CN1132870C - 通过连续加入起始物进行双金属氰化物催化多醇的制备 - Google Patents
通过连续加入起始物进行双金属氰化物催化多醇的制备 Download PDFInfo
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- CN1132870C CN1132870C CN97192141A CN97192141A CN1132870C CN 1132870 C CN1132870 C CN 1132870C CN 97192141 A CN97192141 A CN 97192141A CN 97192141 A CN97192141 A CN 97192141A CN 1132870 C CN1132870 C CN 1132870C
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- C—CHEMISTRY; METALLURGY
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2642—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the catalyst used
- C08G65/2645—Metals or compounds thereof, e.g. salts
- C08G65/2663—Metal cyanide catalysts, i.e. DMC's
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- 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
- C08G18/14—Manufacture of cellular products
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- 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
- C08G18/48—Polyethers
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- 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
- C08G18/48—Polyethers
- C08G18/4866—Polyethers having a low unsaturation value
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- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- 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
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2696—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds characterised by the process or apparatus used
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- 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
- C08G2110/00—Foam properties
- C08G2110/0008—Foam properties flexible
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- 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
- C08G2110/00—Foam properties
- C08G2110/0083—Foam properties prepared using water as the sole blowing agent
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- Polyethers (AREA)
- Polyurethanes Or Polyureas (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
Description
表1.使用DMC催化剂和连续加入起始物来制备聚醚多醇 | |||||||||||
实施例 | 初始加入的起始物(Si) | 连续加入的起始物(Sc) | PO中Sc的浓度(%(重量)) | 催化剂 | 催化剂含量(ppm) | 多醇物理特性OH 不饱和 粘度 峰MW Mn Mw/Mn | |||||
1 | 没有(甲苯) | 丙二醇 | 1.9 | Zn-Co“A” | 50 | 28.2 | 0.007 | 997 | 3080 | 2800 | 1.22 |
2 | 4K二醇 | 丙二醇 | 1.9 | Zn-Co“A” | 25 | 28.3 | 0.007 | 1040 | 3040 | 2750 | 1.21 |
3 | 8K二醇 | 水 | 0.20 | Zn-Co“B” | 25 | 13.5 | 0.007 | 3790 | 9400 | 8130 | 1.22 |
4 | 6K三醇 | 甘油 | 1.5 | Zn-Co“A” | 25 | 27.7 | 0.007 | 2210 | 4760 | 5070 | 1.26 |
5 | 2K二醇 | 丙二醇 | 3.8 | Zn-Co“A” | 25 | 56.2 | 0.007 | 380 | 2340 | 1880 | 1.16 |
C6 | 1.4K二醇 | 丙二醇 | 3.8 | KOH | 2500 | 64.2 | 0.052 | - | 330018301030 | 1790 | 1.31 |
Zn-Co”A”为六氰基钴酸锌/叔丁醇配合物催化剂,粉末,其制备如共同未决申请No.08/435,116中的实施例8-11描述。Zn-Co”B”为六氰基钴酸锌/叔丁醇/聚醚多醇配合物催化剂,其制备如US5,482,908中描述。 |
PO/起始物混合物在2-5小时内连续加入(参见实施例)。 |
表2.连续加入起始物:加入水的量对多醇性质的影响 | |||||||||||
实施例 | 初始加入的起始物(Si) | 连续加入的起始物(Sc) | PO中Sc的浓度(%(重量)) | 催化剂 | 催化剂含量(ppm) | 多醇物理特性OH 不饱和 粘度 峰MW Mn Mw/Mn | |||||
8 | 2K二醇 | 水 | 500 | Zn-Co“A” | 25 | 12.0 | 0.009 | 4090 | 4940 | 5790 | 1.51 |
9 | 2K二醇 | 水 | 250 | Zn-Co“A” | 25 | 15.1 | 0.010 | 4500 | 4910 | 5890 | 1.59 |
10 | 2K二醇 | 水 | 125 | Zn-Co“A” | 25 | 14.1 | 0.010 | 5000 | 4760 | 5860 | 1.73 |
C11 | 2K三醇 | 没有 | 0 | Zn-Co“A” | 25 | 14.4 | 0.011 | 9260 | 4150 | 5640 | 2.17 |
Zn-Co”A”为六氰基钴酸锌/叔丁醇配合物催化剂,粉末,其制备如共同未决No.08/435,116中的实施例8-11描述。PO/起始物混合物在1小时内连续加入。 |
表3.连续加入起始物:加入低含量的起始物对多醇性质的影响 | ||||||||
实施例 | 连续加入的起始物(Sc) | PO中Sc的浓度(%(重量)) | PO封端(%) | 进料时间(h) | 多醇物理性质泡沫体试验 凝胶泡沫 OH(mg KOH/g) 峰尾>100K mw,ppm) | |||
12 | 水 | 500 | 25 | 6 | 通过 | 否 | 51.7 | 180 |
13 | 水 | 200 | 25 | 6 | 通过 | 否 | 52.6 | 180 |
14 | 丙二醇 | 2900 | 25 | 3 | 通过 | 否 | 52.8 | 144 |
15 | 丙二醇 | 1760 | 25 | 3 | 通过 | 否 | 51.5 | 300 |
C16 | 没有 | 0 | 25 | 6 | 失败 | 是 | 51.7 | 396 |
C17 | 没有 | 0 | 25 | 3 | 失败 | 是 | 51.8 | 648 |
详细的临界泡沫体试验显示在实施例B中。峰尾为Mn>100,000的多醇,由凝胶渗透色谱测定(参见实施例A)。 |
Claims (10)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US08/597,781 US5777177A (en) | 1996-02-07 | 1996-02-07 | Preparation of double metal cyanide-catalyzed polyols by continuous addition of starter |
US08/597,781 | 1996-02-07 |
Publications (2)
Publication Number | Publication Date |
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CN1210549A CN1210549A (zh) | 1999-03-10 |
CN1132870C true CN1132870C (zh) | 2003-12-31 |
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Application Number | Title | Priority Date | Filing Date |
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CN97192141A Expired - Lifetime CN1132870C (zh) | 1996-02-07 | 1997-02-01 | 通过连续加入起始物进行双金属氰化物催化多醇的制备 |
Country Status (19)
Country | Link |
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US (2) | US5777177A (zh) |
EP (1) | EP0879259B2 (zh) |
JP (2) | JP4538103B2 (zh) |
KR (1) | KR100509341B1 (zh) |
CN (1) | CN1132870C (zh) |
AR (1) | AR005711A1 (zh) |
AU (1) | AU720298B2 (zh) |
BR (1) | BR9706971A (zh) |
CA (1) | CA2245563C (zh) |
CZ (1) | CZ292400B6 (zh) |
DE (1) | DE69705605T3 (zh) |
ES (1) | ES2158490T5 (zh) |
ID (1) | ID15891A (zh) |
MX (1) | MX9805940A (zh) |
PL (1) | PL186624B1 (zh) |
RU (1) | RU2191784C2 (zh) |
TW (1) | TW518345B (zh) |
WO (1) | WO1997029146A1 (zh) |
ZA (1) | ZA97987B (zh) |
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TW518345B (en) | 2003-01-21 |
KR19990072103A (ko) | 1999-09-27 |
JP2007277583A (ja) | 2007-10-25 |
CZ248198A3 (cs) | 1999-02-17 |
CA2245563C (en) | 2005-10-25 |
PL186624B1 (pl) | 2004-02-27 |
PL328018A1 (en) | 1999-01-04 |
US5777177A (en) | 1998-07-07 |
ES2158490T3 (es) | 2001-09-01 |
CZ292400B6 (cs) | 2003-09-17 |
EP0879259B1 (en) | 2001-07-11 |
ES2158490T5 (es) | 2006-12-01 |
MX9805940A (es) | 1998-11-30 |
JP4538103B2 (ja) | 2010-09-08 |
AR005711A1 (es) | 1999-07-14 |
CN1210549A (zh) | 1999-03-10 |
ZA97987B (en) | 1997-08-18 |
KR100509341B1 (ko) | 2006-01-27 |
EP0879259A1 (en) | 1998-11-25 |
BR9706971A (pt) | 1999-04-06 |
DE69705605T2 (de) | 2001-11-08 |
AU720298B2 (en) | 2000-05-25 |
ID15891A (id) | 1997-08-14 |
EP0879259B2 (en) | 2006-04-12 |
RU2191784C2 (ru) | 2002-10-27 |
JP2000504753A (ja) | 2000-04-18 |
DE69705605T3 (de) | 2006-11-23 |
WO1997029146A1 (en) | 1997-08-14 |
CA2245563A1 (en) | 1997-08-14 |
AU1598397A (en) | 1997-08-28 |
US5919988A (en) | 1999-07-06 |
DE69705605D1 (de) | 2001-08-16 |
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