CN105885030A - Method for preparing low molecular weight distribution polyether - Google Patents

Method for preparing low molecular weight distribution polyether Download PDF

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Publication number
CN105885030A
CN105885030A CN201610490668.8A CN201610490668A CN105885030A CN 105885030 A CN105885030 A CN 105885030A CN 201610490668 A CN201610490668 A CN 201610490668A CN 105885030 A CN105885030 A CN 105885030A
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CN
China
Prior art keywords
low molecular
molecular weight
polyether
weight distribution
distribution
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
Application number
CN201610490668.8A
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Chinese (zh)
Inventor
应珏
翟洪金
郑磊
于文超
许家鹏
徐波涛
董胜
王传超
王成建
许谦
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Jurong Ningwu New Material Co Ltd
Original Assignee
Jurong Ningwu New Material Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Jurong Ningwu New Material Co Ltd filed Critical Jurong Ningwu New Material Co Ltd
Priority to CN201610490668.8A priority Critical patent/CN105885030A/en
Publication of CN105885030A publication Critical patent/CN105885030A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular 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
    • C08G65/2603Macromolecular 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
    • C08G65/2606Macromolecular 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular 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
    • C08G65/2642Macromolecular 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
    • C08G65/2645Metals or compounds thereof, e.g. salts
    • C08G65/2663Metal cyanide catalysts, i.e. DMC's
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G2101/00Manufacture of cellular products

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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)
  • Toxicology (AREA)
  • Polyethers (AREA)

Abstract

The invention discloses a method for preparing low molecular weight distribution polyether. The low molecular weight distribution polyether is prepared from the following raw materials: 8-10 parts of low molecular weight distribution polyether, Propylene oxide, lithium carbonate and 0.005% of a DMC catalyst. The method comprises the following steps: feeding the low molecular weight distribution polyether and the lithium carbonate into a reactor, dehydrating with nitrogen at 115-120 DEG C, after the moisture is qualified, adding the DMC catalyst, introducing epoxypropane, after epoxypropane is added, stirring for 1-3 hours to enable the system to react sufficiently, vacuuming, and cooling, thereby preparing the low molecular weight distribution polyether. By adopting the method, the use amount of the catalyst is small, the monomer conversion rate is high, and polymerization can be relatively stable.

Description

A kind of preparation method of distribution of low molecular weight polyethers
Technical field
The invention belongs to the preparation method of organic high molecular compound, specifically with a kind of new catalyst (DMC) Replace the preparation method of the distribution of low molecular weight polyethers of original base catalyst.
Background technology
Along with updating of PPG production technology, the quality of product is also improving constantly, but conventional polyether Industrialized production is always based on anionic catalytic ring-opening polymerisation, and in product, monohydroxy content of polyether is high, and molecular weight distribution is wider, Double bond content is higher, affects the mechanical and physical performance of polyurethane product.When polyol molecular weight increases, isomerization becomes particularly Significantly.There is presently no and be well solved.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of distribution of low molecular weight polyethers, use poly-ammonia prepared by this polyethers Ester foam can reduce the consumption of TDI, makes the elasticity of foam and comfortableness be improved.
It is an object of the invention to be achieved through the following technical solutions:
A kind of preparation method of distribution of low molecular weight polyethers, it is characterised in that: the method is with low molecular polyether as initiator; Dmc catalyst;Prepare with expoxy propane ring-opening polymerization;Comprise the steps:
1) preparing raw material, raw material weight number is low molecular polyether (molecular weight 800) 8-10;Dmc catalyst 0.04 ‰- 0.05‰;Expoxy propane 80-90;Lithium carbonate 0.01 ‰-0.03 ‰;
2) low molecular polyether, lithium carbonate are put in reactor;Then taken off by nitrogen stream at a temperature of 115-120 DEG C Water, after moisture content is qualified, adds dmc catalyst, is passed through expoxy propane, after expoxy propane adds end, stirs 1-3 hour, make body System's fully reaction, then vacuumizes, and prepares distribution of low molecular weight polyethers after cooling.
Moisture content is qualified refers to that moisture content mass fraction is less than 0.05%.
The distribution of low molecular weight polyethers that above-mentioned preparation method prepares is applied in polyurethane foam.
Distribution of low molecular weight polyethers prepared by the present invention causes PO ring-opening polymerisation, synthesis by using DMC complex catalyst Molecule is regular good, steady quality, and cost performance is high, and preparation polyurethane foam can reduce the consumption of TDI, and makes the bullet of foam Property and comfortableness are improved.
Catalyst amount of the present invention is little, and monomer conversion is high, is polymerized more stable.
Detailed description of the invention
Below by specific embodiment, the present invention is further illustrated, but each embodiment is not the tool to the present invention Body limits.
Embodiment 1
The preparation method of a kind of distribution of low molecular weight polyethers, with low molecular polyether as initiator;Dmc catalyst;With epoxy third Prepared by alkane ring-opening polymerization.Comprise the steps:
1. raw material weight number: low molecular polyether (self-control, molecular weight 800) 8;Dmc catalyst 0.05 ‰ (the permanent auspicious public affairs in Huayin Department);Expoxy propane 90(Jiangsu You Lide Chemical Co., Ltd.).Lithium carbonate 0.01 ‰ (Shanghai is than outstanding company).
2. low molecular polyether, lithium carbonate are put in reactor, then by nitrogen stream at a temperature of 115-120 DEG C Dehydration, after moisture content is qualified (moisture content is qualified refers to that moisture content mass fraction is less than 0.05%), adds dmc catalyst, is passed through epoxy third Alkane, after expoxy propane adds end, stirs 1-3 hour, makes system fully react, then vacuumize, and prepares low molecule after cooling Amount distribution polyethers.
Embodiment 2
The preparation method of a kind of distribution of low molecular weight polyethers, with low molecular polyether as initiator;Dmc catalyst;With epoxy third Prepared by alkane ring-opening polymerization.Comprise the steps:
1. raw material weight number: low molecular polyether (self-control, molecular weight 800) 10;Dmc catalyst 0.04 ‰ (the permanent auspicious public affairs in Huayin Department);Expoxy propane 90(Jiangsu You Lide Chemical Co., Ltd.).Lithium carbonate 0.02 ‰ (Shanghai is than outstanding company).
2. low molecular polyether, lithium carbonate are put in reactor, then by nitrogen stream at a temperature of 115-120 DEG C Dehydration, after moisture content is qualified, adds dmc catalyst, is passed through expoxy propane, after expoxy propane adds end, stirs 1-3 hour, make System is fully reacted, and then vacuumizes, and prepares polyethers after cooling.
Embodiment 3
The application of the distribution of low molecular weight polyethers that above-mentioned preparation method prepares, takes polyether polyol for polyurethane foam 100 parts, silicon Oil 2 parts, triethylene diamine catalyst 0.2 part, 3 parts of water, isocyanates 110 parts, high-speed stirred mixing post-foaming prepares polyurethane Foamed product.

Claims (3)

1. the preparation method of a distribution of low molecular weight polyethers, it is characterised in that: the method is with low molecular polyether as initiator; Dmc catalyst;Prepare with expoxy propane ring-opening polymerization;Comprise the steps:
1) preparing raw material, raw material weight number is low molecular polyether 8-10;Dmc catalyst 0.04 ‰-0.05 ‰;Expoxy propane 80-90;Lithium carbonate 0.01 ‰-0.03 ‰;
2) low molecular polyether, lithium carbonate are put in reactor;Then taken off by nitrogen stream at a temperature of 115-120 DEG C Water, after moisture content is qualified, adds dmc catalyst, is passed through expoxy propane, after expoxy propane adds end, stirs 1-3 hour, make body System's fully reaction, then vacuumizes, and prepares distribution of low molecular weight polyethers after cooling.
The preparation method of distribution of low molecular weight polyethers the most according to claim 1, it is characterised in that: moisture content is qualified refers to water Part mass fraction is less than 0.05%.
The preparation method of distribution of low molecular weight polyethers the most according to claim 1, it is characterised in that: low molecular polyether Molecular weight 800.
CN201610490668.8A 2016-06-29 2016-06-29 Method for preparing low molecular weight distribution polyether Pending CN105885030A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610490668.8A CN105885030A (en) 2016-06-29 2016-06-29 Method for preparing low molecular weight distribution polyether

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610490668.8A CN105885030A (en) 2016-06-29 2016-06-29 Method for preparing low molecular weight distribution polyether

Publications (1)

Publication Number Publication Date
CN105885030A true CN105885030A (en) 2016-08-24

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Country Status (1)

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CN (1) CN105885030A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112480390A (en) * 2020-11-30 2021-03-12 广东聚航新材料研究院有限公司 Antistatic agent for dicyclopentadiene resin and preparation method thereof
CN114456345A (en) * 2022-01-17 2022-05-10 江苏斯德瑞克化工有限公司 Flame-retardant polyether polyol and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101108896A (en) * 2006-07-20 2008-01-23 拜尔材料科学有限公司 High water content tolerant process for the production of polyethers
CN101967226A (en) * 2010-09-28 2011-02-09 山东蓝星东大化工有限责任公司 Method for synthesizing high-activity high molecular weight polyether polyalcohol
CN102574999A (en) * 2009-09-17 2012-07-11 旭硝子株式会社 Polyether preparation method
CN103360595A (en) * 2013-06-26 2013-10-23 淮安巴德聚氨酯科技有限公司 Method for shortening induction time during catalysis of ring opening polymerization of epoxide in discontinuous method
CN103694465A (en) * 2013-11-25 2014-04-02 黎明化工研究设计院有限责任公司 Continuous synthesis method of polyether

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101108896A (en) * 2006-07-20 2008-01-23 拜尔材料科学有限公司 High water content tolerant process for the production of polyethers
CN102574999A (en) * 2009-09-17 2012-07-11 旭硝子株式会社 Polyether preparation method
CN101967226A (en) * 2010-09-28 2011-02-09 山东蓝星东大化工有限责任公司 Method for synthesizing high-activity high molecular weight polyether polyalcohol
CN103360595A (en) * 2013-06-26 2013-10-23 淮安巴德聚氨酯科技有限公司 Method for shortening induction time during catalysis of ring opening polymerization of epoxide in discontinuous method
CN103694465A (en) * 2013-11-25 2014-04-02 黎明化工研究设计院有限责任公司 Continuous synthesis method of polyether

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112480390A (en) * 2020-11-30 2021-03-12 广东聚航新材料研究院有限公司 Antistatic agent for dicyclopentadiene resin and preparation method thereof
CN112480390B (en) * 2020-11-30 2023-05-09 广东聚航新材料研究院有限公司 Antistatic agent for dicyclopentadiene resin and preparation method thereof
CN114456345A (en) * 2022-01-17 2022-05-10 江苏斯德瑞克化工有限公司 Flame-retardant polyether polyol and preparation method thereof

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Application publication date: 20160824

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