CN108070082A - It is a kind of to prepare the method compared with low viscosity high molecular weight polyether - Google Patents
It is a kind of to prepare the method compared with low viscosity high molecular weight polyether Download PDFInfo
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- CN108070082A CN108070082A CN201611024230.7A CN201611024230A CN108070082A CN 108070082 A CN108070082 A CN 108070082A CN 201611024230 A CN201611024230 A CN 201611024230A CN 108070082 A CN108070082 A CN 108070082A
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- polyether polyol
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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
- 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
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
- C08G65/3311—Polymers modified by chemical after-treatment with organic compounds containing oxygen containing a hydroxy group
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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
- 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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- 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
- 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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- 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
- 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
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/331—Polymers modified by chemical after-treatment with organic compounds containing oxygen
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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- General Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Polyethers (AREA)
Abstract
The present invention relates to polyether polyol technical field, more particularly to a kind of method for preparing polyether polyol.Described method includes following steps：1）Initial initiator, non-activated multi-metal cyanide complex catalyst and Bronsted acid are added in reaction kettle, inert gas is passed through after heating and carries out bubbling degassing；2）It is passed through inert gas again into reaction kettle so that the pressure in reaction kettle is in positive pressure；3）Epoxides is added in, triggers multi-metal cyanide complex catalyst；4）Epoxides and low molecule weight initiator are added in, polymerisation occurs；5）Aging, vacuum outgas is to get to the polyether polyol.The present invention catalyzes and synthesizes the high molecular weight polyether compared with low viscosity using batch process, multi-metal cyanide complex catalyst, by controlling the polymerization rate of epoxides and being continuously added to the method for low molecule weight initiator so that the viscosity of polyether polyol is in reduced levels.
Description
Technical field
The present invention relates to polyether polyol technical field, more particularly to it is a kind of prepare it is more compared with low viscosity high molecular weight polyether
The method of first alcohol.
Background technology
Polyether polyol is catalyzed and synthesized using MMC (DMC), the polyether polyol usually prepared has that degree of unsaturation is low, molecule
The advantages that measuring narrowly distributing, but there is also super high molecular weight trailing phenomenon.Due to the presence of ultra high molecular weight material, cause making
During for compared with high equivalent weight molecular weight, the viscosity of polyether polyol steeply rises, and the later stage for limiting polyether polyol uses.
Catalyzing and synthesizing polyether polyol technique using MMC (DMC) mainly has batch process and continuous hair technique.Batch process produces
The technological process of technique is simple, more can flexibly and effectively control yield as needed.Compared with batch process, continuity method work
Skill is more suitable for producing substantial amounts of polyether polyol.It is mainly interval that current country MMC (DMC), which catalyzes and synthesizes polyether polyol technique,
Method production technology.
In general, in terms of being chiefly used in elastomeric material using the polyethers that MMC (DMC) catalyst synthesizes, to poly- during use
The viscosity of ethoxylated polyhydric alcohol has higher requirement, and for high molecular weight polyether, relatively low viscosity can make this poly-
Ethoxylated polyhydric alcohol more easily operates in use, it is desirable on the premise of polyether polyol molecular weight is ensured as far as possible
Reduce its viscosity.
The content of the invention
In view of the foregoing deficiencies of prior art, prepared it is an object of the invention to provide a kind of compared with low viscosity macromolecule
The method for measuring polyether polyol.It the described method comprises the following steps：1) by initial initiator, non-activated multi-metal cyanide network
Mixture catalyst and Bronsted acid are added in reaction kettle, and inert gas is passed through after heating and carries out bubbling degassing；2) into reaction kettle
Inert gas is passed through again so that the pressure in reaction kettle is in positive pressure；3) epoxides is added in, urges multi-metal cyanide complex
Agent triggers；4) epoxides and low molecule weight initiator are added in, polymerisation occurs；5) aging, vacuum outgas is to get to described
Polyether polyol.The present invention synthesizes the high molecular weight polyether compared with low viscosity using batch process, MMC (DMC) catalyst
Polyalcohol, by controlling the polymerization rate of epoxides and being continuously added to the method for low molecule weight initiator so that polyethers
The viscosity of polyalcohol is in reduced levels.
In order to achieve the above objects and other related objects, the present invention provides a kind of method for preparing polyether polyol, including
Following steps：
1) initial initiator, non-activated multi-metal cyanide complex catalyst and Bronsted acid are added to reaction kettle
In, inert gas is passed through after heating and carries out bubbling degassing；
2) continue to be passed through inert gas into reaction kettle so that the pressure in reaction kettle is in positive pressure；
3) epoxides is added in, triggers multi-metal cyanide complex catalyst；
4) epoxides and low molecule weight initiator are added in, polymerisation occurs；
5) aging, vacuum outgas is to get to the polyether polyol.
The multi-metal cyanide complex catalyst is the multi-metal cyanide network in the patent No. 200910197582.6
Mixture catalyst.
Preferably, in step 1), the initial initiator is selected from polyoxypropylene propyleneglycol ether and polypropylene oxide the third three
At least one of alcohol ether, number-average molecular weight are 400~12000, and hydroxy functionality is 1~8.
Preferably, in step 1), it is warming up to after 95~105 DEG C and is passed through inert gas progress bubbling degassing again.
Preferably, in step 1), multi-metal cyanide complex catalyst is dense in final polyether polyol obtained
It spends for 5~100ppm；Concentration of the Bronsted acid in initial initiator is 5~300ppm.
Preferably, in step 2), relative pressure in reaction kettle is 0~0.4MPa, such as 0~0.05MPa, 0.05~
0.1MPa, 0.1~0.2MPa, 0.2~0.3MPa or 0.3~0.4MPa.
Preferably, in step 1) and step 2), the inert gas is in nitrogen, carbon dioxide, helium and argon gas
It is one or more.
Preferably, the epoxides for triggering multi-metal cyanide complex catalyst and initial initiator are added in step 3)
Molar ratio be 2~0.1：1.
Preferably, in step 4), low molecule weight initiator be selected from water, ethylene glycol, propylene glycol, dipropylene glycol, diethylene glycol and
One or more in glycerine, hydroxy functionality are 1~3.
Preferably, in step 3) and step 4), epoxides in propylene oxide, ethylene oxide and epoxy butane one
Kind is a variety of.
Preferably, in step 4), the temperature of polymerisation is 115~135 DEG C.
Preferably, in step 4), time of polymerisation is 10~14hr, such as 10~10.5hr, 10.5~11.5hr,
11.5~12.6hr, 12.6~13.5hr or 13.5~14hr.
The viscosity of the viscosity of polyether polyol prepared by the present invention and polyether polyol made from tradition DMC (MMC) technique
Decline to a great extent compared to having, generally use DMC (MMC) catalyst synthetic molecular weight be 12000 polyether polyol viscosity about
For 25000mPa.s or so, and it is only 6200mPa.s or so to use this method viscosity obtained with molecular weight polyether polyol,
The viscosity for the polyether polyol that synthetic molecular weight is 26714 is 15510mPa.s, under having significantly than the viscosity in existing patent
Drop.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also be based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under the spirit of the present invention.
Required raw material：
Initial initiator：Two degree of functionality polyether polyol, (number-average molecular weight is by hydroxyl value 5~100mgKOH/g, GE-220A
2000), GSE-2028 (number-average molecular weight 4000) or GSE-2010 (number-average molecular weight 11220) etc., purchased from Sinopec
Shanghai Gaoqiao Petrochemical Company is polyoxypropylene propyleneglycol ether；
Low molecule weight initiator：Propylene glycol.Magnificent Chemical Group limited company is won completely purchased from Shandong stone；
Epoxides：Propylene oxide.Purchased from Shandong BinHua Group Co., Ltd；
Examples 1 to 8：Polyether polyol is prepared, is included the following steps：
(1) initial initiator, non-activated multi-metal cyanide complex catalyst (are used into the patent No.
Multi-metal cyanide complex catalyst in 200910197582.6 embodiments 1) and Bronsted acid mixing after, put into reaction kettle
In, it is passed through inert nitrogen gas progress bubbling degassing after being warming up to certain temperature (temperature of each embodiment is shown in Table 1A and table 1B)；
(2) continue to be passed through inert nitrogen gas into reaction kettle so that the pressure in reaction kettle is in positive pressure；
(3) a certain amount of propylene oxide is slowly added to, triggers multi-metal cyanide complex catalyst；
(4) be continuously added into reaction kettle metering propylene oxide and low molecule weight initiator (species of each embodiment is shown in Table
1A and table 1B), polymerisation occurs, the time of polymerisation is 10~14hr, until reaction terminates；
(5) after aging, vacuum outgas obtains polyether polyol.
The index of reaction condition and polyether polyol is shown in Table 1.
Comparative example 1：Polyether polyol is prepared, is included the following steps：
(1) initial initiator GE-220A, non-activated multi-metal cyanide complex catalyst and Bronsted acid are mixed
Afterwards, put into reaction kettle, inert nitrogen gas progress bubbling degassing is passed through after being warming up to certain temperature；
(2) propylene oxide is added in, triggers multi-metal cyanide complex catalyst；
(3) propylene oxide of metering is continuously added into reaction kettle, occurs polymerisation, time of polymerisation for 1~
4hr, until reaction terminates；
(4) after aging, vacuum outgas obtains polyether polyol.
The index of reaction condition and polyether polyol is shown in Table 1.
Table 1A
Table 1B
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (11)
- A kind of 1. method for preparing polyether polyol, which is characterized in that described method includes following steps：1) initial initiator, non-activated multi-metal cyanide complex catalyst and Bronsted acid are added in reaction kettle, risen Inert gas is passed through after temperature and carries out bubbling degassing；2) continue to be passed through inert gas into reaction kettle so that the pressure in reaction kettle is in positive pressure；3) epoxides is added in, triggers multi-metal cyanide complex catalyst；4) epoxides and low molecule weight initiator are added in, polymerisation occurs；5) aging, vacuum outgas is to get to the polyether polyol.
- 2. according to the method described in claim 1, it is characterized in that, in step 1), the initial initiator is selected from polyoxygenated third At least one of allyl glycol ethers and polyoxypropylene glycerol ether, number-average molecular weight are 400~12000, hydroxy functionality For 1~8.
- 3. according to the method described in claim 1, it is characterized in that, in step 1), inertia is passed through again after being warming up to 95~105 DEG C Gas carries out bubbling degassing.
- 4. according to the method described in claim 1, it is characterized in that, in step 1), multi-metal cyanide complex catalyst exists Concentration in final polyether polyol obtained is 5~100ppm；Concentration of the Bronsted acid in initial initiator for 5~ 300ppm。
- 5. according to the method described in claim 1, it is characterized in that, in step 2), relative pressure in reaction kettle for 0~ 0.4MPa。
- 6. according to the method described in claim 1, it is characterized in that, in step 1) and step 2), the inert gas is selected from nitrogen One or more in gas, carbon dioxide, helium and argon gas.
- 7. according to the method described in claim 1, it is characterized in that, being added in step 3) multi-metal cyanide complex is triggered to urge The molar ratio of the epoxides of agent and initial initiator is 2~0.1：1.
- 8. according to the method described in claim 1, it is characterized in that, in step 4), low molecule weight initiator be selected from water, ethylene glycol, One or more in propylene glycol, dipropylene glycol, diethylene glycol and glycerine, hydroxy functionality are 1~3.
- 9. according to the method described in claim 1, it is characterized in that, in step 3) and step 4), epoxides is selected from epoxy third One or more in alkane, ethylene oxide and epoxy butane.
- 10. according to the method described in claim 1, it is characterized in that, in step 4), the temperature of polymerisation is 115~135 ℃。
- 11. according to the method described in claim 1, it is characterized in that, in step 4), the time of polymerisation is 10~14hr.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818889A (en) * | 2019-11-15 | 2020-02-21 | 山东蓝星东大有限公司 | Synthesis method of micromolecular polyether polyol with narrow molecular weight distribution |
| CN111518268A (en) * | 2020-05-28 | 2020-08-11 | 万华化学集团股份有限公司 | Preparation method of polyether polyol |
| CN112011042A (en) * | 2020-08-12 | 2020-12-01 | 上海抚佳精细化工有限公司 | Preparation method of high molecular weight low viscosity polyether polyol |
| CN114409889A (en) * | 2021-12-13 | 2022-04-29 | 山东一诺威新材料有限公司 | Method for reducing tailing of high molecular weight part in polyether polyol synthesized by DMC catalysis |
| CN115181259A (en) * | 2022-08-11 | 2022-10-14 | 万华化学集团股份有限公司 | Method for continuously preparing polyether |
| WO2024126551A1 (en) * | 2022-12-14 | 2024-06-20 | Shell Internationale Research Maatschappij B.V. | Batch process for preparing a polyether alcohol using a double metal cyanide catalyst |
| WO2024126550A1 (en) * | 2022-12-14 | 2024-06-20 | Shell Internationale Research Maatschappij B.V. | Batch process for preparing a polyether alcohol using a double metal cyanide catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110818889A (en) * | 2019-11-15 | 2020-02-21 | 山东蓝星东大有限公司 | Synthesis method of micromolecular polyether polyol with narrow molecular weight distribution |
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| CN114409889A (en) * | 2021-12-13 | 2022-04-29 | 山东一诺威新材料有限公司 | Method for reducing tailing of high molecular weight part in polyether polyol synthesized by DMC catalysis |
| CN115181259A (en) * | 2022-08-11 | 2022-10-14 | 万华化学集团股份有限公司 | Method for continuously preparing polyether |
| CN115181259B (en) * | 2022-08-11 | 2024-04-09 | 万华化学集团股份有限公司 | Method for continuously preparing polyether |
| WO2024126551A1 (en) * | 2022-12-14 | 2024-06-20 | Shell Internationale Research Maatschappij B.V. | Batch process for preparing a polyether alcohol using a double metal cyanide catalyst |
| WO2024126550A1 (en) * | 2022-12-14 | 2024-06-20 | Shell Internationale Research Maatschappij B.V. | Batch process for preparing a polyether alcohol using a double metal cyanide catalyst |
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