JPH10501173A - ポリマーマイクロビーズ及びその製造方法 - Google Patents
ポリマーマイクロビーズ及びその製造方法Info
- Publication number
- JPH10501173A JPH10501173A JP8501165A JP50116596A JPH10501173A JP H10501173 A JPH10501173 A JP H10501173A JP 8501165 A JP8501165 A JP 8501165A JP 50116596 A JP50116596 A JP 50116596A JP H10501173 A JPH10501173 A JP H10501173A
- Authority
- JP
- Japan
- Prior art keywords
- microbead
- microbeads
- group
- water
- emulsion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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- Chemical & Material Sciences (AREA)
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- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Description
Claims (1)
- 【特許請求の範囲】 1.連続な細孔により連通された空洞を有する多孔質の架橋したポリマーマイ クロビーズであって、各マイクロビーズの内部にある前記空洞の少なくとも幾つ かがそのマイクロビーズの表面と通じており、そして前記マイクロビーズの約1 0%が実質的に球状又は実質的に楕円体又はこれらの組合せであるマイクロビー ズ。 2.約5μm〜約5mmの平均直径を有する請求項1記載のマイクロビーズ。 3.少なくとも約70%の気孔率を有する請求項1記載のマイクロビーズ。 4.多孔質の架橋したポリマーマイクロビーズを製造する方法であって、 (a)(i)(1)実質的に水不溶性の単官能価モノマー; (2)実質的に水不溶性の多官能価架橋剤;及び (3)安定な油中水滴型エマルションを形成させるのに適する乳化剤; を含む油相;と (ii)水性不連続相; とを組み合わせ、少なくとも約70%の水性不連続相を含むエマルションを形成さ せること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること;次いで (c)前記エマルション液滴を重合させること; を含む方法。 5.モノマーがスチレンをベースとするモノマーである請求項4記載の方法。 6.モノマーが油相中に約4〜約90重量%の濃度で存在する請求項4記載の 方法。 7.架橋剤が、ジビニルベンゼン化合物、ジ−又はトリアクリル化合物、トリ アリルイソシアヌレート、及びこれらの組合せからなる群より選ばれる、請求項 4記載の方法。 8.架橋剤が油相中に約1〜約90重量%の濃度で存在する請求項4記載の方 法。 9.乳化剤が、ソルビタン脂肪酸エステル、ポリグリセロール脂肪酸エステル 、ポリオキシエチレン脂肪酸又はエステルからなる群より選ばれるか、又は乳化 剤がこれらの組合せである、請求項4記載の方法。 10.乳化剤が油相中に約3〜約50重量%の濃度で存在する請求項4記載の 方法。 11.油相が油溶性重合開始剤を更に含む請求項4記載の方法。 12.開始剤がアゾ開始剤及び過酸化物開始剤からなる群より選ばれる請求項 11記載の方法。 13.油溶性重合開始剤が油相中に重合性ポリマーの合計量の約5重量%以下 の濃度で存在する請求項11記載の方法。 14.油相がポロゲンを更に含む請求項4記載の方法。 15.ポロゲンが、ドデカン、トルエン、シクロヘキサノール、n−ヘプタン 、イソオクタン及び石油エーテルからなる群より選ばれる、請求項14記載の方 法。 16.ポロゲンが油相中に約10〜約60重量%の濃度で存在する請求項14 記載の方法。 17.水性不連続相が水溶性重合開始剤を含む請求項4記載の方法。 18.水溶性重合開始剤が過酸化物開始剤を含む請求項17記載 の方法。 19.水溶性重合開始剤が水性不連続相中に約5重量%以下の濃度で存在する 請求項17記載の方法。 20.水中油滴型サスペンションが安定なサスペンションを生成させるのに適 する量の高内部相エマルションを含む請求項4記載の方法。 21.水性懸濁媒が沈殿防止剤を含む請求項4記載の方法。 22.沈殿防止剤が水溶性ポリマー及び水不溶性無機固形物からなる群より選 ばれる請求項21記載の方法。 23.沈殿防止剤が、改質されて疎水性が増加した水不溶性無機固形物を含む 、請求項23記載の方法。 24.沈殿防止剤が水性懸濁媒中に約1〜約30重量%の濃度で存在する請求 項21記載の方法。 25.水性懸濁媒が水溶性重合開始剤を含む請求項4記載の方法。 26.水溶性重合開始剤が過酸化物開始剤である請求項25記載の方法。 27.水溶性重合開始剤が水性懸濁媒中に約5重量%以下の濃度で存在する請 求項25記載の方法。 28.サスペンションが、安定なサスペンションを形成させるのに十分な剪断 攪拌を提供しながら高内部相エマルションを水性懸濁媒に加えることにより形成 される、請求項4記載の方法。 29.多孔質の架橋したポリマーマイクロビーズを製造する方法であって、 (a)(i)(1)スチレン; (2)ジビニルベンゼン; (3)アゾイソビスブチロニトリル; (4)ドデカン;及び (5)ソルビタンモノオレエート; を含む油相;と (ii)過硫酸カリウムを含む水性不連続相; とを組み合わせ、エマルションを形成させること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること、ここで前記懸濁媒は、 (i) 過硫酸カリウム; (ii) 改質シリカ;及び (iii)ゼラチン; を含む;次いで (c)前記エマルション液滴を重合させること; を含む方法。 30.(a)(i)(1)実質的に水不溶性の単官能価モノマー; (2)実質的に水不溶性の多官能価架橋剤;及び (3)安定な油中水滴型エマルションを形成させるのに適する乳化剤; を含む油相;と (ii)水性不連続相; とを組み合わせ、エマルションを形成させること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること;次いで (c)前記エマルション液滴を重合させること; を含む方法により製造される多孔質の架橋したポリマーマイクロビーズ。 31.(a)(i)(1)スチレン; (2)ジビニルベンゼン; (3)アゾイソビスブチロニトリル; (4)ドデカン;及び (5)ソルビタンモノオレエート; を含む油相;と (ii)過硫酸カリウムを含む水性不連続相; とを組み合わせ、エマルションを形成させること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること、ここで前記懸濁媒は、 (i) 過硫酸カリウム; (ii) 改質シリカ;及び (iii)ゼラチン; を含む;次いで (c)前記エマルション液滴を重合させること; を含む方法により製造される多孔質の架橋したポリマーマイクロビーズ。 32.構造単位: (上式中、Aは架橋された炭素鎖であり、Yは任意のスペーサー基であり、そし てZはイオン性又は極性官能基である) を含む水性及び/又は有機酸性液体を吸収するように官能化された請求項1記載 のマイクロビーズ。 33.メチルオレエート吸収量に対する官能化されたマイクロビ ーズによる水性及び/又は有機酸の吸収量の比が約1.2以上である、請求項3 2記載の官能化されたマイクロビーズ。 34.Zが、8個以上の炭素原子を有する有機基である対イオンの存在のもと で、アミノ基又は置換アミノ基;8個以上の炭素原子を有するアルキルカチオン 第4級アンモニウム基;及び8個以下の炭素原子を有するアルキルカチオン第4 級アンモニウム基からなる群より選ばれる、請求項32記載の官能化されたマイ クロビーズ。 35.Zが、下記化学種1〜3: (上式中、R2、R3、R4、R5及びR6は同一であっても異なっていてもよく、 アルキル、シクロアルキル、アリール、及びヒドロキシアルキルからなる群より 選ばれるか、又はR2及びR3は環構造の一部を形成し、そしてカチオン第4級ア ンモニウム(3)に対してR4とR5とR6の全体に存在する炭素原子の数が10 以上であり、アミン塩(2)に対してR4とR5の全体に存在する炭素原子の数が 8以上であり、そして対イオンX-は有機又は無機イオンである) からなる群より選ばれるイオン性又は極性官能基を含む、請求項32記載の官能 化されたマイクロビーズ。 36.カチオン第4級アンモニウム(3)に対してR4とR5とR6の全体に存 在する炭素原子の数が10未満であり、アミン塩(2)に対してR4とR5の全体 に存在する炭素原子の数が8未満であり、そして対イオンX-が8個以上の炭素 原子を有する有機基である、請求項35記載の官能化されたマイクロビーズ。 37.架橋度が約1〜約20%である請求項32記載の官能化されたマイクロ ビーズ。 38.架橋度が約2〜約10%である請求項32記載の官能化されたマイクロ ビーズ。 39.気孔率が約95%以上である請求項32記載の官能化されたマイクロビ ーズ。 40.官能化度が約50%以上である請求項32記載の官能化されたマイクロ ビーズ。 41.下記構造単位: (上式中、Aは架橋された炭素鎖であり、Yは任意のスペーサー基であり、そし てZはイオン性又は極性官能基である) を含む、水性液体を吸収するように官能化された請求項1記載のマイクロビーズ 。 42.吸水量に対する官能化されたマイクロビーズによる10%塩化ナトリウ ムの吸収量の比が約0.1以上である請求項41記載の官能化されたマイクロビ ーズ。 43.吸水量に対する10%塩化ナトリウムの吸収量の比が約0.5以上であ る請求項42記載の官能化されたマイクロビーズ。 44.吸水量に対する10%塩化ナトリウムの吸収量の比が約0.7以上であ る請求項43記載の官能化されたマイクロビーズ。 45.Zが、10個以下の炭素原子を有するアルキルカチオン第4級アンモニ ウム基;8個以下の炭素原子を有するアルキルアミン塩基;アルコキシレート基 ;硫酸、炭酸、リン酸又はスルホン酸基 の金属塩、アンモニウム塩、又は置換アンモニウム塩;からなる群より選ばれ、 但し、Zがスルホン酸である場合には、Yは下記の構造: を有しない、請求項41記載の官能化されたマイクロビーズ。 46.Zが、下記構造1〜2: (上式中、R2、R3、及びR4は同一であっても異なっていてもよく、アルキル 、シクロアルキル、アリール、及びヒドロキシアルキルからなる群より選ばれる か、又はR2及びR3は環構造の一部を形成し、そしてカチオン第4級アンモニウ ム(1)に対してR2とR3とR4の全体に存在する炭素原子の数が10未満であ り、アミン塩(2)に対してR4とR5の全体に存在する炭素原子の数が8未満で あり、そして対イオンX-は無機イオン又は8個未満の炭素原子を有するカルボ キシレート基である) からなる群より選ばれるイオン性又は極性官能基を含む、請求項41記載の官能 化されたマイクロビーズ。 47.Zが、下記構造: (上式中、pは1〜680であり、そして であり、ここでR5は水素又はアルキル基であり、Mは、金属、アンモニウム又 は置換アンモニウムカチオンである) を有するアルコキシレート基である、請求項41記載の官能化されたマイクロビ ーズ。 48.架橋度が約1〜約20%である請求項41記載の官能化されたマイクロ ビーズ。 49.架橋度が約2〜約10%である請求項41記載の官能化されたマイクロ ビーズ。 50.気孔率が約95%以上である請求項41記載の官能化されたマイクロビ ーズ。 51.官能化度が約50%以上である請求項41記載の官能化されたマイクロ ビーズ。 52.炭素含有構造を有する請求項1記載のマイクロビーズ。 53.少なくとも約90%の気孔率及び約0.25g/cc以下の乾燥密度を有 する請求項52記載の官能化されたマイクロビーズ。 54.(a)連続な細孔により連通された空洞を有する安定な多孔質の架橋し たポリマーマイクロビーズを製造すること;及び (b)不活性雰囲気中で前記安定なマイクロビーズを少なくとも約500℃の 温度に加熱すること; を含む炭素含有マイクロビーズを製造する方法。 55.(i)連続な細孔により連通された空洞を有する安定な多孔質の架橋し たポリマーマイクロビーズに少なくとも2種の成分を含む溶液を通すこと、ここ で前記2種の成分の一方と選択的に相互作用する化学基が前記マイクロビーズの 表面に結合されている;及び (ii)前記2種の成分を互いに分離すること; を含む分離方法。 56.分離方法がイオン交換クロマトグラフィーである請求項55記載の方法 。 57.化学基がマイクロビーズの表面に結合されている請求項55記載の方法 。 58.化学基がマイクロビーズの空洞内のゲル又はプレゲルに結合されている 請求項55記載の方法。 59.連続な細孔により連通された空洞を有する多孔質の架橋したポリマーマ イクロビーズに反応体を含む溶液を通すことを含む方法であって、反応体と相互 作用する化学基が前記マイクロビーズの表面に結合されている方法。 60.化学基がマイクロビーズの表面に結合されている請求項59記載の方法 。 61.化学基がマイクロビーズの空洞内のゲル又はプレゲルに結合されている 請求項60記載の方法。 62.化学合成において溶液及び反応体の成分からなる群より選ばれる化学物 質と相互作用する化学基を含むゲル又はプレゲルを空洞内に更に含む請求項1記 載のマイクロビーズ。 63.空洞が約1〜約100μmの直径を有する請求項62記載のマイクロビ ーズ。 64.液体の存在のもとで、その乾燥体積の約2倍を超えない体 積に膨潤する請求項62記載のマイクロビーズ。 65.マイクロビーズに対する膨潤したゲルの重量比が約60:40〜約95 :5になる請求項62記載のマイクロビーズ。 66.(a)連続な細孔により連通された空洞を有する多孔質の架橋したポリ マーマイクロビーズを製造すること;次いで (b)前記マイクロビーズの空洞内にゲル又はプレゲルを沈着及び保持させる こと; を含む、ゲル又はプレゲルを有するマイクロビーズを製造する方法。 67.工程(b)が、マイクロビーズを、そのマイクロビーズに適するプレゲル 成分及び膨潤溶剤を含む溶液に、膨潤したマイクロビーズに前記プレゲルが浸透 し、そしてマイクロビーズの空洞内にゲルを形成させるのに十分な時間接触させ ることを含む、請求項66記載の方法。 68.ポリペプチド及びオリゴヌクレオチドからなる群より選ばれる分子がそ の表面に結合される請求項1記載のマイクロビーズ。 69.分子が、抗体、レクチン、酵素及びハプテンからなる群より選ばれるポ リペプチドである、請求項68記載のマイクロビーズ。 70.分子が、非共有結合的吸着、共有結合、及び架橋分子を介する結合から なる群より選ばれる結合によりマイクロビーズの表面に結合される、請求項68 記載のマイクロビーズ。 71.(a)培地の存在のもとで、連続な細孔により連通された空洞を有する 多孔質の架橋したポリマーマイクロビーズに細胞を接触させる工程;次いで (b)マイクロビーズを攪拌する工程; の各工程を上記の順で含む方法。 72.油相が油溶性重合開始剤を更に含み、そして重合開始剤が水性不連続相 又は水性懸濁媒のいずれかの中に存在する、請求項4記載の方法。 73.油溶性開始剤が、過酸化ベンゾイル、過酸化ラウロイル、及びVAZO 開始剤からなる群より選ばれる、請求項72記載の方法。 74.油溶性重合開始剤が油相中に重合性モノマーの合計量の約5重量%以下 の濃度で存在する請求項72記載の方法。 75.水性不連続相が基本的に水からなる請求項72記載の方法。 76.前記エマルションが、 (a)天然又は合成ポリマー安定剤;及び (b)不活性溶剤; を更に含む請求項72記載の方法。 77.ポリマー安定剤がセルロース誘導体である請求項76記載の方法。 78.ポリマー安定剤が、メチルセルロース、エチルセルロース、 及びポリビニルアルコールからなる群より選ばれる、請求項76記載の方法。 79.ポリマー安定剤が油相中に約0.01〜約15重量%の濃度で存在する 請求項76記載の方法。 80.不活性溶剤がトリクロロエタン及びトルエンからなる群より選ばれる請 求項76記載の方法。 81.沈殿防止剤が天然ゴムである請求項72記載の方法。 82.(a)(i)(1)スチレン; (2)ジビニルベンゼン; (3)過酸化ラウロイル; (4)トリクロロエタン;及び (5)ソルビタンモノオレエート; を含む油相;と (ii)重合開始剤を含まない水性不連続相; とを組み合わせ、エマルションを形成させること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること、ここで前記懸濁媒はアラビアゴムを 含み、且つ、重合開始剤を含まない;次いで (c)前記エマルション液滴を重合させること; を含む多孔質の架橋したポリマーマイクロビーズを製造する方法。 83.(a)(i)(1)スチレン; (2)ジビニルベンゼン; (3)過酸化ラウロイル; (4)トリクロロエタン;及び (5)ソルビタンモノオレエート; を含む油相;と (ii)重合開始剤を含まない水性不連続相; とを組み合わせ、エマルションを形成させること; (b)前記エマルションを水性懸濁媒に加え、分散したエマルション液滴の水 中油滴型サスペンションを形成させること、ここで前記懸濁媒はアラビアゴムを 含み、且つ、重合開始剤を含まない;次いで (c)前記エマルション液滴を重合させること; を含む方法により製造される多孔質の架橋したポリマーマイクロビーズ。 84.油相がポロゲンを更に含む請求項72記載の方法。
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WO2011125673A1 (ja) | 2010-03-31 | 2011-10-13 | Jsr株式会社 | アフィニティークロマトグラフィー用充填剤 |
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Also Published As
Publication number | Publication date |
---|---|
US5863957A (en) | 1999-01-26 |
EP0764047B1 (en) | 2003-08-27 |
EP0764047B2 (en) | 2008-10-01 |
JP2009057578A (ja) | 2009-03-19 |
AU702241B2 (en) | 1999-02-18 |
US5583162A (en) | 1996-12-10 |
DE69531617T3 (de) | 2009-02-05 |
DE69531617D1 (de) | 2003-10-02 |
AU2693795A (en) | 1996-01-04 |
EP0764047A4 (en) | 1998-01-07 |
EP0764047A1 (en) | 1997-03-26 |
US5653922A (en) | 1997-08-05 |
US5760097A (en) | 1998-06-02 |
US6100306A (en) | 2000-08-08 |
CN1150764A (zh) | 1997-05-28 |
DE69531617T2 (de) | 2004-08-12 |
CA2190731A1 (en) | 1995-12-14 |
WO1995033553A1 (en) | 1995-12-14 |
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