CN115181259A - Method for continuously preparing polyether - Google Patents
Method for continuously preparing polyether Download PDFInfo
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- CN115181259A CN115181259A CN202210966793.7A CN202210966793A CN115181259A CN 115181259 A CN115181259 A CN 115181259A CN 202210966793 A CN202210966793 A CN 202210966793A CN 115181259 A CN115181259 A CN 115181259A
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- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 76
- 229920000570 polyether Polymers 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 77
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 229920005862 polyol Polymers 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 150000003077 polyols Chemical class 0.000 claims abstract description 39
- 239000000047 product Substances 0.000 claims abstract description 22
- 230000032683 aging Effects 0.000 claims abstract description 21
- 239000003999 initiator Substances 0.000 claims abstract description 20
- 230000006698 induction Effects 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 30
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 22
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 15
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 15
- 238000009826 distribution Methods 0.000 claims description 13
- 150000002924 oxiranes Chemical class 0.000 claims description 12
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 9
- 239000007858 starting material Substances 0.000 claims description 4
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 7
- 150000002118 epoxides Chemical class 0.000 abstract 2
- 239000002002 slurry Substances 0.000 description 30
- 239000007788 liquid Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 230000002431 foraging effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 229920002635 polyurethane Polymers 0.000 description 5
- 239000004814 polyurethane Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000010998 test method Methods 0.000 description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000001588 bifunctional effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
Abstract
The invention provides a method for continuously preparing polyether, which comprises the following steps: 1) Adding polyether polyol and DMC catalyst into a reaction kettle in advance, heating and raising the temperature, and introducing epoxide into the reaction kettle to perform induction reaction; 2) Continuously introducing epoxide, DMC catalyst and initiator into the reaction kettle for reaction after the catalyst induction reaction succeeds, allowing the reaction product to flow out of the kettle top and enter an aging kettle, and obtaining polyether after aging is completed; wherein the initiator is water or a mixture of water and a dihydric alcohol, and the addition amount of the initiator is controlled so that the average water content in the reaction system is not less than 0.01wt% and not more than 1.15wt%. The invention can greatly reduce the raw material cost in the polyether polyol production process by replacing all or part of the initiator with water, and can keep all indexes of the product consistent with those of the conventional process polyether.
Description
Technical Field
The invention belongs to the technical field of polyether polyol preparation, and particularly relates to a method for continuously preparing polyether, which can reduce production cost.
Background
Polyether polyol is an important chemical raw material, and polyurethane foam produced by using the polyether polyol is widely applied to the fields of furniture and household appliances, automobiles, aerospace, buildings, clothes, packaging and the like. Due to the characteristics of the polyether polyol industry, the polyether polyol productivity in the market is excessive, so that the polyether price is mainly influenced by the raw material price, the overall profit margin is low, and the raw material cost is reduced to become a development direction for improving profits of various polyether manufacturers.
The continuous production process generally adopts Double Metal Cyanide (DMC) catalyst for catalysis, has the advantages of high productivity, small occupied area, low cost and the like, is adopted by a plurality of companies in the world, and the productivity and the yield are gradually expanded. In polyether production, it is generally believed that moisture in the feedstock can reduce the activity of the DMC catalyst and even cause complete deactivation of the catalyst, and therefore, the moisture content of the feedstock can be tightly controlled in either batch or continuous polyether production processes. Chinese patent publication CN113087892A also reports that the degeneration of the catalyst by water is inhibited by adding an acid to protect the activity of the catalyst. However, in the actual production process, it is found that a small amount of moisture in the raw materials can react with the epoxide to generate polyether, and the cost of water as a bifunctional initiator is extremely low compared with that of the common micromolecule dihydric alcohol for polyether production, so that if water is used as the initiator to produce polyether polyol, the raw material cost can be greatly saved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for continuously preparing polyether polyol with low cost.
In order to achieve the purpose, the invention adopts the following technical scheme.
A method for continuously preparing polyether comprises the following steps:
1) Adding polyether polyol and Double Metal Cyanide (DMC) catalyst into a reaction kettle in advance, heating, introducing epoxide for induction reaction,
2) Continuously introducing epoxide, DMC catalyst and initiator into the reaction kettle for reaction after the catalyst induction reaction succeeds, allowing the reaction product to flow out of the kettle top and enter an aging kettle, and obtaining polyether after aging is completed;
wherein the initiator is water or a mixture of water and dihydric alcohol, and the addition amount of the initiator is controlled so that the average water content of a reaction system under continuous operation conditions is greater than or equal to 0.01wt% and less than or equal to 1.15wt%, and the average water content of the reaction system is the weight percentage of the water in the initiator converted to the total feed amount according to the feed proportion.
More preferably, the average water content in the reaction system is controlled within the following range in accordance with the concentration of the catalyst in the reaction system:
| catalyst concentration c, unit: ppm of | Water content, wt% |
| c≤15 | 0.01～0.15 |
| 15≤c＜30 | 0.15～0.30 |
| 30≤c＜60 | 0.30～0.45 |
| 60≤c＜100 | 0.45～0.65 |
| 100≤c＜200 | 0.65～0.85 |
| c≥200 | 0.85～1.15。 |
The average water content in the reaction system is the concentration of the water in the initiator converted to the total feeding amount according to the feeding proportion, and is not the water content value in the actually obtained polyether product.
Preferably, in the process, in step 1), the polyether polyol added beforehand has a hydroxyl value of from 20 to 280mg KOH/g, preferably from 40 to 120mg KOH/g.
Preferably, in step 1), the amount of catalyst added is relatively large and the concentration of DMC catalyst in the initially charged mass is from 20 to 5000ppm, preferably from 60 to 1000ppm.
Preferably, the reactor temperature is raised to 130 to 190 ℃, preferably 145 to 160 ℃.
Preferably, the epoxide is ethylene oxide, propylene oxide or a mixture of the two in any proportion.
Preferably, the epoxide is added in the induction reaction of step 1) in an amount of 1% to 5% by mass of the previously added polyether polyol.
The DMC catalyst is a conventional commercially available catalyst.
Preferably, in the method, in the step 2), the glycol is one or more mixture selected from the group consisting of ethylene glycol, propylene glycol, diethylene glycol and dipropylene glycol.
Preferably, in step 2), the ratio of epoxide and initiator added is controlled according to the hydroxyl value of the product of 20 to 168 mgKOH/g.
The catalyst concentration (c) in the reaction kettle refers to the catalyst concentration in the reaction system.
The epoxide, DMC catalyst and small molecule starter may be fed in a manner conventional in the art.
After the system is stable, the temperature of the reaction kettle and the aging kettle is 130-190 ℃, and the pressure is 0-1 MPa.
Preferably, the hydroxyl number of the polyether prepared according to the process of the present invention is from 20 to 168mg KOH/g.
Preferably, the viscosity of the polyether prepared according to the process of the present invention is 100 to 10000cP @25 ℃, more preferably 100 to 2000cP @25 ℃.
Preferably, the polyether prepared according to the process of the present invention has a molecular weight distribution of 1.00 to 2.00.
The invention has the following advantages:
by replacing the difunctional initiator with water completely or partially, the raw material cost in the polyether polyol production process can be greatly reduced, and all indexes of the product can be kept consistent with those of polyether in the conventional process. In addition, by controlling the water content under different conditions, the activity of the catalyst can be fully ensured, and the safe and stable operation of production equipment can be guaranteed.
Detailed Description
The method provided by the present invention is further illustrated by the following examples, but the present invention includes but is not limited to the examples listed, and also includes any other known variations within the scope of the claims of the present invention.
The product performance testing method comprises the following steps:
polyether polyol hydroxyl value test method reference: GB/T12008.3-2009
Polyether polyol viscosity test method reference: GB/T12008.7-2009
The polyether polyol molecular weight distribution test method adopts gel chromatography (GPC).
Example 1
(1) Preparation of catalyst slurry: 0.3g of DMC catalyst (Huaian Bade polyurethane science and technology Co., ltd.) was dispersed in advance into 1.5kg of polyether polyol (polyether base material, hydroxyl value 56 mgKOH/g) to prepare a catalyst slurry, and the catalyst slurry was added into a catalyst slurry tank.
(2) Induction reaction: 0.06g of DMC catalyst was dispersed in 1.5kg of polyether polyol (polyether base material, hydroxyl value 56mg KOH/g) to obtain a dispersion, and the dispersion was put into a 5L reactor, heated to 150 ℃ and introduced with 50g of propylene oxide.
(3) Polymerization reaction: when the pressure of the reaction kettle rapidly drops and the temperature rapidly rises to indicate that the catalyst is successfully activated, continuously feeding a mixture of propylene glycol and water (the water content is 10wt%, and the concentration is converted to be 0.247wt% in the reaction system), ethylene oxide, a propylene oxide mixture and catalyst slurry (the mass ratio of propylene glycol, water, propylene oxide, ethylene oxide and catalyst slurry is = 9: 1: 304.7: 33.9: 56.7), overflowing polyether polyol from the kettle top into an aging kettle for aging reaction after the reaction kettle is full of liquid, and overflowing the polyether polyol from the kettle top into a product storage tank after the aging kettle is full of liquid. During continuous and stable operation, the temperature of the reaction kettle is controlled to be 150 ℃, the pressure of the reaction kettle is controlled to be 0.4MPa, the concentration of the catalyst is controlled to be 28ppm, the residence time is controlled to be 2 hours, and finally the hydroxyl value of the product is 56.12mgKOH/g, the viscosity is 360cP (25 ℃), and the molecular weight distribution is 1.20.
Comparative example 1
Based on example 1, under otherwise identical conditions, the starter was fed in the desired ratio using propylene glycol, giving a product having a hydroxyl number of 56.03mgKOH/g and a viscosity of 355cP (25 ℃ C.), and a molecular weight distribution of 1.21.
Example 2
(1) Preparation of catalyst slurry: 0.75g of DMC catalyst (Huaian Bade polyurethane science and technology Co., ltd.) was dispersed in advance into 1.5kg of polyether polyol (polyether substrate, hydroxyl value 112 mgKOH/g) to prepare a catalyst slurry, and the catalyst slurry was added into a catalyst slurry tank.
(2) Induction reaction: 0.25g of DMC catalyst was dispersed in 2.5kg of polyether polyol (polyether base material, hydroxyl value 112 mgKOH/g) to obtain a dispersion, and the dispersion was put into a 5L reactor, heated to 150 ℃ and introduced with 50g of propylene oxide.
(3) Polymerization reaction: when the pressure of the reaction kettle rapidly decreases and the temperature rapidly rises, the catalyst is successfully activated, then a mixture of ethylene glycol and water (the water content is 17wt% and the concentration is converted to be 0.63wt% in the reaction system), propylene oxide and catalyst slurry (the mass ratio of ethylene glycol, water, propylene oxide and catalyst slurry is = 83: 17: 2187.2: 403.6) are continuously fed (the target hydroxyl value is 112 mgKOH/g), polyether polyol overflows from the top of the reaction kettle to the aging kettle for aging reaction after the reaction kettle is full of liquid, and the polyether polyol overflows from the top of the aging kettle to a product storage tank after the aging kettle is full of liquid. During the continuous and stable operation, the temperature of the reaction kettle is controlled to be 180 ℃, the pressure of the reaction kettle is controlled to be 0.5MPa, the concentration of the catalyst is controlled to be 75ppm, the residence time is 4 hours, and the hydroxyl value of the product is finally 111.45mgKOH/g, the viscosity is 160cP (25 ℃), and the molecular weight distribution is 1.25.
Comparative example 2
Based on example 2, the initiator was ethylene glycol fed in the required proportions under otherwise identical conditions, giving a product with a hydroxyl number of 111.87mgKOH/g, a viscosity of 162cP (25 ℃) and a molecular weight distribution of 1.24.
Example 3
(1) Preparation of catalyst slurry: 0.45g of DMC catalyst (Huaian Bade polyurethane science and technology Co., ltd.) was dispersed in advance into 1.5kg of polyether polyol (polyether substrate, hydroxyl value 28 mgKOH/g) to prepare a catalyst slurry, and the catalyst slurry was added into a catalyst slurry tank.
(2) Induction reaction: 0.25g of DMC catalyst was dispersed in 2.5kg of polyether polyol (polyether substrate, hydroxyl value 28 mgKOH/g) to obtain a dispersion, which was then put into a 5L reactor, heated to 170 ℃ and introduced with 30g of propylene oxide.
(3) Polymerization reaction: when the pressure of the reaction kettle rapidly decreases and the temperature rapidly rises, the catalyst is successfully activated, then, continuously (the target hydroxyl value is 28 mgKOH/g) feeding water (the weight ratio of the water to the propylene oxide to the catalyst slurry is = 1: 221.6: 30.9) feeding water, propylene oxide and the catalyst slurry, after the reaction kettle is full of liquid, the polyether polyol overflows from the kettle top to the aging kettle for aging reaction, and after the aging kettle is full of liquid, the polyether polyol overflows from the kettle top of the aging kettle and enters a product storage tank. During the continuous and stable operation, the temperature of the reaction kettle is controlled to be 180 ℃, the pressure of the reaction kettle is controlled to be 0.5MPa, the concentration of the catalyst is controlled to be 36.6ppm, the residence time is controlled to be 6 hours, and finally the hydroxyl value of the product is 28.23mgKOH/g, the viscosity is 950cP (25 ℃), and the molecular weight distribution is 1.16.
Comparative example 3
Based on example 3, under otherwise identical conditions, the starter was fed in the desired proportions using diethylene glycol, giving a product with a hydroxyl number of 28.05mgKOH/g and a viscosity of 940cP (25 ℃ C.) and a molecular weight distribution of 1.24.
Example 4
(1) Preparation of catalyst slurry: 3g of DMC catalyst (Huaian polyurethane technology Co., ltd.) was dispersed in 1.5kg of polyether polyol (polyether base, hydroxyl value 47 mgKOH/g) in advance to prepare a catalyst slurry, and the catalyst slurry was added to a catalyst slurry tank.
(2) Induction reaction: 1.5g of DMC catalyst was dispersed in 2.5kg of polyether polyol (polyether base material, hydroxyl value 47 mgKOH/g) to obtain a dispersion, which was then charged into a 5L reactor, heated to 140 ℃ and charged with 60g of propylene oxide for induction.
(3) Polymerization reaction: when the pressure of the reaction kettle rapidly decreases and the temperature rapidly rises, the catalyst is successfully activated, then diethylene glycol and water (the concentration is 1.14wt% converted to the concentration of the reaction system), a mixture of propylene oxide and ethylene oxide (the ethylene oxide accounts for 20 wt%) and catalyst slurry (the mass ratio of diethylene glycol to water to propylene oxide to ethylene oxide to catalyst slurry is = 2: 1: 57.2: 14.3: 13.1) are continuously fed according to the required ratio (the target hydroxyl value is 47 mgKOH/g), polyether polyol overflows from the kettle top to the aging kettle for aging reaction after the reaction kettle is full of liquid, and the polyether polyol overflows from the kettle top to a product storage tank after the aging kettle is full of liquid. During continuous and stable operation, the temperature of the reaction kettle is controlled to be 140 ℃, the pressure of the reaction kettle is controlled to be 0.3MPa, the concentration of the catalyst is controlled to be 299ppm, the residence time is controlled to be 8 hours, and finally the hydroxyl value of the product is 112.20mgKOH/g, the viscosity is 180cP (25 ℃), and the molecular weight distribution is 1.19.
Comparative example 4
Based on example 4, under otherwise identical conditions, dipropylene glycol was used as the initiator and fed in the desired proportions to give a product having a hydroxyl value of 112.11mgKOH/g and a viscosity of 184cP (25 ℃ C.), and a molecular weight distribution of 1.20.
Example 5
(1) Preparation of catalyst slurry: 1.5g of DMC catalyst (Huaian Bade polyurethane science and technology Co., ltd.) was dispersed in 1.5kg of polyether polyol (polyether substrate, hydroxyl value 23 mgKOH/g) in advance to prepare a catalyst slurry, and the catalyst slurry was added into a catalyst slurry tank.
(2) Induction reaction: 2.5g of DMC catalyst was dispersed in 2.5kg of polyether polyol (polyether base material, hydroxyl value 23 mgKOH/g) to obtain a dispersion, and the dispersion was put into a 5L reactor, heated to 160 ℃ and introduced with 40g of propylene oxide.
(3) Polymerization reaction: when the pressure of the reaction kettle rapidly decreases and the temperature rapidly rises, the catalyst is successfully activated, then the water (converted to the concentration of the reaction system of 0.35 wt%) and the ethylene oxide and the catalyst slurry (the mass ratio of the water to the ethylene oxide to the catalyst slurry is = 1: 270.0: 12.9) are continuously fed according to the required proportion (the target hydroxyl value is 23 mgKOH/g), the polyether polyol overflows from the kettle top to the aging kettle for aging reaction after the reaction kettle is full of liquid, and the polyether polyol overflows from the kettle top of the aging kettle and enters a product storage tank after the aging kettle is full of liquid. During continuous and stable operation, the temperature of the reaction kettle is controlled at 160 ℃, the pressure of the reaction kettle is controlled at 0.4MPa, the concentration of the catalyst is controlled at 45ppm, and the residence time is controlled at 6h, so that the hydroxyl value of the product is 22.86mgKOH/g, the viscosity is 205cP (60 ℃), and the molecular weight distribution is 1.26.
Comparative example 5
Based on example 5, under otherwise identical conditions, the initiator was ethylene glycol and fed in the desired proportions to give a product having a hydroxyl number of 22.99mgKOH/g and a viscosity of 215cP (25 ℃ C.), and a molecular weight distribution of 1.26.
In the invention, by using water or the mixture thereof, the raw material cost in the polyether polyol production process can be greatly reduced under the condition that all indexes of the product are consistent with those of conventional process polyether. In addition, the activity of the catalyst can be fully ensured by controlling the water content under different conditions, and the safe and stable operation of production equipment is ensured.
Claims (10)
1. A method for continuously preparing polyether comprises the following steps:
1) Adding polyether polyol and DMC catalyst into a reaction kettle in advance, heating, introducing epoxide for induction reaction,
2) Continuously introducing epoxide, DMC catalyst and initiator into the reaction kettle for reaction after the catalyst induction reaction succeeds, allowing the reaction product to flow out of the kettle top and enter an aging kettle, and obtaining polyether after aging is completed;
wherein the initiator is water or a mixture of water and dihydric alcohol, the addition amount of the initiator is controlled so that the average water content in the reaction system under the continuous operation condition is more than or equal to 0.01wt% and less than or equal to 1.15wt%, and the average water content in the reaction system is the weight percentage of the water in the initiator converted into the total feed amount according to the feed proportion.
2. The method according to claim 1, wherein the average water content in the reaction system is controlled within the following range in accordance with the concentration of the catalyst in the reaction system:
3. a process according to claim 1 or 2, wherein the pre-added polyether polyol has a hydroxyl number of from 20 to 280mg KOH/g, preferably from 40 to 120mg KOH/g.
4. A process according to any one of claims 1 to 3, wherein the DMC catalyst is added in step 1) in a concentration of 20 to 5000ppm, preferably 60 to 1000ppm;
preferably, the epoxide is added in the induction reaction of step 1) in an amount of 1% to 5% by mass of the previously added polyether polyol.
5. The process according to any one of claims 1 to 4, wherein in step 1) the reactor temperature is raised to 130 to 190 ℃, preferably 145 to 160 ℃.
6. The process of any one of claims 1 to 5, wherein the epoxide is ethylene oxide, propylene oxide or a mixture of the two in any proportion.
7. The method according to any one of claims 1 to 6, wherein the glycol is one or more mixtures selected from ethylene glycol, propylene glycol, diethylene glycol and dipropylene glycol.
8. A process as claimed in any one of claims 1 to 7, wherein the ratio of the epoxide to the starter is controlled in accordance with the hydroxyl number of the resulting polyether product being from 20 to 168 mgKOH/g.
9. The process according to any one of claims 1 to 8, wherein the temperature of the reaction vessel and the aging vessel in step 2) is 130 to 190 ℃ and the pressure is 0 to 1MPa.
10. The method of any one of claims 1 to 9,
the polyether prepared according to the method has a hydroxyl value of 20 to 168mgKOH/g,
preferably, the polyether prepared according to the process has a viscosity of 100 to 10000cP @25 ℃, more preferably 100 to 2000cP @25 ℃,
preferably, the molecular weight distribution of the polyether prepared according to the method is 1.00 to 2.00.
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