CN113956137A - Preparation method for alcohol head polymerization purification - Google Patents
Preparation method for alcohol head polymerization purification Download PDFInfo
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- CN113956137A CN113956137A CN202111404166.6A CN202111404166A CN113956137A CN 113956137 A CN113956137 A CN 113956137A CN 202111404166 A CN202111404166 A CN 202111404166A CN 113956137 A CN113956137 A CN 113956137A
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/05—Preparation of ethers by addition of compounds to unsaturated compounds
- C07C41/06—Preparation of ethers by addition of compounds to unsaturated compounds by addition of organic compounds only
- C07C41/08—Preparation of ethers by addition of compounds to unsaturated compounds by addition of organic compounds only to carbon-to-carbon triple bonds
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
- C07C41/01—Preparation of ethers
- C07C41/34—Separation; Purification; Stabilisation; Use of additives
- C07C41/40—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation
- C07C41/42—Separation; Purification; Stabilisation; Use of additives by change of physical state, e.g. by crystallisation by distillation
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Abstract
The invention provides a preparation method of alcohol head polymerization purification, which is used for preparing C6 alcohol head diethylene glycol monovinyl ether. The preparation method comprises the steps of carrying out full polymerization reaction on diethylene glycol, a prefabricated mixed solution and acetylene in a reaction kettle to obtain a reaction mixture, rectifying the reaction mixture by a first-stage rectifying tower and a second-stage rectifying tower, and collecting a diether byproduct and C6 alcohol head diethylene glycol monovinyl ether by adjusting a reflux ratio. The purity of the C6 alcohol head obtained by the invention is more than 98%, and the alcohol head basically has no by-product of diether and reaches the factory standard.
Description
Technical Field
The invention belongs to the technical field of synthesis of diethylene glycol monovinyl ether, and particularly relates to a preparation method for purifying an alcohol head by polymerization.
Background
At present, the conservation of polyether macromonomers for the polycarboxylic acid water reducing agent at home is estimated to be 100 ten thousand tons/year, the first alcohol dosage is estimated according to 3 percent, and the first 3 ten thousand tons/year is demanded at home. The alcohol heads currently used for synthesizing the polyether macromonomer are mainly methyl allyl alcohol (commonly called C4 alcohol head) and 3-methyl-3-butylene-1-alcohol (commonly called C5 alcohol head), the C4 alcohol head is mainly produced by the domestic product, and the C5 alcohol head is mainly imported from Collar of Japan. The actual production capacity of the domestic diethylene glycol monovinyl ether (commonly called C6 alcohol head) is about 2400 tons/year at present, the polycarboxylic acid water reducing agent synthesized by the polyether macromonomer prepared by the C6 alcohol head has obvious advantages on the C4 alcohol head and the C5 alcohol head in the aspects of mud resistance, slump retention and the like, and the capacity demand of the C6 alcohol head has obvious growth trend and growth space.
Diethylene glycol monovinyl ether (CAS: 929-37-3) is the largest amount of C6 alcohol heads, and is colorless transparent liquid with a density of 0.968g/cm 3 (20 deg.C), melting point-21 deg.C, boiling point 208 deg.C, and flash point 83 deg.C. The polyether monomer can be used as a reactive diluent of a UV cation curing coating and a comonomer for modifying a polymer, particularly, diethylene glycol monovinyl ether is used as an initiator, alkylene oxide is used as a polymerization monomer, and the polyether monomer with a certain molecular weight and vinyl double bond at the tail end is synthesized through anionic ring-opening polymerization. The carboxylic acid water reducer synthesized by the polyether monomer, acrylic acid, acrylate and other monomers through aqueous phase free radical polymerization has the characteristics of good mud resistance effect, low doping sensitivity and the like, and has certain application in the fields of commercial mixing, tubular piles, UHPC and the like.
The synthesis of diethylene glycol monovinyl ether (4-hydroxybutyl vinyl ether is synthesized by acetylene method) is obtained by reacting diethylene glycol with acetylene under the action of catalyst, the reaction process not only obtains diethylene glycol monovinyl ether, but also obtains byproduct diethylene glycol divinyl ether, and the reaction process is as follows:
after the reaction of acetylene and diethylene glycol is finished, a target product diethylene glycol monovinyl ether needs to be separated by rectification, and a byproduct diethylene glycol divinyl ether is a common diluent with chemical reaction activity and can be sold as a chemical for the second time. In the prior art, the yield of the diethylene glycol monovinyl ether is 60%, so that a preparation method of the diethylene glycol monovinyl ether, which reduces the content of byproducts and improves the yield of the diethylene glycol monovinyl ether, needs to be provided.
Disclosure of Invention
The invention aims to solve the technical problems and provides a preparation method for alcohol head polymerization purification.
In order to achieve the purpose, the invention adopts the following technical scheme:
an alcohol head polymerization purification preparation method comprises the following steps:
(A) adding a prefabricated mixed solution of diethylene glycol, a catalyst, a polymerization inhibitor and a stabilizer into a reaction kettle;
(B) replacing air in the reaction kettle by nitrogen, vacuumizing the reaction kettle, introducing acetylene into the reaction kettle at the temperature of 150-170 ℃, and fully performing the following reactions:
(C) cooling the reaction kettle, and discharging the reaction mixture after the temperature is reduced to below 45 ℃;
(D) rectifying the reaction mixture from the step (C), adding the reaction mixture from the step (C) into a rectifying tower, setting the temperature of a tower bottom of the rectifying tower to be 137-plus 143 ℃, gradually increasing the temperature to be 157-plus 163 ℃, wherein the rectifying tower comprises a primary rectifying tower and a secondary rectifying tower, setting the temperature of the primary rectifying tower and the temperature of the secondary rectifying tower to be 107-plus 113 ℃, gradually increasing the temperature to be 112-plus 118 ℃, condensing the gas-phase component rectified by the primary rectifying tower through a condenser, collecting the gas-phase component into a first monoether receiving tank, adding the liquid-phase component rectified by the primary rectifying tower into the secondary rectifying tower, condensing the gas-phase component rectified by the secondary rectifying tower through the condenser, adjusting the reflux ratio, collecting the gas-phase component into a second monoether receiving tank and a diether receiving tank, vacuumizing the rectifying tower, the first monoether receiving tank, the second monoether receiving tank and the diether receiving tank, and vacuumizing the first monoether receiving tank, The second monoether receiving tank is the alcohol head product.
Preferably, in the step (D), the liquid phase component rectified by the secondary rectifying tower is recycled and added into the reaction kettle in the step (1).
Preferably, a step (C1) is further included between step (C) and step (D): sampling a reaction mixture, testing the gas phase and the water content of the sampled reaction mixture, and adding alcohol head products in a first monoether receiving tank and a second monoether receiving tank into the reaction mixture according to a test result, or adding flash liquid containing a certain proportion of alcohol heads in a flash tank of a first-stage rectifying tower, or adding tower bottom liquid containing a certain proportion of alcohol heads in a rectifying tower, so that the proportion of the alcohol heads in the reaction mixture added into the rectifying tower is 38-41%.
Preferably, the weight components of the diethylene glycol, the acetylene and the pre-prepared mixed solution are as follows: 270 parts of diethylene glycol 250-one, 25-35 parts of acetylene and 8-9 parts of a prepared mixed solution.
Preferably, the weight components of the diethylene glycol, the acetylene and the pre-prepared mixed solution are as follows: 265 parts of diethylene glycol 255-.
Preferably, in the step (B), the acetylene is fed into the reaction kettle at a constant speed, the pressure in the reaction kettle is kept to be less than or equal to 0.3MPa, and the heat-preservation reaction is continued for at least 1h after the acetylene is fed.
Preferably, in the step (D), the temperature of the distillation tower bottom is set to 139-.
After the technical scheme is adopted, the invention has the following advantages:
because the boiling points of the diether byproduct and the C6 alcohol head are close and are between 196 ℃ and 200 ℃, the difficulty of rectifying the C6 alcohol head is mainly the separation between the diether byproduct and C6. The method adopts the first-stage rectifying tower and the second-stage rectifying tower to solve the separation problem between the diether byproduct and the C6 alcohol head, the fraction collected firstly is the diether byproduct with the content of about 80 percent, and the rest components are C6 alcohol heads with the content of about 20 percent; and secondly, the collected C6 alcohol head has the purity of over 98 percent, basically has no diether by-product and reaches the factory standard.
Drawings
FIG. 1 shows a process flow of alcohol head reaction and rectification;
FIG. 2 is a gas phase test spectrum of the 4 th polymerization solution;
FIG. 3 is a flash liquid vapor phase test spectrum;
FIG. 4 is a gas phase test spectrum of the overhead distillation fraction;
FIG. 5 is a gas phase test spectrum of the residual liquid in the tower bottom.
Detailed Description
The present invention will be described in further detail with reference to the following drawings and specific examples.
An alcohol head polymerization purification preparation method comprises the following steps:
(A) a pre-prepared mixed solution of diethylene glycol, catalyst, inhibitor and stabilizer is added into a reaction kettle.
The weight components of the diethylene glycol, the acetylene and the prepared mixed solution are as follows: 270 parts of diethylene glycol 250-one, 25-35 parts of acetylene and 8-9 parts of a prefabricated mixed solution; preferably: 265 parts of diethylene glycol 255-.
In one embodiment, the weight composition of the diethylene glycol, acetylene, and pre-formed mixed solution is: 250 parts of diethylene glycol, 25 parts of acetylene and 8 parts of a prefabricated mixed solution; in one embodiment, the weight composition of the diethylene glycol, acetylene, and pre-formed mixed solution is: 270 parts of diethylene glycol, 35 parts of acetylene and 9 parts of a prefabricated mixed solution; in one embodiment, the weight composition of the diethylene glycol, acetylene, and pre-formed mixed solution is: 260 parts of diethylene glycol, 30 parts of acetylene and 8.5 parts of a prefabricated mixed solution; in one embodiment, the weight composition of the diethylene glycol, acetylene, and pre-formed mixed solution is: 255 parts of diethylene glycol, 27 parts of acetylene and 8.3 parts of a prefabricated mixed solution; in one embodiment, the weight composition of the diethylene glycol, acetylene, and pre-formed mixed solution is: 265 parts of diethylene glycol, 32 parts of acetylene and 8.7 parts of a prepared mixed solution.
(B) Replacing air in the reaction kettle by nitrogen, vacuumizing the reaction kettle, introducing acetylene into the reaction kettle at the temperature of 150-170 ℃, keeping the acetylene fed at a constant speed when introducing the acetylene into the reaction kettle, keeping the pressure in the reaction kettle to be less than or equal to 0.3MPa, and continuing to perform heat preservation reaction for at least 1h after the acetylene is fed, so as to fully perform the following reactions:
(C) and (3) cooling the reaction kettle, and discharging the reaction mixture after the temperature is reduced to below 45 ℃.
(C1) Sampling a reaction mixture, testing the gas phase and the water content of the sampled reaction mixture, and adding alcohol head products in a first monoether receiving tank and a second monoether receiving tank into the reaction mixture according to a test result, or adding flash liquid containing a certain proportion of alcohol heads in a flash tank of a first-stage rectifying tower, or adding tower bottom liquid containing a certain proportion of alcohol heads in a rectifying tower, so that the proportion of the alcohol heads in the reaction mixture added into the rectifying tower is 38-41%.
(D) Rectifying the reaction mixture from the step (C), adding the reaction mixture from the step (C) into a rectifying tower, setting the temperature of a tower kettle of the rectifying tower at 137-.
Condensing gas-phase components rectified by a first-stage rectifying tower through a condenser and then collecting the gas-phase components into a first monoether receiving tank, adding liquid-phase components rectified by the first-stage rectifying tower into a second-stage rectifying tower, condensing the gas-phase components rectified by the second-stage rectifying tower through the condenser, adjusting the reflux ratio, collecting the gas-phase components into a second monoether receiving tank and a diether receiving tank, vacuumizing the rectifying tower, the first monoether receiving tank, the second monoether receiving tank and the diether receiving tank, and obtaining alcohol head products in the first monoether receiving tank and the second monoether receiving tank.
In one embodiment, the temperature of the tower kettle of the rectifying tower is set to be 137 ℃, and gradually increased to 157 ℃, and the temperatures of the primary rectifying tower and the secondary rectifying tower are set to be 107 ℃ and gradually increased to 112 ℃; in one embodiment, the temperature of the tower bottom of the rectifying tower is set to be 143 ℃, gradually increased to 163 ℃, and the temperatures of the primary rectifying tower and the secondary rectifying tower are set to be 113 ℃ and gradually increased to 118 ℃; in one embodiment, the temperature of the tower kettle of the rectifying tower is set to be 140 ℃, and gradually increased to 160 ℃, and the temperature of the primary rectifying tower and the secondary rectifying tower is set to be 110 ℃, and gradually increased to 115 ℃; in one embodiment, the temperature of the tower kettle of the rectifying tower is set to be 139 ℃, and gradually increased to 159 ℃, and the temperature of the primary rectifying tower and the secondary rectifying tower is set to be 109 ℃, and gradually increased to 114 ℃; in one embodiment, the column bottom temperature of the rectification column is set at 141 ℃ and gradually increased to 161 ℃, and the temperatures of the first rectification column and the second rectification column are set at 111 ℃ and gradually increased to 116 ℃.
In this example, a pilot test of a C6 alcohol head was conducted using the alcohol head reaction and rectification process flow shown in FIG. 1.
1. C6 alcohol head reaction step
The catalyst, polymerization inhibitor and stabilizer which are totally finished by C6 alcohol head synthesis are prepared mixed solution, which is named as CZW, and the mixture ratio is shown in Table 1.
Polymerization solution experimental procedure: 2600g of diethylene glycol and CZW85g are weighed, added into a reaction kettle, the reaction kettle is sealed and replaced by nitrogen for 3 times, and vacuum pumping is carried out again until the pressure is-0.1 MPa. An acetylene cylinder with a pressure reducing meter is connected, and the acetylene cylinder is placed on an electronic scale with the measuring range of 50Kg to prepare for feeding. And opening a steam valve to heat the reaction kettle, and opening an acetylene feeding valve to start feeding when the temperature of the reaction kettle rises to 150 ℃. Controlling the feeding amount of acetylene to be 25g/h, the pressure of the reaction kettle to be less than or equal to 0.3MPa, and the temperature of the reaction kettle to be 150-170 ℃. After acetylene feeding is finished, continuing to carry out heat preservation reaction for 1h, then opening circulating cooling water for cooling, and when the temperature of the reaction kettle is reduced to about 40 ℃, discharging and sampling to carry out gas phase and water content tests.
The rectifying tower comprises the following experimental steps: 2000g of polymerization liquid is weighed and added into a rectifying tower kettle, a condenser at the top of the tower and circulating cooling water of a reflux ratio regulating valve are started, a circulating cooling water inlet switch is opened by a vacuum water pump, and the vacuum degree stability of a vacuum pump is ensured. Setting the temperature of a tower kettle to be 140 ℃, and gradually increasing the temperature to 160 ℃; the temperature of the first-stage rectifying tower and the second-stage rectifying tower is 110 ℃, and gradually rises to 115 ℃; and opening a vacuum pump, and pumping the rectifying tower to-0.1 MPa. And when the total reflux is stable for more than or equal to 30min, sampling fractions, performing gas phase test analysis on the fraction composition, adjusting the reflux ratio, and collecting diether and C6 alcohol head.
Gas phase test conditions: the sample injector is 250 ℃, the detector is 250 ℃, the column incubator is 150 ℃, the peak emergence time of the by-product diether is 1.83min, the peak emergence time of the target product C6 is 3.3min, and the peak emergence time of the diethylene glycol is 7.8 min.
2. C6 alcohol head bench test results analysis
2.1C 6 alcohol head polymerization
A6-kettle C6 polymerization liquid test is performed in an accumulated mode, wherein the 1 st kettle and the 2 nd kettle fail to react due to air leakage of the reaction kettles, the polymerization reactions of the 3 rd kettle to the 5 th kettle are normal, and the 6 th kettle uses the polymerization liquid failed in the reaction of the 1 st kettle as a bottom material to continue acetylene reaction to be normal. The gas phase test and water content test data are shown in table 2.
Table 3 table of chromatographic analysis results in fig. 2
As can be seen from Table 2, FIG. 2 and Table 3, after the air leakage problem of the reaction kettle is repaired, the content of C6 in the prepared C6 polymer solution is basically between 41% and 47%, and the polymer solution synthesis experiment is basically successful. As the C6 level increased, the proportion of diether byproduct increased from 10% in the 3 rd kettle to 13% in the 5 th kettle. From the test results of the polymerization liquid, the content of C6 should be properly controlled to be between 38% and 41%, so as to ensure that the content of the diether byproduct is low.
2.2C 6 alcohol head rectification purification
The difficulty of C6 alcohol head rectification mainly lies in the separation between the diether byproduct and C6, the boiling points of the two compounds are close, and the boiling points are reported in the literature to be 196-200 ℃. This pilot plant purchased a packing rectification column set specifically for separating diether by-product and C6 alcohol heads with similar boiling points.
Table 4 table of chromatographic analysis results of fig. 3
Table 5 table of results of chromatogram analysis in fig. 4
Table 6 table of results of chromatogram analysis in fig. 5
As shown in fig. 3-5 and tables 4-6, the rectification experiments showed that the first collected fraction was a diether byproduct with a content of about 80%, and the remaining component was C6 alcohol head with a content of about 20%. And secondly, the collected C6 alcohol head has the purity of over 98 percent, basically has no diether by-product and reaches the factory standard. And finally, the residual liquid in the tower bottom is mainly diethylene glycol with the content of about 97 percent, and the residual component is C6 alcohol head with the content of about 2 percent.
Through calculation on the collected C6 alcohol head, the following results are found: 2000g of column bottom feed contains 840g of C6 alcohol head theoretically according to 42 percent of C6 alcohol head content, 702g of C6 alcohol head is actually rectified, and the single rectification yield is 83.6 percent. The flash liquid contains 20% of C6 alcohol head, the tower bottom liquid contains 2% of C6 alcohol head, the liquid can be reused, and the yield of the C6 alcohol head is further improved.
Other embodiments of the present invention than the preferred embodiments described above will be apparent to those skilled in the art from the present invention, and various changes and modifications can be made therein without departing from the spirit of the present invention as defined in the appended claims.
Claims (7)
1. The preparation method for purifying the alcohol head by polymerization is characterized by comprising the following steps of:
(A) adding a prefabricated mixed solution of diethylene glycol, a catalyst, a polymerization inhibitor and a stabilizer into a reaction kettle;
(B) replacing air in the reaction kettle by nitrogen, vacuumizing the reaction kettle, introducing acetylene into the reaction kettle at the temperature of 150-170 ℃, and fully performing the following reactions:
(C) cooling the reaction kettle, and discharging the reaction mixture after the temperature is reduced to below 45 ℃;
(D) rectifying the reaction mixture from the step (C), adding the reaction mixture from the step (C) into a rectifying tower, setting the temperature of a tower bottom of the rectifying tower to be 137-plus 143 ℃, gradually increasing the temperature to be 157-plus 163 ℃, wherein the rectifying tower comprises a primary rectifying tower and a secondary rectifying tower, setting the temperature of the primary rectifying tower and the temperature of the secondary rectifying tower to be 107-plus 113 ℃, gradually increasing the temperature to be 112-plus 118 ℃, condensing the gas-phase component rectified by the primary rectifying tower through a condenser, collecting the gas-phase component into a first monoether receiving tank, adding the liquid-phase component rectified by the primary rectifying tower into the secondary rectifying tower, condensing the gas-phase component rectified by the secondary rectifying tower through the condenser, adjusting the reflux ratio, collecting the gas-phase component into a second monoether receiving tank and a diether receiving tank, vacuumizing the rectifying tower, the first monoether receiving tank, the second monoether receiving tank and the diether receiving tank, and vacuumizing the first monoether receiving tank, The second monoether receiving tank is the alcohol head product.
2. The method for preparing alcohol head polymerization purification according to claim 1, wherein in the step (D), the liquid phase component rectified by the secondary rectifying tower is recycled and added into the reaction kettle in the step (1).
3. The alcohol head polymerization purification preparation method of claim 1, further comprising a step (C1) between the step (C) and the step (D): sampling a reaction mixture, testing the gas phase and the water content of the sampled reaction mixture, and adding alcohol head products in a first monoether receiving tank and a second monoether receiving tank into the reaction mixture according to a test result, or adding flash liquid containing a certain proportion of alcohol heads in a flash tank of a first-stage rectifying tower, or adding tower bottom liquid containing a certain proportion of alcohol heads in a rectifying tower, so that the proportion of the alcohol heads in the reaction mixture added into the rectifying tower is 38-41%.
4. The alcohol head polymerization purification preparation method according to claim 1, wherein the weight components of the diethylene glycol, the acetylene and the pre-prepared mixed solution are as follows: 270 parts of diethylene glycol 250-one, 25-35 parts of acetylene and 8-9 parts of a prepared mixed solution.
5. The alcohol head polymerization purification preparation method according to claim 4, wherein the weight components of the diethylene glycol, the acetylene and the pre-prepared mixed solution are as follows: 265 parts of diethylene glycol 255-.
6. The alcohol head polymerization purification preparation method of claim 1, wherein in the step (B), the acetylene is fed into the reaction kettle at a constant speed, the pressure in the reaction kettle is kept to be less than or equal to 0.3MPa, and the heat preservation reaction is continued for at least 1h after the acetylene is fed.
7. The method as claimed in claim 1, wherein in the step (D), the temperature of the distillation column is set to 139-.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114478203A (en) * | 2022-01-28 | 2022-05-13 | 沧州中润化学助剂有限公司 | Preparation method of vinyl low-carbon alcohol for polyether initiator |
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| CN101898939A (en) * | 2010-08-06 | 2010-12-01 | 湖北新景新材料有限公司 | Method for preparing compound 4-hydroxy butyl vinyl ether |
| CN111643918A (en) * | 2020-06-16 | 2020-09-11 | 山东中盛药化设备有限公司 | Rectification purification device and purification method for multi-component material |
| CN112778102A (en) * | 2020-07-31 | 2021-05-11 | 江苏金木土新材料有限公司 | Method for purifying vinyl ether monomer |
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| JPH0454145A (en) * | 1990-06-20 | 1992-02-21 | Nisso Maruzen Chem Kk | Purification of alkylene glycol monovinyl ethers |
| JP2002193881A (en) * | 2000-10-17 | 2002-07-10 | Nippon Shokubai Co Ltd | Method for producing vinyl ether group-containing (meth) acrylic esters |
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