TW589330B - Process for the preparation of monodisperse polymer particles - Google Patents

Process for the preparation of monodisperse polymer particles Download PDF

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Publication number
TW589330B
TW589330B TW089107457A TW89107457A TW589330B TW 589330 B TW589330 B TW 589330B TW 089107457 A TW089107457 A TW 089107457A TW 89107457 A TW89107457 A TW 89107457A TW 589330 B TW589330 B TW 589330B
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seed particles
aqueous dispersion
particles
organic compound
monomer
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TW089107457A
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English (en)
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Arne Jorgedal
Elin Marie Aksnes
Geir Fonnum
Astrid Evenrod Molteberg
Rolf Nordal
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Dynal Biotech Asa
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/16—Making expandable particles
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00—Processes of polymerisation
    • C08F2/12—Polymerisation in non-solvents
    • C08F2/16—Aqueous medium
    • C08F2/22—Emulsion polymerisation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F257/00—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00
    • C08F257/02—Macromolecular compounds obtained by polymerising monomers on to polymers of aromatic monomers as defined in group C08F12/00 on to polymers of styrene or alkyl-substituted styrenes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
    • C08F265/04—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
    • C08F265/10—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of amides or imides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F291/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds according to more than one of the groups C08F251/00 - C08F289/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/22—After-treatment of expandable particles; Forming foamed products
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/22—After-treatment of expandable particles; Forming foamed products
    • C08J9/224—Surface treatment
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
    • C08J2325/02—Homopolymers or copolymers of hydrocarbons
    • C08J2325/04—Homopolymers or copolymers of styrene
    • C08J2325/06—Polystyrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2347/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Derivatives of such polymers

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Polymerisation Methods In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Paper (AREA)

Description

589330
申清專利範園 聚合引發劑。 項之方法，其中具有 泛乙婦吡咯烷被用作 根據申請專利範圍第1至3項中任 一 Ά 重量平均分予量為1〇至2〇〇〇 kD之聚 該空間安定劑。 •根據申請專利範圍第1至3 J員中任一項之方法，其中聚乙 婦峨錢被用作空間安定劑而該膨脹之晶種顆粒的模式 直徑取多為16 //m。 6·根據申請專利範圍第1至3項中任一項之方法，其中當該 膨脹之晶種顆粒之水性分散液在聚合時之水相更包含水 溶性纖維素醚料空間安定齊卜該_服之晶種顆粒^模 式直徑大於15 //m 〇 7·根據申請專利範圍第丨至3項中任一項之方法，其中羥基 丙基甲基纖維素被用作該空間安定劑。 8.根據中請專利範圍第7項之方法，纟中職基丙基甲基
9·根據申請專利範圍第丨至3項中任一項之方法，其中具有 分子量1 0至100 kD之纖維素醚被用作該空間安定劑。 10. —種多孔性單分散聚合物顆粒之製備方法，該方法包 (1)形成水性分散液，其包含⑴單分散可膨脹晶種 聚合物（或寡聚物）顆粒，（⑴含有分子量在5〇〇〇道爾頓 以下及在25 C下水溶解度為低於1〇-2 g/L之有機化合物 之液滴’（in)陰離子介面活性劑，及視需要而定，（iv) 該有機化合物可溶於其中之有機溶劑；及使該有機化 本紙張尺度適用中國國家標準(cns) A4規格(210x 297公董) 589330
合物擴散於該晶種顆粒中， =將晶種顆粒之水性分散液接觸單體，且使該單體 :晶種顆粒中以形成膨脹之晶種顆粒之水性分 :履’且如需要，則加入水溶性空間安定劑，如需 双則加入普《精（porogen)，及如需要，則加入聚合 引發劑；以及 引發該單體於膨脹之晶種顆粒的水性分散液中之 二奋，其特徵為該膨脹之晶種顆粒包含至少二個普洛 ，’至其中為溶劑供步驟（3)製成之聚合物及至 少其中之一並非溶劑供步驟（3)製成之聚合物。 Π·—種多孔性單分«合物顆粒之製備方法，該方法包 括： (1) 形成水性分散液，其包含單分散可膨脹晶種寡聚 物顆粒與較佳為陰離子介面活性劑； (2) 將晶種顆粒之水性分散液接觸單體，且使該單體 ，散於該晶種顆粒中以形成膨脹之晶種顆粒之水性分 政液，且如需要，則加入水溶性空間安定劑，如需 要’則加入普洛精（P〇r〇gen)，及如需要，則加入聚合 引發劑；以及 (3 )引發該單體於膨脹之晶種顆粒的水性分散液中之 聚合’其特徵為該膨脹之晶種顆粒包含至少二個普洛 精’至少其中之一為溶劑供步驟製成之聚合物及至 少其中之一並非溶劑供步驟（3)製成之聚合物。 12·根據申請專利範圍第丨〇項之方法，其中該有機化合物為 -4- 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公楚) 589330 申清專利範圍
A BCD 月 > ¼
正 ι合引發劑。 13.根據申請專利範圍第1〇至12項中任一項之方法，其中該 普洛精包含甲苯及正庚烷。 14·根據申請專利範圍第1或1〇項之方法，其中： (1) 早分散可膨脹晶種顆粒係藉乳液聚合製備，其中 陰離子介面活性劑在實質上無氧條件下被用作乳化 劑，該可膨脹晶種顆粒具有模式粒徑範圍為0 2至i V m ; (2) 當孩晶種顆粒為非寡聚合（及視需要當其為寡聚 合時）時，⑷將該晶種顆粒接觸含有分子量在5〇〇〇道爾 頓以下及在25°C下水溶解度為低於1〇-2 g/L之有機化合 物之水性分散液、陰離子介面活性劑及視需要該有機 化合物可溶於其中之有機溶劑，及0)使該有機化合物 擴散於該晶種顆粒内； (3) 將晶種顆粒之水性分散液接觸單體，當該有機化 合物存在時，該單體較該有機化合物具至少倍以上 水溶性；如需要水溶性空間安定劑，如需要普洛精 (porogen)，及如需要聚合引發劑，則使該單體擴散於 該晶種顆粒中以形成膨脹之晶種顆粒之水性分散液； 及 (4) 引發該單體於含空間安定劑之水性分散液内於連 續相中之聚合。 15.根據申請專利範圍第丨4項之方法，其中該有機化合物為 聚合引發劑。 本紙張尺度適用中國國家標準(CNS) A4規格(210 X 297公釐）
16·根射請專利範圍第14項之方法，其中在步驟⑴中水 相之氧含量為〇與1 ppm之間。 17·根據申請專利範圍第1至3及1 〇至1 2項中任一項之方 法’其中該單體包含至少3 〇重量％二乙烯苯。 18·根據申請專利範園第j、3、i 〇及丨2項中任一項之方 法’其中該有機化合物為過氧化二辛醯。 19·根據申請專利範圍第i、2、i 〇及丨丨項中任一項之方 法，其特徵另為該單體包括至少二個丙烯酸或甲基丙 酸或酿單體。 ' 20.根據申請專利範圍第19項之方法，其中甲基丙埽酸縮水 甘油酯被用作該單體。 21·根據申請專利範圍第1 4項之方法，其中，當單體為胺其 耳能化之單體（或當使用二或以上個單體而一共聚用單體 為胺基官能化之單體）時，該有機化合物，若存在時，為 非引發劑，而聚合引發劑在該晶種顆粒已膨脹後被加 入0 22·根據申請專利範圍第2或η項之方法，其中該單體為胺 基官能化之單體（或當使用二或以上個單體時，一共聚用 單體為胺基官能化之單體）。 23.根據申請專利範圍第2 2項之方法，其中步驟（2)係使用 聚合引發劑。 24·根據申請專利範圍第21項之方法，其中該非引發劑為二 辛基己二酸酯。 25·根據申請專利範圍第21項之方法，其中該聚合引發劑為 -6- 本紙張尺度適用中國國家標準(CNS) Α4規格(210X 297公釐） 589330
2,2’-偶氮雙_(2_甲基丁腈）。 26·根據申請專利範圍第24項之方法，其中該聚合引發劑為 2，2、偶氮雙- (2 -甲基丁腈）。 27·根據申請專利範圍第22項之方法，其中該聚合引發劑為 2,2’_偶氮雙_(2-甲基丁腈）。 28·根據申請專利範圍第2 3項之方法，其中該聚合引發劑為 2,2、偶氮雙-(2-甲基丁腈）。 29·根據申請專利範圍第i至3及丨〇至丨2項中任一項之方 法’其中該陰離子介面活性劑為硫酸十二烷基鈉。 30·根據申請專利範圍第i至3及丨〇至丨2項中任一項之方 法其中该單分散聚合物顆粒後續被塗佈、浸潰或衍生 化。 31·種清潔由申請專利範圍第1至3及1 〇至1 2項中任_项 足万法所製得之單分散聚合物顆粒之方法，該方法包 括將該單分散聚合物顆粒接觸乙酸丁酯。 ^紙張尺度適用中國國家標準(CNS) A4：規格(210X 297公楚） "-—
TW089107457A 1999-04-09 2000-04-20 Process for the preparation of monodisperse polymer particles TW589330B (en)

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GBGB9908163.0A GB9908163D0 (en) 1999-04-09 1999-04-09 Process
GBGB0007008.6A GB0007008D0 (en) 1999-04-09 2000-03-22 Process

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US (6) US7217762B1 (zh)
EP (2) EP1177231B1 (zh)
CN (2) CN1311005C (zh)
AU (2) AU777829B2 (zh)
CA (1) CA2369293C (zh)
NO (1) NO332815B1 (zh)
TW (1) TW589330B (zh)
WO (1) WO2000061647A1 (zh)

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