JP2016530349A - 自動食器洗浄のための配合物における、ポリエーテル化合物の存在下で酸基含有モノマーを重合することによって得ることができるゲル様ポリマー組成物の使用の方法 - Google Patents
自動食器洗浄のための配合物における、ポリエーテル化合物の存在下で酸基含有モノマーを重合することによって得ることができるゲル様ポリマー組成物の使用の方法 Download PDFInfo
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- JP2016530349A JP2016530349A JP2016522600A JP2016522600A JP2016530349A JP 2016530349 A JP2016530349 A JP 2016530349A JP 2016522600 A JP2016522600 A JP 2016522600A JP 2016522600 A JP2016522600 A JP 2016522600A JP 2016530349 A JP2016530349 A JP 2016530349A
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- KFNGWPXYNSJXOP-UHFFFAOYSA-N 3-(2-methylprop-2-enoyloxy)propane-1-sulfonic acid Chemical compound CC(=C)C(=O)OCCCS(O)(=O)=O KFNGWPXYNSJXOP-UHFFFAOYSA-N 0.000 claims description 3
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- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 claims description 3
- ZTWTYVWXUKTLCP-UHFFFAOYSA-N vinylphosphonic acid Chemical compound OP(O)(=O)C=C ZTWTYVWXUKTLCP-UHFFFAOYSA-N 0.000 claims description 3
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 claims description 3
- XVOUMQNXTGKGMA-OWOJBTEDSA-N (E)-glutaconic acid Chemical compound OC(=O)C\C=C\C(O)=O XVOUMQNXTGKGMA-OWOJBTEDSA-N 0.000 claims description 2
- 239000001124 (E)-prop-1-ene-1,2,3-tricarboxylic acid Substances 0.000 claims description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 claims description 2
- PRAMZQXXPOLCIY-UHFFFAOYSA-N 2-(2-methylprop-2-enoyloxy)ethanesulfonic acid Chemical compound CC(=C)C(=O)OCCS(O)(=O)=O PRAMZQXXPOLCIY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 2
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 2
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- GQTFHSAAODFMHB-UHFFFAOYSA-N 2-prop-2-enoyloxyethanesulfonic acid Chemical compound OS(=O)(=O)CCOC(=O)C=C GQTFHSAAODFMHB-UHFFFAOYSA-N 0.000 claims description 2
- OXOHMAPRQAJJIR-UHFFFAOYSA-N 3-(2,3-dihydroxypropoxy)propane-1,2-diol;sulfuric acid Chemical compound OS(O)(=O)=O.OCC(O)COCC(O)CO OXOHMAPRQAJJIR-UHFFFAOYSA-N 0.000 claims description 2
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L71/02—Polyalkylene oxides
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- C09D133/00—Coating compositions based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
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- C09J133/00—Adhesives based on 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
Description
a)A)少なくとも1種のα,β−エチレン性不飽和酸、および
B)モノマー組成物M)の合計質量に対して、0質量%から0.1質量%の、1分子当たり2個以上の重合性α,β−エチレン性不飽和二重結合を有する架橋性モノマー
からなるモノマー組成物M)を提供し、
b)工程a)において提供されたモノマー組成物M)を、少なくとも200g/molの数平均分子量を有するポリエーテルオールならびにそのモノおよびジ−(C1〜C6−アルキルエーテル)、ポリエーテル基を含有する界面活性剤、ならびにそれらの混合物から選択される少なくとも1種のポリエーテル構成成分PE)の存在下でフリーラジカル重合にかける
プロセスによって得られるゲル形態のポリマー組成物を使用する方法を提供する。
− 本発明に従って使用されるポリマー組成物は、清澄なゲルの形態で提供することができる。それらは、特定の実施において、それら自体がゲル形態である機械食器洗浄のための配合物に適当である。
− 使用されるポリマー組成物は、ポリエーテル構成成分とポリアクリル酸との間の高い適合性およびさらなる界面活性剤との高い適合性の両方で注目に値する。
− 本発明に従って使用される配合物において使用されるポリマー組成物の生成において、架橋性モノマーの使用で実質的にまたは完全に分注することが可能である。こうして得られたポリマー組成物は、有利には水溶性である。
工程a)において提供されるモノマー組成物M)は、構成成分A)として、少なくとも1種のα,β−エチレン性不飽和酸を含む。
− α,β−エチレン性不飽和カルボン酸A1)としてアクリル酸、
− 任意に、少なくとも1種のさらなるα,β−エチレン性不飽和酸A2)、および
− モノマー組成物M)の合計質量に対して、0質量%から0.1質量%の、1分子当たり2個以上の重合性α,β−エチレン性不飽和二重結合を有する架橋性モノマー
からなる。
本発明ポリマー組成物は、未架橋または軽く架橋されているポリマーからなる。本発明ポリマー組成物の製造のために使用されるモノマー組成物M)は、そのため、あるとしたら少量の架橋性モノマーB)だけを含む。架橋剤は、本発明に関連して、1分子当たり2個以上の重合性エチレン性不飽和二重結合を有する化合物である。
適当なポリエーテル構成成分PE)は、少なくとも200g/molの数平均分子量を有するポリエーテルオールおよびそのモノおよびジ(C1〜C6−アルキルエーテル)である。
− 低分子量C3〜C6アルコールまたはC7〜C30脂肪アルコールに由来するアルキルポリオキシアルキレンエーテル。本発明におけるエーテル構成成分は、エチレンオキシド単位、プロピレンオキシド単位、1,2−ブチレンオキシド単位、1,4−ブチレンオキシド単位、ならびにそれらのランダムコポリマーおよびブロックコポリマーから由来してもよい。適当な非イオン性界面活性剤は、とりわけ、一般式(VI)
R10−O−(CH2CH2O)x−(CHR11CH2O)y−R12(VI)
(式中、
R10は、6個から22個の炭素原子を有する直鎖または分岐アルキル基であり、
R11およびR12は、各々独立して、水素、または1個から10個の炭素原子もしくはHを有する直鎖または分岐アルキル基であり、R12は、好ましくはメチルであり、
xおよびyは、各々独立して、0から300である。好ましくは、x=1から100およびy=0から30である)
の界面活性剤を含む。
R13−O−(CH2CH2O)s−(CH2CH2CH2O)t−(CH2CH2CH2CH2O)u−(CH2CHR14O)v−CH2CH(OH)R15(VII)
(式中、
式(VII)の化合物におけるアルキレンオキシド単位の配列は任意であり、
s、t、uおよびvは、各々独立して、0から500の整数であり、s、t、uおよびvの和は0より大きく、
R13およびR15は、各々独立して、直鎖または分岐の飽和C1〜C40−アルキル基またはモノまたはポリ不飽和C2〜C40−アルケニル基であり、
R14は、メチル、エチル、n−プロピル、イソプロピルおよびn−ブチルから選択される)
のヒドロキシル基を含有する界面活性剤。
R13−O−(CH2CH2O)s−(CH2CH(CH3)O)v−CH2CH(OH)R15(VII.1)
(式中、
−(CH2CH2O)−および(CH2CH(CH3)O)−単位の配列は任意であり、
sおよびvは、各々独立して、0から500の整数であり、sおよびvの和は0より大きく、
R13およびR15は、各々独立して、直鎖飽和C1〜C30−アルキル基または分岐飽和C3〜C30−アルキル基またはモノまたはポリ不飽和C2〜C30−アルケニル基である)
のヒドロキシル基を含有する界面活性剤である。
R16−O−(CH2CH2O)p−(CH2CHR17O)q−C(=O)R18(VIII)
(式中、
式(VIII)の化合物におけるアルキレンオキシド単位の配列は任意であり、
pおよびqは、各々独立して、0から500の整数であり、pおよびqの和は0より大きく、
R16およびR18は、各々独立して、直鎖または分岐の飽和C1〜C40−アルキル基またはモノまたはポリ不飽和C2〜C40−アルケニル基であり、
R17は、メチル、エチル、n−プロピル、イソプロピルおよびn−ブチルから選択される)
のアルコールポリオキシアルキレンエステル。
− アルコキシ化された動物および/または植物の脂肪および/または油、例えばコーン油エトキシレート、ヒマシ油エトキシレート、タロー脂肪エトキシレート、
− アルキルフェノールアルコキシレート、例えばエトキシ化イソオクチル−、オクチル−またはノニルフェノール、トリブチルフェノールポリオキシエチレンエーテル、
− 脂肪アミンアルコキシレート、脂肪酸アミドおよび脂肪酸ジエタノールアミドアルコキシレート、特にそのエトキシレート、
− ポリオキシアルキレンソルビタン脂肪酸エステル。
工程b)におけるフリーラジカル重合は、水、C1〜C6−アルカノール、PE)以外のポリオール、そのモノおよびジアルキルエーテル、ならびにそれらの混合物から選択される溶媒S)の存在下で行い得る。適当なポリオールならびにそのモノおよびジアルキルエーテルは、アルキレングリコールモノ(C1〜C4−アルキル)エーテル、アルキレングリコールジ(C1〜C4−アルキル)エーテル、200g/mol未満の数平均分子量を有するオリゴアルキレングリコールならびにそのモノ(C1〜C4−アルキル)エーテルおよびジ(C1〜C4−アルキル)エーテルも含む。
本発明に従って使用されるポリマー組成物の製造は、少なくとも1種のポリエーテル構成成分PE)の存在下でのモノマー組成物M)のフリーラジカル重合を含む。それは、好ましくは供給法で行われる。これは、一般に、少なくとも、液状形態の該モノマーを反応混合物中に計量供給することを含む。計量供給条件下でのモノマー液体は、溶媒S)の添加なく反応混合物中に供給することができ、そうでなければ、モノマーは、適当な溶媒S)中の溶液として使用される。
b1)ポリエーテル構成成分PE)の少なくとも一部、任意に連鎖移動剤CTA)の少なくとも一部、および重合が溶媒S)の存在下で行われるならば、任意にS)の少なくとも一部を含む初期投入材料を提供すること;
b2)1つまたは複数の供給材料中にモノマー組成物M)を添加すること、ならびに少なくとも1種のポリエーテル構成成分PE)および/または溶媒S)の一部に溶解させたフリーラジカル開始剤FRI)を含む供給材料を添加すること、ならびに任意に、初期投入材料において使用されない連鎖移動剤CTA)の量を含む供給材料を添加すること、
b3)任意に、工程b2)において得られた反応混合物の重合を続けること
を含む。
アスコルビン酸/硫酸鉄(II)/ペルオキソ二硫酸ナトリウム、
tert−ブチルヒドロペルオキシド/二亜硫酸ナトリウム、
tert−ブチルヒドロペルオキシド/ヒドロキシメタンスルフィン酸ナトリウム、
H2O2/CuI
である。
本発明に従って使用されるポリマー組成物は、界面活性剤としておよび共ビルダーとしての両方で有効である。機械食器洗浄のためのポリマー組成物を含む発明配合物の例は、したがって、機械食器洗浄用洗剤、リンス助剤、およびリンス助剤機能を持つ機械食器洗浄用洗剤を含む。室温(20℃)での配合物は、特に、ゲル形態、固体形態、または一部ゲル形態および一部固体形態である。
a)少なくとも1種のゲル形態の発明ポリマー組成物、
b)少なくとも1種のビルダー(金属イオン封鎖剤、ビルダー材料、錯化剤、キレーター、キレート化剤または軟化剤とも称される)、
c)任意に、少なくとも1種の酵素、
d)任意に、少なくとも1種の漂白剤、
e)水、
f)任意に、少なくとも1種の増粘剤、ならびに
g)任意に、好ましくはa)以外の以下の添加剤から選択される少なくとも1種の添加剤:界面活性剤、塩基、腐食抑制剤、消泡剤、染料、芳香、充填剤、可溶化剤および有機溶媒。
a)少なくとも1種のゲル形態の発明ポリマー組成物0.1質量%から50質量%、
b)少なくとも1種のビルダーおよび/または共ビルダー5質量%から90質量%、
c)少なくとも1種の酵素0質量%から8質量%、
d)少なくとも1種の漂白剤0質量%から30質量%、
e)水0.1質量%から90質量%、
f)少なくとも1種の増粘剤0質量%から8質量%、
g)少なくとも1種のさらなる添加剤0質量%から25質量%、
但し、構成成分a)からg)の質量が最大100質量%までとなるという条件である。
a)少なくとも1種のゲル形態の発明ポリマー組成物2質量%から40質量%、
b)少なくとも1種のビルダーおよび/または共ビルダー5質量%から80質量%、
c)少なくとも1種の酵素0.1質量%から6質量%、
d)少なくとも1種の漂白剤0質量%から30質量%、
e)水0.1質量%から80質量%、
f)少なくとも1種の増粘剤0質量%から6質量%、
g)少なくとも1種のさらなる添加剤0質量%から25質量%、
但し、構成成分a)からg)の質量が、最大100質量%までとなるという条件である。
a)少なくとも1種のゲル形態の発明ポリマー組成物0.12質量%から30質量%、
b)少なくとも1種のビルダーおよび/または共ビルダー5質量%から75質量%、
c)少なくとも1種の酵素0.1質量%から6質量%、
d)少なくとも1種の漂白剤0質量%から25質量%、
e)水0.1質量%から80質量%、
f)少なくとも1種の増粘剤0.1質量%から5質量%、
g)少なくとも1種のさらなる添加剤0質量%から25質量%、
但し、構成成分a)からg)の質量が、最大100質量%までとなるという条件である。
構成成分a)として適当なおよび好ましい発明ポリマー組成物に関して、上記の詳細が参照される。
捕捉剤、ビルダー材料、錯化剤、キレーター、キレート化剤または軟化剤とも時々称されるビルダーおよび共ビルダーは、アルカリ土類金属塩および他の水溶性金属塩を結合する。それらは、汚れを分解すること助け、汚れ構成成分を分散し、汚れを剥離することを助け、一部の場合において、それら自体が洗浄効果を有する。加えて、それらが固体であり、粉状配合物において使用される場合、それらは粉末を易流動性に保持する。
酵素は、好ましくは、ヒドロラーゼ、例えばプロテアーゼ、エステラーゼ、グルコシダーゼ、リパーゼ、アミラーゼ、セルラーゼ、マンナナーゼ、他のグリコシルヒドロラーゼ、および前述の酵素の混合物から選択される。全てのこれらのヒドロラーゼは、タンパク質、グリースまたはデンプンを含有するしみからの汚れの溶解および除去に寄与する。漂白するためにオキシレダクターゼを使用することも可能である。特によく適しているのは、Bacillus subtilis、Bacillus licheniformis、Streptomyceus griseusおよびHumicola insolensなどの細菌株または真菌から得られる活性酵素成分である。
漂白剤d)は、好ましくは、漂白剤と同様に、任意に漂白剤活性化剤、漂白剤触媒および/または漂白剤安定剤も含む漂白剤系である。
本発明に従って使用されるポリマー組成物は、増粘する目的でレオロジー的特性を修飾するのに単独でも適当である。
構成成分a)以外の適当な追加の界面活性剤g)は、アニオン性界面活性剤、非イオン性界面活性剤、カチオン性界面活性剤、両性界面活性剤、およびそれらの混合物である。
− グリセリルエステル、例えばモノステアリン酸グリセリル、
− 糖界面活性剤、ソルビトールエステル、例えばソルビタン脂肪酸エステル(モノオレイン酸ソルビタン、トリステアリン酸ソルビタン)、ポリオキシエチレンポリオキシエチレンソルビタン脂肪酸エステル、アルキルポリグリコシド、N−アルキルグルコンアミド、
− アルキルメチルスルホキシド、
− アルキルジメチルホスフィンオキシド、例えばテトラデシルテトラデシルジメチルホスフィンオキシド。
EO:エチレンオキシド
PO:プロピレンオキシド
BO:ブチレンオキシド
Mn:数平均分子量
Mw:重量平均分子量
PET:ポリエチレンテレフタレート
TL:透明度値
n.d.:未決定
rad/s:1秒当たりのラジアント
pphm:モノマー100質量部当たりの質量部(モノマー百当たりの部)。
I.a)水溶性の決定
水溶性を決定するため、特別なポリマー組成物5gを1lのビーカーに導入し、事前に40℃に加熱されていた水900mlを添加した。磁気撹拌機を用いて混合物を40℃で20分間撹拌し、pHを8に水酸化ナトリウム溶液で調整した。水溶性ポリマーゲルは、透明なまたは僅かに濁っている溶液に至った。
ポリマーの重量平均分子量をゲル浸透クロマトグラフィー(GPC)によって決定した。この目的のため、以下の機器およびクロマトグラフィー法を使用した:
標準:中和されたポリアクリル酸
溶出液:0.08mol/lのトリス、pH7.0、+0.15mol/lのNaCl+脱イオン水中の0.01mol/lのNaN3
流量:0.8ml/min
カラムセット:1プレカラム(l=5cm)、2つの分離カラム(各々l=30cm)
カラム温度:35℃
検出器:DRI(屈折率検出器)Agilent 1100
500nmの波長および20℃でのその光透過率(TL)によって、試験片の透明度を決定した。使用された100%基準は水であった。
一般的製造方法:
3つの供給材料、窒素導入口およびアンカー撹拌機が備えられているガラス反応器に、初めに、ポリエーテル構成成分(PE)、任意に連鎖移動剤(CTA)および任意に溶媒(S)を表1に従った量で投入し、窒素で2〜3分間パージし、75℃に加熱した。引き続いて、供給材料1〜3を初期投入材料に75℃でおよび100回転/分にて4時間以内で撹拌しながら同時に添加した。供給材料1はモノマー(M)を含み、供給材料2は、少量の非イオン性界面活性剤(PE)および/または溶媒(S)中に溶解させた開始剤(FRI)を含み、供給材料3は、任意に、さらなる量の連鎖移動剤(CTA)を含んでいた。供給材料1、2および3の添加後、混合物を75℃でおよび100回転/分にてさらなる時間の間、連続重合のために撹拌した。引き続いて、ポリマーをビーカーに注ぎ入れ、直ちに室温に冷却した。
M1: アクリル酸
PE1:液体非イオン性界面活性剤;EO 5.5mol、PO 2molおよびトリデカノール1molの反応生成物
PE2:液体非イオン性界面活性剤;EO 7.8mol、BO 1.2molおよび主に非分岐C9〜C11オキソアルコール1.0molの反応生成物
PE3:400g/molの平均モル質量を有するポリエチレングリコールからなる液体ポリエーテル
PE4:変性脂肪アルコールポリグリコールエーテルからなる固体非イオン性界面活性剤
PE5:C13C15アルコール+9 EO+2 BuO
PE6:C6アルコール+6 EO(ヘキシルグリコールまたはヘキシルジグリコールから進行)
PE7:C13C15オキソアルコール+8 EO+3.8 PO
CTA1:2−エチルヘキシルチオグリコレート
CTA2:2−メルカプトエタノール
CTA3:NaH2PO2(55%の水溶液)
S1:プロピレングリコール
S2:ジプロピレングリコール
S3: 水
S4: イソプロパノール
FRI1:tert−ブチルペルオキシネオデカノエート(純度:97%)(CAS番号26748−41−4)
FRI2:tert−ブチルペルオキシピバレート(純度:75%)(CAS番号927−07−1)
FRI3:2,2’−アゾビス(2−メチルメチルプロピオンアミジン)ジヒドロクロリド(CAS番号2997−92−4)
III.a)粘弾性パラメータ
温度の関数としての粘度:
検査されるべき試料について温度の関数としての粘度プロファイルを、回転式レオメーター(Peltierシステムを用いるTA InstrumentsからのDHR−1、プレート/プレート形状、φ40mm、h=1mm)の手段によって20℃から80℃の温度で検査した。温度傾斜(Mmin=100μNmでγ=1%)。80℃から20℃の往復の測定温度、各々2回の実行(冷却/加熱速度2K/min)。測定時間1回の実行当たり30分。
合計質量:10gから25g
Claims (23)
- 機械食器洗浄のための配合物における、
a)A)少なくとも1種のα,β−エチレン性不飽和酸、および
B)モノマー組成物M)の合計質量に対して、0質量%から0.1質量%の、1分子当たり2個以上の重合性α,β−エチレン性不飽和二重結合を有する架橋性モノマー
からなるモノマー組成物M)を提供し、
b)工程a)において提供されたモノマー組成物M)を、少なくとも200g/molの数平均分子量を有するポリエーテルオールならびにそのモノおよびジ−(C1〜C6−アルキルエーテル)、ポリエーテル基を含有する界面活性剤、ならびにそれらの混合物から選択される少なくとも1種のポリエーテル構成成分PE)の存在下で、フリーラジカル重合にかける
プロセスによって得られるゲル形態のポリマー組成物を使用する方法。 - 但し、ポリエーテル構成成分PE)が、繰り返しプロピレンオキシド単位を有するポリエーテルオールまたは繰り返しプロピレンオキシド単位を有するポリエーテルオールのモノもしくはジ−(C1〜C6−アルキルエーテル)を含む場合、これらの繰り返しプロピレンオキシド単位の割合が、平均して、1分子当たり18単位以下、好ましくは1分子当たり17単位以下、より好ましくは1分子当たり15単位以下、特に1分子当たり10単位以下である、請求項1に記載の方法。
- 工程b)におけるフリーラジカル重合が、水、C1〜C6−アルカノール、PE)以外のポリオール、そのモノおよびジアルキルエーテル、ならびにそれらの混合物から選択される溶媒S)の存在下で追加的に行われる、請求項1または2に記載の方法。
- 工程b)における重合が、供給モードにて、ポリエーテル構成成分PE)の少なくとも一部および任意に、存在するならば、溶媒S)の少なくとも一部を初期に投入すること、ならびに工程a)において提供されたモノマー組成物の少なくとも一部および少なくとも1種のフリーラジカル開始剤FRI)を初期投入材料に供給することによって行われる、請求項1から3のいずれか一項に記載の方法。
- 工程b)におけるフリーラジカル重合が、溶媒S)の存在下で追加的に行われ、
− 工程b)における反応の開始時の反応混合物が、反応混合物の合計質量に対して、0質量%から90質量%、好ましくは0.1質量%から70質量%の量で溶媒S)を含み、
− 工程b)における反応の終結後の反応混合物が、反応混合物の合計質量に対して、0質量%から50質量%、好ましくは0.1質量%から40質量%の量で溶媒S)を含む、
請求項3または4に記載の方法。 - 工程b)におけるフリーラジカル重合が、プロピレングリコール、ジプロピレングリコール、水、およびそれらの混合物から選択される溶媒S)の存在下で行われる、請求項3から5のいずれか一項に記載の方法。
- 工程b)における重合が、20℃から150℃、好ましくは30℃から120℃、特に40℃から90℃の範囲の温度で行われる、請求項1から6のいずれか一項に記載の方法。
- 工程a)において提供されたモノマー組成物が、アクリル酸A1)および任意に少なくとも1種のさらなるα,β−エチレン性不飽和酸A2)からなる、請求項1から7のいずれか一項に記載の方法。
- 構成成分A)が、カルボン酸、スルホン酸、リン酸およびそれらの混合物から選択される少なくとも1種のα,β−エチレン性不飽和酸A2)を含む、請求項1から8のいずれか一項に記載の方法。
- さらなるα,β−エチレン性不飽和酸A2)が、メタクリル酸、エタクリル酸、α−クロロアクリル酸、クロトン酸、マレイン酸、イタコン酸、シトラコン酸、メサコン酸、グルタコン酸、アコニット酸、フマル酸、2−アクリルアミド−2−メチルプロパンスルホン酸、ビニルスルホン酸、アリルスルホン酸、スルホエチルアクリレート、スルホエチルメタクリレート、スルホプロピルアクリレート、スルホプロピルメタクリレート、2−ヒドロキシ−3−アクリロイルオキシプロピルスルホン酸、2−ヒドロキシ−3−メタクリロイルオキシプロピルスルホン酸、スチレンスルホン酸、ビニルホスホン酸、アリルホスホン酸およびそれらの混合物から選択される、請求項8または9に記載の方法。
- モノマー組成物M)がアクリル酸のみからなる、請求項1から8のいずれか一項に記載の方法。
- フリーラジカル重合が連鎖移動剤の存在下で実施される、請求項1から11のいずれか一項に記載の方法。
- ポリエーテル構成成分PE)が、約200から100000の範囲の数平均分子量を有する少なくとも1種のポリエーテルオールまたはそのモノもしくはジ−(C1〜C2−アルキルエーテル)を含む、請求項1から12のいずれか一項に記載の方法。
- ポリエーテル構成成分PE)が、アルキレンオキシド単位として組み込まれるエチレンオキシド単位のみを含む少なくとも1種のポリエーテルオールまたはそのモノもしくはジ−(C1〜C2−アルキルエーテル)を含むかまたはそれからなる、請求項1から13のいずれか一項に記載の方法。
- ポリエーテル構成成分PE)が、アルキルポリオキシアルキレンエーテル、アリールポリオキシアルキレンエーテル、アルキルアリールポリオキシアルキレンエーテル、アルコキシ化された動物および/または植物の脂肪および/または油、脂肪アミンアルコキシレート、脂肪酸アミドアルコキシレート、脂肪酸ジエタノールアミドアルコキシレート、ポリオキシエチレンソルビタン脂肪酸エステル、アルキルポリエーテルスルフェート、アリールポリエーテルスルフェート、アルキルアリールポリエーテルスルフェート、アルキルポリエーテルスルホネート、アリールポリエーテルスルホネート、アルキルアリールポリエーテルスルホネート、アルキルポリエーテルホスフェート、アリールポリエーテルホスフェート、アルキルアリールポリエーテルホスフェート、グリセリルエーテルスルホネート、グリセリルエーテルスルフェート、モノグリセリド(エーテル)スルフェート、脂肪酸アミドエーテルスルフェート、ポリオキシアルキレンソルビタン脂肪酸エステルおよびそれらの混合物から選択される、ポリエーテル基を含有する少なくとも1種の界面活性剤を含む、請求項1から14のいずれか一項に記載の方法。
- ポリエーテル構成成分PE)が、
− 一般式(VI)
R10−O−(CH2CH2O)x−(CHR11CH2O)y−R12
[式中、
R10は、8個から22個の炭素原子を有する直鎖または分岐アルキル基であり、
R11およびR12は、各々独立して、水素であるか、または1〜10個の炭素原子またはHを有する直鎖もしくは分岐アルキル基であり、R12は、好ましくはメチルであり、
xおよびyは、各々独立して、0から300であり、xおよびyの和は0より大きい]
のアルキルポリオキシアルキレンエーテル、
− 一般式(VII)
R13−O−(CH2CH2O)s−(CH2CH2CH2O)t−(CH2CH2CH2CH2O)u−(CH2CHR14O)v−CH2CH(OH)R15
[式中、
式(VII)の化合物におけるアルキレンオキシド単位の配列は任意であり、
s、t、uおよびvは、各々独立して、0から500の整数であり、s、t、uおよびvの和は0より大きく、
R13およびR15は、各々独立して、直鎖または分岐の飽和C1〜C40−アルキル基またはモノまたはポリ不飽和C2〜C40−アルケニル基であり、
R14は、メチル、エチル、n−プロピル、イソプロピルおよびn−ブチルから選択される]
のヒドロキシル基を含有する界面活性剤、
− 一般式(VIII)
R16−O−(CH2CH2O)p−(CH2CHR17O)q−C(=O)R18
[式中、
式(VIII)の化合物におけるアルキレンオキシド単位の配列は任意であり、
pおよびqは、各々独立して、0から500の整数であり、pおよびqの和は0より大きく、
R16およびR18は、各々独立して、直鎖または分岐の飽和C1〜C40−アルキル基またはモノ−もしくはポリ不飽和C2〜C40−アルケニル基であり、
R17は、メチル、エチル、n−プロピル、イソプロピルおよびn−ブチルから選択される]
の脂肪アルコールポリオキシアルキレンエステル
から選択される、ポリエーテル基を含有する少なくとも1種の界面活性剤を含む、請求項1から15のいずれか一項に記載の方法。 - ポリマー組成物が、1.5mmol/gから15mmol/g、好ましくは4mmol/gから7mmol/gの酸基の含有量を有する、請求項1から16のいずれか一項に記載の方法。
- ポリマー組成物が、水の透明度に対して少なくとも85%、より好ましくは少なくとも90%の、500nmで測定されるTLとして報告される透明度を有する、請求項1から17のいずれか一項に記載の方法。
- ポリマー組成物における酸基の最大80mol%まで、好ましくは酸基の最大70mol%まで、特に酸基の最大20mol%までが中和形態である、請求項1から18のいずれか一項に記載の方法。
- ポリマー組成物における酸基が中和形態でない、請求項1から18のいずれか一項に記載の方法。
- ポリマー組成物に存在するポリマーが1000ダルトンから70000ダルトンの重量平均分子量を有する、請求項1から20のいずれか一項に記載の方法。
- 機械食器洗浄のための配合物が、以下の構成成分:
a)請求項1から21のいずれか一項に記載の少なくとも1種のポリマー組成物、
b)少なくとも1種のビルダー、
c)任意に、少なくとも1種の酵素、
d)任意に、少なくとも1種の漂白剤、
e)水、
f)任意に、少なくとも1種の増粘剤、ならびに
g)任意に、好ましくは、a)以外の以下の添加剤から選択される少なくとも1種の添加剤:界面活性剤、塩基、腐食抑制剤、消泡剤、染料、芳香、充填剤、可溶化剤および有機溶媒
を含む、請求項1から21のいずれか一項に記載の方法。 - 清浄されるべき食器類が、請求項22に記載の機械食器洗浄のための配合物を含む処理溶液と接触される、食器類の機械清浄のための方法。
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WO2018110638A1 (ja) * | 2016-12-16 | 2018-06-21 | 花王株式会社 | マイクロカプセルの製造方法 |
JP6360642B1 (ja) * | 2016-12-16 | 2018-07-18 | 花王株式会社 | マイクロカプセルの製造方法 |
US11179695B2 (en) | 2016-12-16 | 2021-11-23 | Kao Corporation | Method for producing microcapsule |
WO2023074720A1 (ja) * | 2021-10-27 | 2023-05-04 | 住友精化株式会社 | α,β-不飽和カルボン酸化合物の架橋重合体及びその用途 |
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