JP7098540B2 - ポリウレタン分散液からのケタジンの蒸留分離 - Google Patents
ポリウレタン分散液からのケタジンの蒸留分離 Download PDFInfo
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- JP7098540B2 JP7098540B2 JP2018567874A JP2018567874A JP7098540B2 JP 7098540 B2 JP7098540 B2 JP 7098540B2 JP 2018567874 A JP2018567874 A JP 2018567874A JP 2018567874 A JP2018567874 A JP 2018567874A JP 7098540 B2 JP7098540 B2 JP 7098540B2
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- acid
- distillation
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- polyols
- polyurethane dispersion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0828—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing sulfonate groups or groups forming them
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0838—Manufacture of polymers in the presence of non-reactive compounds
- C08G18/0842—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents
- C08G18/0861—Manufacture of polymers in the presence of non-reactive compounds in the presence of liquid diluents in the presence of a dispersing phase for the polymers or a phase dispersed in the polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
- C08G18/3231—Hydrazine or derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/82—Post-polymerisation treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G85/00—General processes for preparing compounds provided for in this subclass
- C08G85/002—Post-polymerisation 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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/05—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media from solid polymers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C243/00—Compounds containing chains of nitrogen atoms singly-bound to each other, e.g. hydrazines, triazanes
- C07C243/10—Hydrazines
- C07C243/12—Hydrazines having nitrogen atoms of hydrazine groups bound to acyclic carbon atoms
- C07C243/16—Hydrazines having nitrogen atoms of hydrazine groups bound to acyclic carbon atoms of an unsaturated carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G71/00—Macromolecular compounds obtained by reactions forming a ureide or urethane link, otherwise, than from isocyanate radicals in the main chain of the macromolecule
- C08G71/04—Polyurethanes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Dispersion Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Description
R3はアルコキシ末端ポリエチレンオキシド基である)
も含む。
粗分散液を以下のように調製した:ポリエステルポリオールおよび400g/mol未満のモル質量を有するさらなるポリオールを重合反応器に入れ、70℃に加熱した。次いで、ポリイソシアネート混合物を計量導入し、内部反応器温度を100℃に上昇させた。4.47重量%の理論NCO値に達するまで反応混合物を100℃で撹拌した。次いで、得られたイソシアネート官能性プレポリマーを60℃に冷却し、アセトンに溶解した。アセトンに完全に溶解した後、プレポリマー溶液を蒸留反応器に移し、40℃でアミノエチルアミノエタンスルホン酸のナトリウム塩と鎖延長のためのヒドラジンとの混合物の水溶液を撹拌しながら添加し、次いで、混合物をさらに15分間撹拌した。最後に、水分散を行った。わずかに乳白色のポリウレタン粗分散液は、pH6.9および23.8重量%の固形分を有していた。
粗分散液を蒸留反応器中で40℃に加熱した。その後真空を適用し、120mbarまで段階的に低下した。120mbarに達した後、底部温度および蒸気温度も連続的に上昇した。48.5℃の蒸気温度に達すると、分散液のアセトン含有量は1重量%未満であり、蒸留を終了した。
粗分散液を蒸留反応器中で40℃に加熱した。その後真空を適用し、120mbarまで段階的に低下した。120mbarに達した後、底部温度および蒸気温度も連続的に上昇した。
Claims (6)
- ポリウレタン分散液からケタジンを除去する方法であって、前記ポリウレタン分散液の蒸留工程を含み、ここで、蒸気温度は53℃以下であり、前記蒸留が120hPa~140hPaの圧力で行われ、前記蒸気温度は51℃に達し、そして、前記蒸留終了後の前記ポリウレタン分散液のケタジン含有量が1000ppm未満である、方法。
- 底部の温度が53℃以下である、請求項1に記載の方法。
- 底部の温度が45℃以下で前記蒸留が開始され、前記底部の温度が最大53℃になるまで継続される、請求項2に記載の方法。
- 底部の温度が48℃に達した後、少なくとも2時間前記蒸留が継続される、請求項1~3のいずれかに記載の方法。
- 前記ポリウレタン分散液が、アセトンおよび水を含む、請求項1~4のいずれかに記載の方法。
- 前記ポリウレタンが、プレポリマーをヒドラジンで鎖延長することによって構成される、請求項1~5のいずれかに記載の方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP16176762.9 | 2016-06-28 | ||
EP16176762.9A EP3263627B1 (de) | 2016-06-28 | 2016-06-28 | Destillative abtrennung von ketazin aus polyurethandispersionen |
PCT/EP2017/065880 WO2018002067A1 (de) | 2016-06-28 | 2017-06-27 | Destillative abtrennung von ketazin aus polyurethandispersionen |
Publications (3)
Publication Number | Publication Date |
---|---|
JP2019519654A JP2019519654A (ja) | 2019-07-11 |
JPWO2018002067A5 JPWO2018002067A5 (ja) | 2022-01-20 |
JP7098540B2 true JP7098540B2 (ja) | 2022-07-11 |
Family
ID=56321765
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP2018567874A Active JP7098540B2 (ja) | 2016-06-28 | 2017-06-27 | ポリウレタン分散液からのケタジンの蒸留分離 |
Country Status (8)
Country | Link |
---|---|
US (1) | US11511211B2 (ja) |
EP (2) | EP3263627B1 (ja) |
JP (1) | JP7098540B2 (ja) |
KR (1) | KR102422483B1 (ja) |
CN (1) | CN109312078B (ja) |
ES (1) | ES2828359T3 (ja) |
TW (1) | TWI758299B (ja) |
WO (1) | WO2018002067A1 (ja) |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101565494A (zh) | 2009-06-05 | 2009-10-28 | 天津博苑高新材料有限公司 | 水性阳离子聚氨酯热熔胶预聚体及其乳液的生产方法 |
Family Cites Families (16)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE2446440C3 (de) | 1974-09-28 | 1981-04-30 | Bayer Ag, 5090 Leverkusen | Verfahren zur Herstellung von wäßrigen Dispersionen von Sulfonatgruppen aufweisenden Polyurethanen |
DE19750186A1 (de) | 1997-11-13 | 1999-05-20 | Bayer Ag | Hydrophilierungsmittel, ein Verfahren zu dessen Herstellung sowie dessen Verwendung als Dispergator für wäßrige Polyurethan-Dispersionen |
DE10138765A1 (de) | 2001-08-07 | 2003-02-20 | Bayer Ag | Wässrige Dispersionen hydrophiler Polyurethanharze |
DE10254119A1 (de) | 2001-12-03 | 2003-06-18 | Bayer Ag | Verfahren zur Extraktion von Ketazinlösungen |
EP1851259B1 (en) * | 2005-02-07 | 2018-04-11 | Lubrizol Advanced Materials, Inc. | Aqueous dispersions of polyurethane compositions |
DE102005019397A1 (de) * | 2005-04-25 | 2006-10-26 | Bayer Materialscience Ag | Polyurethan-Dispersionen mit verbesserten Verfilmungseigenschaften |
CN101189284B (zh) * | 2005-06-03 | 2011-12-21 | 三菱化学株式会社 | 水性树脂分散体及其制造方法、涂料和层积体 |
DE102006002156A1 (de) * | 2006-01-17 | 2007-07-19 | Bayer Materialscience Ag | Polyurethan-Polyharnstoff-Dispersionen auf Basis von Polyether-Polycarbonat-Polyolen |
EP2377895A1 (de) * | 2010-04-14 | 2011-10-19 | Bayer MaterialScience AG | Wässrige Polyurethanpolyharnstoff-Dispersionen |
JP5614105B2 (ja) * | 2010-05-28 | 2014-10-29 | 三菱瓦斯化学株式会社 | ケタジン及び水加ヒドラジンの製造方法 |
JP5864595B2 (ja) * | 2010-10-29 | 2016-02-17 | ルブリゾル アドバンスド マテリアルズ, インコーポレイテッド | 水性カチオン性ポリウレタン分散体 |
CN102070768B (zh) * | 2010-12-06 | 2012-10-03 | 安徽好思家涂料有限公司 | 一种木器漆用水性聚氨酯及其制备方法 |
JP2016513158A (ja) * | 2013-02-22 | 2016-05-12 | ビーエーエスエフ ソシエタス・ヨーロピアBasf Se | 水性ポリウレタン配合物の製造法 |
JP6164456B2 (ja) * | 2013-03-28 | 2017-07-19 | Dic株式会社 | ウレタン樹脂組成物、プライマー、積層体及び画像表示装置 |
CN105399067B (zh) * | 2015-10-27 | 2017-12-15 | 宜宾海丰和锐有限公司 | 一种提高酮连氮法水合肼蒸馏过程中酮连氮收率的方法 |
CN105347319B (zh) * | 2015-11-17 | 2017-09-26 | 宜宾海丰和锐有限公司 | 一种去除酮连氮法水合肼有机杂质的方法 |
-
2016
- 2016-06-28 EP EP16176762.9A patent/EP3263627B1/de active Active
- 2016-06-28 ES ES16176762T patent/ES2828359T3/es active Active
-
2017
- 2017-06-26 TW TW106121208A patent/TWI758299B/zh active
- 2017-06-27 JP JP2018567874A patent/JP7098540B2/ja active Active
- 2017-06-27 CN CN201780039742.7A patent/CN109312078B/zh active Active
- 2017-06-27 US US16/311,010 patent/US11511211B2/en active Active
- 2017-06-27 KR KR1020187037433A patent/KR102422483B1/ko active IP Right Grant
- 2017-06-27 WO PCT/EP2017/065880 patent/WO2018002067A1/de unknown
- 2017-06-27 EP EP17733818.3A patent/EP3475344A1/de not_active Withdrawn
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101565494A (zh) | 2009-06-05 | 2009-10-28 | 天津博苑高新材料有限公司 | 水性阳离子聚氨酯热熔胶预聚体及其乳液的生产方法 |
Also Published As
Publication number | Publication date |
---|---|
US20200306660A1 (en) | 2020-10-01 |
JP2019519654A (ja) | 2019-07-11 |
WO2018002067A1 (de) | 2018-01-04 |
TW201819478A (zh) | 2018-06-01 |
TWI758299B (zh) | 2022-03-21 |
KR102422483B1 (ko) | 2022-07-20 |
US11511211B2 (en) | 2022-11-29 |
EP3263627B1 (de) | 2020-08-12 |
EP3475344A1 (de) | 2019-05-01 |
CN109312078A (zh) | 2019-02-05 |
KR20190022555A (ko) | 2019-03-06 |
CN109312078B (zh) | 2022-03-01 |
EP3263627A1 (de) | 2018-01-03 |
ES2828359T3 (es) | 2021-05-26 |
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