grants-2012_04