CN110386915B - Method for separating mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane - Google Patents

Method for separating mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane Download PDF

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CN110386915B
CN110386915B CN201810370863.6A CN201810370863A CN110386915B CN 110386915 B CN110386915 B CN 110386915B CN 201810370863 A CN201810370863 A CN 201810370863A CN 110386915 B CN110386915 B CN 110386915B
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tower
dichloroethane
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vinyl sulfate
hexane
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CN110386915A (en
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贺鹏
周培林
曹妍
王利国
李会泉
黄科林
陈家强
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Institute of Process Engineering of CAS
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives
    • C07C17/383—Separation; Purification; Stabilisation; Use of additives by distillation
    • C07C17/386—Separation; Purification; Stabilisation; Use of additives by distillation with auxiliary compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/04—Purification; Separation; Use of additives by distillation
    • C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
    • C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D327/00—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms
    • C07D327/10—Heterocyclic compounds containing rings having oxygen and sulfur atoms as the only ring hetero atoms two oxygen atoms and one sulfur atom, e.g. cyclic sulfates
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00—Systems containing only non-condensed rings
    • C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/14—The ring being saturated

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Abstract

A separation method of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane comprises the following steps: the raw materials are put in a rectifying tower T1Feeding at the bottom, collecting a solution I with the total mass fraction of normal hexane and 1, 2-dichloroethane being more than 99.8% at the top of the tower, and collecting a solution II with the mass fraction of vinyl sulfate being more than 90% at the bottom of the tower; pouring the solution II into a crystallizer B1Cooling and filtering to obtain a filter cake which is vinyl sulfate with the purity of more than 99.8 percent; mixing the solution I with an extracting agent and then putting the mixture in a rectifying tower T2Feeding at the bottom, extracting a normal hexane product at the top of the tower, and extracting an extracting agent and a solution III with the total mass fraction of 1, 2-dichloroethane of more than 99.8% at the bottom of the tower; the solution III is put in a rectifying tower T3Feeding at the bottom, collecting 1, 2-dichloroethane product at the top of the column, collecting extractant at the bottom of the column, and returning the extractant to the rectifying tower T2. The separation method of the mixed solution of the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane is simple, easy to operate, high in safety, low in energy consumption, high in purity of extracted products and high in product recovery rate.

Description

Method for separating mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane
Technical Field
The invention belongs to the technical field of separation, and particularly relates to a separation method of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane.
Background
With the development of electronic information industry in China, the demand of chemical energy sources is getting larger and larger. Because the lithium ion battery has the advantages of small volume, light weight, good safety performance, high specific energy, high voltage, long service life, no pollution and the like, the lithium ion battery is a main source of portable electronic equipment such as mobile phones, notebook computers and the like. The performance of the battery can be greatly improved by adding some additives into the lithium ion battery electrolyte. The vinyl sulfate is a novel SEI film forming additive, can inhibit the reduction of the initial capacity of the battery, increase the initial discharge capacity, reduce the expansion of the battery after high-temperature placement, and improve the charge and discharge performance and cycle number of the battery.
The current main method for preparing the vinyl sulfate is to take sulfur trioxide and ethylene oxide as raw materials to react in a heterogeneous catalysis environment containing normal hexane and 1, 2-dichloroethane solvent to prepare the vinyl sulfate. The process has high product quality and less three wastes, but the process produces a byproduct of mixed solution of normal hexane and 1, 2-dichloroethane containing part of vinyl sulfate. On one hand, a small amount of vinyl sulfate product needs to be recovered; on the other hand, high purity n-hexane and 1, 2-dichloroethane need to be recovered for use in the front end unit process. There are two main problems associated with the recovery of this mixed liquor: (1) the vinyl sulfate is a heat-sensitive substance, is easy to decompose when heated to a certain temperature, and the decomposition temperature of the vinyl sulfate is close to the boiling points of n-hexane and 1, 2-dichloroethane; (2) the normal hexane and the 1, 2-dichloroethane are azeotropic systems, the mass composition of the azeotropic system is about 1: 1, and the normal hexane and the 1, 2-dichloroethane with high purity are difficult to obtain by adopting common separation methods such as simple rectification and pressure swing rectification separation.
Therefore, the development of a process for recovering vinyl sulfate and separating a mixed solution of high-purity n-hexane and 1, 2-dichloroethane has important application significance.
Disclosure of Invention
In view of the shortcomings of the prior art, the present invention provides a method for separating a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane, so as to solve at least one of the above problems.
The invention is realized by the following technical scheme:
a separation method of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane comprises the following steps: (1) the mixed solution containing the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane is put in a rectifying tower T1Bottom feedA solution I with the total mass fraction of normal hexane and 1, 2-dichloroethane being more than 99.8% is extracted from the top of the tower, and a solution II with the mass fraction of vinyl sulfate being more than 90% is extracted from the bottom of the tower; (2) pouring said solution II into a crystallizer B1Cooling and filtering, and returning the filtrate to the rectifying tower T1The filter cake is vinyl sulfate with the purity of more than 99.8 percent; (3) mixing the solution I with an extracting agent and then putting the mixture in a rectifying tower T2Feeding at the bottom, extracting a normal hexane product at the top of the tower, and extracting an extracting agent and a solution III with the total mass fraction of 1, 2-dichloroethane of more than 99.8% at the bottom of the tower; (4) subjecting the solution III to a rectification column T3Feeding at the bottom, collecting 1, 2-dichloroethane product at the top of the column, collecting extractant at the bottom of the column, and returning the extractant to the rectifying tower T2。
Preferably, in the step (3), the extractant is one or a combination of more than two of cyclohexanone, cyclohexanol, 1, 2-propylene glycol, N-dimethylaniline, ethylene glycol, formamide and diethylene glycol.
Preferably, in the step (3), the mass ratio of the extracting agent to the solution I is 1-5: 1.
Preferably, said rectification column T1The number of theoretical plates is 10-30, the operation pressure is 30-70 kPa, the temperature of a tower kettle is 30-80 ℃, and the reflux ratio is 0.1-5.
Preferably, said rectification column T2The number of theoretical plates is 10-50, the temperature of a tower kettle is 50-120 ℃, and the reflux ratio is 1-10.
Preferably, said rectification column T3The theoretical plate number of the tower is 10-50, and the temperature of the tower kettle is 60-150 ℃.
According to the technical scheme, the separation method of the mixed solution of the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane has the following beneficial effects:
the separation method is simple, easy to operate, high in safety, low in energy consumption, high in purity of extracted products and high in product recovery rate. The purity of the n-hexane obtained by separation can reach more than 99.7 percent, the purity of the 1, 2-dichlorohexane can reach more than 99.8 percent, and the purity of the vinyl sulfate can reach more than 99.9 percent.
Drawings
FIG. 1 is a flow chart of a separation process of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane in the embodiment of the present invention;
[ description of the elements of the drawings ]
1-raw material recovery liquid; 2-concentrated vinyl sulfate solution;
crystallizing 3-vinyl sulfate and filtering; 4-a vinyl sulfate ester product;
5-a solution rich in n-hexane and 1, 2-dichloroethane; 6-n-hexane product;
7-an extractant-rich 1, 2-dichloroethane stream; 8-1, 2-dichloroethane product;
9-an extractant; t is1、T2、T3-a rectification column;
B1-a crystallizer.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention provides a separation method of a mixed solution of vinyl sulfate, normal hexane and 1, 2-dichloroethane, which comprises the following steps: the raw materials are put in a rectifying tower T1Feeding at the bottom, collecting a solution I with the total mass fraction of normal hexane and 1, 2-dichloroethane being more than 99.8% at the top of the tower, and collecting a solution II with the mass fraction of vinyl sulfate being more than 90% at the bottom of the tower; pouring the solution II into a crystallizer B1Cooling and filtering to obtain a filter cake which is vinyl sulfate with the purity of more than 99.8 percent; mixing the solution I with an extracting agent and then putting the mixture in a rectifying tower T2Feeding at the bottom, extracting a normal hexane product at the top of the tower, and extracting an extracting agent and a solution III with the total mass fraction of 1, 2-dichloroethane of more than 99.8% at the bottom of the tower; the solution III is put in a rectifying tower T3Feeding at the bottom, collecting 1, 2-dichloroethane product at the top of the column, collecting extractant at the bottom of the column, and returning the extractant to the rectifying tower T2. The separation method of the mixed solution of the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane is simple, easy to operate, high in safety, low in energy consumption, high in purity of extracted products and high in product recovery rate.
Specifically, the invention provides a separation method of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane, which comprises the following steps: (1) the mixed solution containing the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane is put in a rectifying tower T1Feeding at the bottom, collecting a solution I with the total mass fraction of normal hexane and 1, 2-dichloroethane being more than 99.8% at the top of the tower, and collecting a solution II with the mass fraction of vinyl sulfate being more than 90% at the bottom of the tower; (2) pouring said solution II into a crystallizer B1Cooling and filtering, and returning the filtrate to the rectifying tower T1The filter cake is vinyl sulfate with the purity of more than 99.8 percent; (3) mixing the solution I with an extracting agent and then putting the mixture in a rectifying tower T2Feeding at the bottom, extracting a normal hexane product at the top of the tower, and extracting an extracting agent and a solution III with the total mass fraction of 1, 2-dichloroethane of more than 99.8% at the bottom of the tower; (4) subjecting the solution III to a rectification column T3Feeding at the bottom, collecting 1, 2-dichloroethane product at the top of the column, collecting extractant at the bottom of the column, and returning the extractant to the rectifying tower T2。
In the step (3), the extracting agent is one or a combination of more than two of cyclohexanone, cyclohexanol, 1, 2-propylene glycol, N-dimethylaniline, ethylene glycol, formamide and diethylene glycol.
In the step (3), the mass ratio of the extracting agent to the solution I is 1-5: 1.
The rectifying tower T1The number of theoretical plates is 10-30, the operation pressure is 30-70 kPa, the temperature of a tower kettle is 30-80 ℃, and the reflux ratio is 0.1-5.
The rectifying tower T2The number of theoretical plates is 10-50, the temperature of a tower kettle is 50-120 ℃, and the reflux ratio is 1-10.
The rectifying tower T3The theoretical plate number of the tower is 10-50, and the temperature of the tower kettle is 60-150 ℃.
The method for separating a mixed solution of vinyl sulfate, n-hexane, and 1, 2-dichloroethane according to the present invention will be described in further detail below with reference to specific examples and drawings.
Example 1
The separation scheme is shown in FIG. 1, wherein the raw materials (n-hexane content 30%, 1, 2-dichloroethane content 65%, and ethylene sulfate)5 percent of ester mass fraction) enters a rectifying tower kettle T with 10 theoretical plates from a position with 7 theoretical plates at the bottom1The raw material flow rate is 95kg/h, the operation pressure is 60kPa, the operation temperature is 60 ℃, the reflux ratio is set to be 0.1, the control distillate is extracted from the tower top and does not contain the solution of the vinyl sulfate, the solution rich in the vinyl sulfate is obtained from the tower bottom, and the tower bottom enters a crystallizer B1Cooling to separate out high-purity solid vinyl sulfate, and returning filtrate to tower bottom T1。T1The distillate enters a rectifying tower T with the theoretical plate number of 15 from the position with the theoretical plate number of 12 at the bottom2Feeding at a flow rate of 90kg/h, an operating pressure of 101kPa, a column bottom operating temperature of 85 ℃, a reflux ratio of 10, and addition of an extractant and T1The distillate is combined into T2The feeding flow rate is 120kg/h, the extracting agent is cyclohexanol, extracting agent and T1The mass ratio of the distillate at the top of the tower is 1, the normal hexane product is extracted at the top of the tower, and the solution rich in the extracting agent and the 1, 2-dichloroethane is extracted at the bottom of the tower. T is2The tower bottom liquid enters a rectifying tower T with the theoretical plate number of 15 from a position with the theoretical plate number of 12 at the bottom3The feeding flow rate is 80kg/h, the operation temperature of the tower bottom is 125 ℃, the reflux ratio is 5, 1, 2-dichloroethane product is extracted from the tower top, and the extractant extracted from the tower bottom returns to the rectifying tower T2。
Example 2
The separation flow is shown in figure 1, raw materials (the mass fraction of normal hexane is 30%, the mass fraction of 1, 2-dichloroethane is 65%, and the mass fraction of vinyl sulfate is 5%) enter a rectifying tower kettle T with theoretical plate number of 15 from a position with theoretical plate number of 13 at the bottom1The raw material flow rate is 95kg/h, the operation pressure is 30kPa, the operation temperature is 30 ℃, the reflux ratio is set to be 2, the distillate is extracted from the tower top and does not contain the solution of the vinyl sulfate, the solution rich in the vinyl sulfate is obtained at the tower bottom, and the tower bottom enters a crystallizer B1Cooling to separate out high-purity solid vinyl sulfate, and returning filtrate to tower bottom T1。T1The distillate enters a rectifying tower T with the theoretical plate number of 10 from the position with the theoretical plate number of 7 at the bottom2The feed flow rate is 90kg/h, the operating pressure is 30kPa, the operating temperature of the tower bottom is 30 ℃, the reflux ratio is 1, and an extracting agent and T are added1The distillate is combined into T2The feeding flow rate is 120kg/h, the extracting agent is cyclohexanone, the extracting agent and T1The mass ratio of the distillate at the top of the tower is 2, the normal hexane product is extracted at the top of the tower, and the solution rich in the extracting agent and the 1, 2-dichloroethane is extracted at the bottom of the tower. T is2The tower bottom liquid enters a rectifying tower T with the theoretical plate number of 35 from a position with the bottom theoretical plate number of 323Extracting 1, 2-dichloroethane product from the top of the tower, operating the tower kettle at 120 ℃, reflux ratio of 3, and returning the extractant extracted from the tower kettle to the rectifying tower T2。
Example 3
The separation flow is shown in figure 1, raw materials (the mass fraction of normal hexane is 30%, the mass fraction of 1, 2-dichloroethane is 65%, and the mass fraction of vinyl sulfate is 5%) enter a rectifying tower kettle T with 20 theoretical plates from a position with 17 theoretical plates at the bottom1The raw material flow rate is 95kg/h, the operation pressure is 50kPa, the operation temperature is 55 ℃, the reflux ratio is set to be 3, the control distillate is extracted from the tower top and does not contain the solution of the vinyl sulfate, the solution rich in the vinyl sulfate is obtained from the tower bottom, and the tower bottom enters a crystallizer B1Cooling to separate out high-purity solid vinyl sulfate, and returning filtrate to tower bottom T1。T1The distillate enters a rectifying tower T with the theoretical plate number of 35 from the position with the theoretical plate number of 32 at the bottom2The feed flow rate was 90kg/h, the operating pressure was 45kPa, the operating temperature was 50 ℃ and the reflux ratio was 3, and the extractant and T were added1The distillate is combined into T2The feeding flow rate is 120kg/h, the extracting agent is N, N dimethylaniline, the extracting agent and T1The mass ratio of the distillate at the top of the tower is 3, the normal hexane product is extracted at the top of the tower, and the solution rich in the extracting agent and the 1, 2-dichloroethane is extracted at the bottom of the tower. T is2Tower bottom liquid enters a rectifying tower T with the theoretical plate number of 10 from a position with the theoretical plate number of 7 at the bottom3The operation temperature is 130 ℃, the reflux ratio is 1, 2-dichloroethane product is extracted from the tower top, and the extractant extracted from the tower bottom returns to the rectifying tower T2。
Example 4
The separation flow is shown in figure 1, raw materials (the mass fraction of normal hexane is 30%, the mass fraction of 1, 2-dichloroethane is 65%, and the mass fraction of vinyl sulfate is 5%) enter theoretical plates from the position with the bottom of 26 theoretical platesNumber of 30 rectifying tower kettle T1The raw material flow rate is 95kg/h, the operation pressure is 70kPa, the operation temperature is 80 ℃, the reflux ratio is set to be 5, the control distillate is extracted from the tower top and does not contain the solution of the vinyl sulfate, the solution rich in the vinyl sulfate is obtained from the tower bottom, and the tower bottom enters a crystallizer B1Cooling to separate out high-purity solid vinyl sulfate, and returning filtrate to tower bottom T1。T1The distillate enters a rectifying tower T with the theoretical plate number of 50 from the position with the theoretical plate number of 45 at the bottom2The feed flow rate was 90kg/h, the operating pressure was 50kPa, the operating temperature was 65 ℃ and the reflux ratio was 7, and the extractant and T were added1The distillate is combined into T2The feed flow rate is 120kg/h, the extractant is selected from ethylene glycol, extractant and T1The mass ratio of the distillate at the top of the tower is 5, a normal hexane product is extracted at the top of the tower, and a solution which is rich in an extracting agent and 1, 2-dichloroethane is extracted at the bottom of the tower. T is2Tower bottom liquid enters into a rectifying tower T with the theoretical plate number of 50 from the position with the theoretical plate number of 30 at the bottom3The operation temperature is 90 ℃, the reflux ratio is 2, 1, 2-dichloroethane product is extracted from the tower top, and the extractant extracted from the tower bottom returns to the rectifying tower T2。
Example 5
The specific steps are the same as those in the embodiment 1, and the differences are only that:
the extraction agent is changed into 1, 2-propylene glycol, and the product purity is shown in table 1 after the operation is stable.
Example 6
The specific steps are the same as those in the embodiment 1, and the differences are only that:
the extraction agent is changed into formamide, and after the operation is stable, the purity of the product is shown in table 1.
Example 7
The specific steps are the same as those in the embodiment 1, and the differences are only that:
the extraction agent is changed into N-methyl-2-pyrrolidone, and the product purity is shown in table 1 after the operation is stable.
Example 8
The specific steps are the same as those in the embodiment 1, and the differences are only that:
the extractant is changed into diethylene glycol, and after the operation is stable, the purity of the product is shown in table 1.
Comparative example
The raw material composition, the feeding amount and the operation conditions are the same as those of the example 1, and the differences are only that: the results of the initial degree of the product obtained by direct rectification without addition of an extractant are shown in Table 1.
TABLE 1 summary of the results
Item Purity of n-hexane% Purity of 1, 2-dichloroethane%
Example 1 99.5 99.3
Example 2 99.6 99.4
Example 3 99.2 99.5
Example 4 98.6 99.6
Example 5 99.1 99.3
Example 6 99.4 99.4
Example 7 99.8 99.2
Example 8 98.8 99.5
Comparative example 80.0 75.0
In conclusion, the separation method of the mixed solution of the vinyl sulfate, the normal hexane and the 1, 2-dichloroethane is simple, easy to operate, high in safety, low in energy consumption, high in purity of the extracted product and high in product recovery rate. The purity of the n-hexane obtained by separation can reach more than 99.7 percent, the purity of the 1, 2-dichlorohexane can reach more than 99.8 percent, and the purity of the vinyl sulfate can reach more than 99.9 percent.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (2)

1. A separation method of a mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane is characterized by comprising the following steps:
(1) mixing solution containing vinyl sulfate, n-hexane and 1, 2-dichloroethane in a rectifying tower (T)1) Feeding at the bottom, collecting solution I with total mass fraction of n-hexane and 1, 2-dichloroethane more than 99.8% at the top of the tower, and collecting sulfur at the bottom of the towerSolution II with the mass fraction of vinyl acetate greater than 90%; wherein the rectifying column (T)1) The number of theoretical plates is 10-30, the operating pressure is 30-70 kPa, the temperature of a tower kettle is 30-80 ℃, and the reflux ratio is 0.1-5;
(2) pouring the solution II into a crystallizer (B)1) Cooling and filtering, returning the filtrate to the rectification column (T)1) The filter cake is vinyl sulfate with the purity of 99.8 percent;
(3) mixing the solution I with an extractant and then placing the mixture in a rectifying tower (T)2) Feeding at the bottom, extracting a normal hexane product at the top of the tower, and extracting an extracting agent and a solution III with the total mass fraction of 1, 2-dichloroethane of more than 99.8% at the bottom of the tower; wherein the rectifying column (T)2) The number of theoretical plates is 10-50, the temperature of a tower kettle is 50-120 ℃, and the reflux ratio is 1-10; the extractant is one or the combination of more than two of cyclohexanone, cyclohexanol, 1, 2-propylene glycol, N-dimethylaniline, ethylene glycol, formamide and diethylene glycol;
(4) subjecting the solution III to a rectification column (T)3) Feeding at the bottom, collecting 1, 2-dichloroethane product at the top of the column, collecting extractant at the bottom of the column, and returning the extractant to the rectifying column (T)2) Wherein the rectification column (T)3) The theoretical plate number of the tower is 10-50, and the temperature of the tower kettle is 60-150 ℃.
2. The method for separating vinyl sulfate, n-hexane and 1, 2-dichloroethane according to claim 1, wherein in the step (3), the mass ratio of the extracting agent to the solution I is 1-5: 1.
CN201810370863.6A 2018-04-23 2018-04-23 Method for separating mixed solution of vinyl sulfate, n-hexane and 1, 2-dichloroethane Active CN110386915B (en)

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