CN111533899A - Method for synthesizing high molecular weight pentaerythritol polyoxyethylene ether - Google Patents
Method for synthesizing high molecular weight pentaerythritol polyoxyethylene ether Download PDFInfo
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- CN111533899A CN111533899A CN202010449716.5A CN202010449716A CN111533899A CN 111533899 A CN111533899 A CN 111533899A CN 202010449716 A CN202010449716 A CN 202010449716A CN 111533899 A CN111533899 A CN 111533899A
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- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229920000056 polyoxyethylene ether Polymers 0.000 title claims abstract description 28
- 229940051841 polyoxyethylene ether Drugs 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 46
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229960000583 acetic acid Drugs 0.000 claims abstract description 23
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 23
- 150000001339 alkali metal compounds Chemical class 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims abstract description 15
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000007039 two-step reaction Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 86
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 42
- 229910052757 nitrogen Inorganic materials 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 238000007872 degassing Methods 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 16
- 238000005086 pumping Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 6
- VFFFESPCCPXZOQ-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;oxirane Chemical compound C1CO1.OCC(CO)(CO)CO VFFFESPCCPXZOQ-UHFFFAOYSA-N 0.000 claims 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 9
- 229920000570 polyether Polymers 0.000 description 9
- 238000010926 purge Methods 0.000 description 7
- 230000002045 lasting effect Effects 0.000 description 6
- 239000002904 solvent Substances 0.000 description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 230000004913 activation Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000007664 blowing Methods 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000000977 initiatory effect Effects 0.000 description 3
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
-
- 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
- C08G65/2648—Alkali metals or compounds thereof
Abstract
A high molecular weight pentaerythritol polyoxyethylene ether is prepared by taking pentaerythritol, an alkali metal compound, glacial acetic acid and ethylene oxide as raw materials through two-step reaction, and the method comprises the steps of feeding, replacing, feeding, curing, neutralizing, discharging and the like, and can be used for synthesizing the high molecular weight pentaerythritol polyoxyethylene ether, wherein the molecular weight of the pentaerythritol polyoxyethylene ether can reach 7000 plus 10000.
Description
Technical Field
The invention relates to the field of new materials synthesized by organic chemistry, in particular to a method for synthesizing high molecular weight pentaerythritol polyoxyethylene ether.
Background
The existing pentaerythritol polyoxyethylene ether synthesized by connecting ethylene oxide has low ethylene oxide number, and the maximum is not more than 100 (the molar ratio of pentaerythritol to ethylene oxide).
Meanwhile, the synthesis of the high molecular weight pentaerythritol polyoxyethylene ether only connects ethylene oxide and PO, the molecular weight of the pentaerythritol polyoxyethylene ether can only reach 4500-7500, and a single process of purely connecting ethylene oxide to 7000-10000 of high molecular weight is not available.
Amine catalysts (triethylamine, ammonia water and trimethylamine) are usually adopted in the synthesis of high molecular weight pentaerythritol polyoxyethylene ether at the present stage, so that byproducts are easy to produce, the chroma of the synthesized product is too deep, in addition, the process of adopting a solvent (ethylene glycol dimethyl ether) is too complex, and the solvent is difficult to recover and treat.
Disclosure of Invention
The invention aims to provide a method for synthesizing pentaerythritol polyoxyethylene ether with high molecular weight.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for synthesizing high molecular weight pentaerythritol polyoxyethylene ether is characterized in that pentaerythritol, alkali metal compounds, glacial acetic acid and ethylene oxide are used as raw materials to prepare the high molecular weight pentaerythritol polyoxyethylene ether through two-step reaction, and the method comprises the following steps:
the first step is as follows:
preparing materials, namely 15-17% of pentaerythritol, 0.5% of alkali metal compound, 82-84% of ethylene oxide and 0.5% of glacial acetic acid;
1) feeding, heating the kettle to 90-100 ℃, vacuumizing the kettle to negative pressure, feeding 0.5% of alkali metal compound and 15-17% of pentaerythritol;
2) performing replacement, namely pumping negative pressure to the reaction kettle, and introducing nitrogen to replace air in the kettle;
3) feeding, namely adding 82-84% of ethylene oxide into the reaction kettle twice;
4) curing, maintaining the reaction temperature in the reaction kettle at 115 ℃ and 125 ℃ for 1 h;
5) neutralizing, cooling and degassing the reaction kettle, adding 0.5% glacial acetic acid, and stirring for 30 min;
6) discharging, and collecting a reaction product A after the temperature is reduced to 50-60 ℃;
the second step is that:
preparing materials, wherein the reaction product A accounts for 10-12%, the alkali metal compound accounts for 0.8%, the ethylene oxide accounts for 86.5-89%, and the glacial acetic acid accounts for 0.7%;
1) feeding materials, maintaining the temperature of a reaction kettle at 30-50 ℃, pumping negative pressure by using a vacuum pump, feeding 10-12% of a reaction product A into the reaction kettle, stirring, and then feeding 0.8% of an alkali metal compound;
2) replacing, pumping negative pressure to the reaction kettle, and introducing nitrogen to replace air in the kettle;
3) heating for dehydration, and carrying out nitrogen drum dehydration for 1.5 h;
4) feeding ethylene oxide, adding 86.5-89% of ethylene oxide;
5) curing, maintaining the reaction temperature of 115 ℃ and 125 ℃ for 1 h;
6) neutralizing, cooling and degassing the reaction kettle, adding 0.7% glacial acetic acid, and stirring for 30 min;
7) discharging, cooling to 75-80 ℃, discharging, stopping stirring, and collecting to obtain the product, namely the high molecular weight pentaerythritol polyoxyethylene ether.
Further, the reaction temperature of the step 3) in the first step is 90-120 ℃, and the pressure in the reaction kettle is less than or equal to 350 kPa. The temperature of 90-120 ℃ is the optimum temperature for the reaction of the ethylene oxide in the step.
Further, the reaction temperature in the step 4) in the second step is 100-. 100 ℃ and 125 ℃ are the optimal temperature for the reaction of the ethylene oxide in the step.
Further, the storage barrel was purged with nitrogen for 20 seconds before the discharge was operated in step 6) of the first step. The effect of sealing with nitrogen is ensured, and the material is prevented from being polluted by air in subsequent storage to cause the color to become dark.
Further, in the second step, step 7) was performed by purging the storage tank with nitrogen for 20 seconds before the discharge was performed. The effect of sealing with nitrogen is ensured, and the material is prevented from being polluted by air in subsequent storage to cause the color to become dark.
Further, the alkali metal compound is potassium hydroxide.
Compared with the prior art, the invention has the beneficial effects that: the invention can synthesize high molecular weight pentaerythritol polyoxyethylene ether, and the molecular weight of the pentaerythritol polyoxyethylene ether can reach 7000-10000; the alkali metal compound is used as the catalyst, so that the generation of side reactants is reduced, and the economic benefit is improved; the adopted raw materials are few in variety, the solvent is not required to be recycled, and the production efficiency is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a diagram of the reaction equation of the present invention;
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments, not all embodiments, of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1: firstly, preparing materials, wherein the pentaerythritol content is 15%, the potassium hydroxide content is 0.5%, the ethylene oxide content is 84%, the glacial acetic acid content is 0.5%, vacuumizing the reaction kettle to-95 KPa at the temperature of 90 ℃ in the reaction kettle, adding 0.5% of potassium hydroxide, stirring, adding 15% of pentaerythritol into the kettle by utilizing negative pressure, pumping the negative pressure of the reaction kettle to-95 KPa after the feeding is finished, replacing nitrogen gas in the reaction kettle for 4 times, pressurizing to ensure that the air pressure of the reaction kettle reaches-50 KPa, controlling the temperature of the reaction kettle to be 80 ℃, adding 2.8% of ethylene oxide, heating to 90 ℃, initiating a reaction activation period, continuously adding 81.2% of ethylene oxide into the kettle, gradually increasing the temperature from 90 ℃ to 120 ℃ in the feeding process, controlling the temperature of the reaction kettle to not increase any more, keeping the pressure in the kettle not to exceed 350KPa, keeping the reaction temperature to be 115 ℃ for curing after the feeding is finished, lasting for 1h, cooling to 90 ℃ after curing, performing degassing operation, adding 0.5% glacial acetic acid after degassing, stirring for 30min, cooling to 50 ℃, purging a storage barrel with nitrogen for 20 seconds, discharging into the storage barrel, and collecting the synthetic pentaerythritol polyether;
secondly, preparing materials, namely 10% pentaerythritol polyether, 0.8% potassium hydroxide, 89% ethylene oxide and 0.7% glacial acetic acid, vacuumizing the reaction kettle to-95 KPa at the temperature of 30 ℃ in the reaction kettle, adding 10% pentaerythritol polyether, stirring, adding 0.8% potassium hydroxide into the kettle, pumping negative pressure to-95 KPa in the reaction kettle after the feeding is finished, heating the reaction kettle to 100 ℃, blowing nitrogen into the reaction kettle for dehydration for 1.5h to ensure that the air pressure of the reaction kettle reaches-60 KPa and 89% ethylene oxide is added, gradually increasing the temperature from 100 ℃ to 125 ℃ in the feeding process, controlling the temperature of the reaction kettle not to rise any more and the pressure of the kettle not to exceed 400KPa, finishing the feeding, maintaining the temperature of the reaction kettle at 115 ℃ for curing, lasting for 1h, curing, performing degassing operation, finishing the degassing operation, reducing the temperature to 80 ℃, adding 0.7% glacial acetic acid, stirring for 30min, cooling the temperature of the reaction kettle to 75 ℃, purging the storage barrel with nitrogen for 20 seconds, discharging the materials into the storage barrel, and collecting the high molecular weight pentaerythritol polyoxyethylene ether product.
Example 2: preparing materials, wherein the pentaerythritol content is 17%, the potassium hydroxide content is 0.5%, the ethylene oxide content is 82%, the glacial acetic acid content is 0.5%, vacuumizing the reaction kettle to-95 KPa at the temperature of 90 ℃ in the reaction kettle, adding 0.5% of potassium hydroxide, stirring, adding 17% of pentaerythritol into the kettle by utilizing negative pressure, after the feeding is finished, vacuumizing the reaction kettle to-95 KPa, replacing nitrogen at the top of the reaction kettle for 4 times, pressurizing to enable the air pressure of the reaction kettle to reach-50 KPa, controlling the temperature of the reaction kettle to be 80 ℃, adding 2.8% of ethylene oxide, heating to 90 ℃, initiating a reaction activation period, continuously adding 79.2% of ethylene oxide into the kettle, gradually increasing the temperature from 90 ℃ to 120 ℃ in the feeding process, controlling the temperature of the reaction kettle to be not increased, keeping the pressure in the kettle to be not higher than 350KPa, keeping the reaction temperature to be 115 ℃ for curing, lasting for 1h, cooling to 90 ℃ after curing, performing degassing operation, adding 0.5% glacial acetic acid after degassing, stirring for 30min, cooling to 50 ℃, purging a storage barrel with nitrogen for 20 seconds, discharging into the storage barrel, and collecting the synthetic pentaerythritol polyether;
secondly, preparing materials, namely 12% pentaerythritol polyether, 0.8% potassium hydroxide, 86.5% ethylene oxide and 0.7% glacial acetic acid, vacuumizing the reaction kettle to-95 KPa at the temperature of 30 ℃ in the reaction kettle, adding 12% pentaerythritol polyether, stirring, adding 0.8% potassium hydroxide into the kettle, pumping negative pressure to-95 KPa in the reaction kettle after the feeding is finished, heating the reaction kettle to 100 ℃, blowing nitrogen into the reaction kettle for dehydration for 1.5h to ensure that the air pressure of the reaction kettle reaches-60 KPa, controlling the temperature of the reaction kettle to 100 ℃, adding 86.5% ethylene oxide, gradually increasing the temperature from 100 ℃ to 125 ℃ in the feeding process, then controlling the temperature of the reaction kettle not to rise any more, ensuring that the air pressure in the kettle cannot exceed 400KPa, finishing the feeding, maintaining the degassing temperature of the reaction kettle to 115 ℃ for curing, lasting for 1h, and performing operation after the curing is finished, and after degassing, cooling to 80 ℃, adding 0.7% glacial acetic acid, stirring for 30min, cooling the temperature of the reaction kettle to 75 ℃, purging the storage barrel for 20 seconds by nitrogen, discharging into the storage barrel, and collecting to obtain the high molecular weight pentaerythritol polyoxyethylene ether product.
Example 3: firstly, preparing materials, wherein 16 percent of pentaerythritol, 0.5 percent of potassium hydroxide, 83 percent of ethylene oxide and 0.5 percent of glacial acetic acid are adopted, vacuumizing the reaction kettle to-95 KPa under the condition that the temperature in the reaction kettle is 90 ℃, adding 0.5 percent of potassium hydroxide, stirring, adding 16 percent of pentaerythritol into the kettle by utilizing negative pressure, pumping the reaction kettle to-95 KPa, replacing nitrogen gas in the reaction kettle for 4 times, pressurizing to ensure that the air pressure of the reaction kettle reaches-50 KPa, controlling the temperature of the reaction kettle to be 80 ℃, adding 2.8 percent of ethylene oxide, heating to 90 ℃, initiating a reaction activation period, continuously adding 80.2 percent of ethylene oxide into the kettle, gradually increasing the temperature from 90 ℃ to 120 ℃ in the feeding process, controlling the temperature of the reaction kettle to not rise any more, ensuring that the air pressure in the kettle cannot exceed 350KPa, finishing feeding, maintaining the reaction temperature to be 115 ℃ for curing, lasting for 1h, cooling to 90 ℃ after curing, performing degassing operation, adding 0.5% glacial acetic acid after degassing, stirring for 30min, cooling to 50 ℃, purging a storage barrel with nitrogen for 20 seconds, discharging into the storage barrel, and collecting the synthetic pentaerythritol polyether;
secondly, preparing materials, 11 percent of pentaerythritol polyether, 0.8 percent of potassium hydroxide, 87.5 percent of ethylene oxide and 0.7 percent of glacial acetic acid, vacuumizing the reaction kettle to-95 KPa under the condition that the temperature of the reaction kettle is 30 ℃, adding 12 percent of pentaerythritol polyether, stirring, adding 0.8 percent of potassium hydroxide into the kettle, pumping negative pressure to-95 KPa into the reaction kettle after the feeding is finished, heating the reaction kettle to 100 ℃, blowing nitrogen into the reaction kettle for dehydration for 1.5h to ensure that the air pressure of the reaction kettle reaches-60 KPa, controlling the temperature of the reaction kettle to 100 ℃, adding 87.5 percent of ethylene oxide, gradually increasing the temperature from 100 ℃ to 125 ℃ in the feeding process, then controlling the temperature of the reaction kettle not to rise any more, ensuring that the air pressure in the kettle cannot exceed 400KPa, finishing the feeding, maintaining the degassing temperature of the reaction kettle to be 115 ℃ for curing, lasting for 1h, and performing operation after the curing is finished, and after degassing, cooling to 80 ℃, adding 0.7% glacial acetic acid, stirring for 30min, cooling the temperature of the reaction kettle to 75 ℃, purging the storage barrel for 20 seconds by nitrogen, discharging into the storage barrel, and collecting to obtain the high molecular weight pentaerythritol polyoxyethylene ether product.
Has the advantages that: the invention can synthesize high molecular weight pentaerythritol polyoxyethylene ether, and the molecular weight of the pentaerythritol polyoxyethylene ether can reach 7000-10000; the alkali metal compound is used as the catalyst, so that the generation of side reactants is reduced, and the economic benefit is improved; the adopted raw materials are few in variety, the solvent is not required to be recycled, and the production efficiency is improved.
The foregoing is a more detailed description of the present invention that is presented in conjunction with specific embodiments, and the specific embodiments of the present invention should not be considered limited to the foregoing description. It will be apparent to those skilled in the art that several simple deductions or substitutions can be made to the above embodiments without departing from the inventive concept, the scope of which is defined by the appended claims and their equivalents.
Claims (6)
1. A method for synthesizing high molecular weight pentaerythritol polyoxyethylene ether is characterized in that pentaerythritol, alkali metal compounds, glacial acetic acid and ethylene oxide are used as raw materials to prepare the high molecular weight pentaerythritol polyoxyethylene ether through two-step reaction, and the method specifically comprises the following steps:
the first step is as follows:
preparing materials, namely 15-17% of pentaerythritol, 0.5% of alkali metal compound, 82-84% of ethylene oxide and 0.5% of glacial acetic acid;
1) feeding, heating the kettle to 90-100 ℃, vacuumizing the kettle to negative pressure, feeding 0.5% of alkali metal compound and 15-17% of pentaerythritol;
2) performing replacement, namely pumping negative pressure to the reaction kettle, and introducing nitrogen to replace air in the kettle;
3) feeding, namely adding 82-84% of ethylene oxide into the reaction kettle twice;
4) curing, maintaining the reaction temperature in the reaction kettle at 115 ℃ and 125 ℃ for 1 h;
5) neutralizing, cooling and degassing the reaction kettle, adding 0.5% glacial acetic acid, and stirring for 30 min;
6) discharging, and collecting a reaction product A after the temperature is reduced to 50-60 ℃;
the second step is that:
preparing materials, wherein the reaction product A accounts for 10-12%, the alkali metal compound accounts for 0.8%, the ethylene oxide accounts for 86.5-89%, and the glacial acetic acid accounts for 0.7%;
1) feeding materials, maintaining the temperature of a reaction kettle at 30-50 ℃, pumping negative pressure by using a vacuum pump, feeding 10-12% of a reaction product A into the reaction kettle, stirring, and then feeding 0.8% of an alkali metal compound;
2) replacing, pumping negative pressure to the reaction kettle, and introducing nitrogen to replace air in the kettle;
3) heating for dehydration, and carrying out nitrogen drum dehydration for 1.5 h;
4) feeding ethylene oxide, adding 86.5-89% of ethylene oxide;
5) curing, maintaining the reaction temperature of 115 ℃ and 125 ℃ for 1 h;
6) neutralizing, cooling and degassing the reaction kettle, adding 0.7% glacial acetic acid, and stirring for 30 min;
7) discharging, cooling to 75-80 ℃, discharging, stopping stirring, and collecting to obtain the product, namely the high molecular weight pentaerythritol polyoxyethylene ether.
2. The method for synthesizing pentaerythritol polyoxyethylene ether with high molecular weight according to claim 1, wherein the reaction temperature in the step 3) in the first step is 90-120 ℃, and the pressure in the reaction kettle is less than or equal to 350 kPa.
3. The method for synthesizing pentaerythritol polyoxyethylene ether with high molecular weight as claimed in claim 1, wherein the reaction temperature in the step 4) in the second step is 100 ℃ to 125 ℃, and the pressure in the reaction kettle is less than or equal to 400 kPa.
4. The method for synthesizing pentaerythritol polyoxyethylene ether with high molecular weight according to claim 1, wherein the storage barrel is purged with nitrogen for 20 seconds before the discharging in step 6) in the first step.
5. The method for synthesizing pentaerythritol ethoxylate having a high molecular weight according to claim 1, wherein the storage tank is purged with nitrogen for 20 seconds before the discharging in step 7) in the second step.
6. The method of synthesizing high molecular weight pentaerythritol polyoxyethylene ether according to claim 1, wherein the alkali metal compound is potassium hydroxide.
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| CN114773167A (en) * | 2022-04-15 | 2022-07-22 | 上海抚佳精细化工有限公司 | Pentaerythritol polyoxyethylene ether with low addition number and preparation method thereof with high conversion rate |
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Cited By (2)
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| CN114773167A (en) * | 2022-04-15 | 2022-07-22 | 上海抚佳精细化工有限公司 | Pentaerythritol polyoxyethylene ether with low addition number and preparation method thereof with high conversion rate |
| CN114773167B (en) * | 2022-04-15 | 2023-12-22 | 上海抚佳精细化工有限公司 | Pentaerythritol polyoxyethylene ether with low addition number and high conversion rate preparation method thereof |
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