CN211226975U - Production device of vinyl sulfate - Google Patents
Production device of vinyl sulfate Download PDFInfo
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- CN211226975U CN211226975U CN202021317259.6U CN202021317259U CN211226975U CN 211226975 U CN211226975 U CN 211226975U CN 202021317259 U CN202021317259 U CN 202021317259U CN 211226975 U CN211226975 U CN 211226975U
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Abstract
The utility model discloses a production device of vinyl sulfate belongs to additive apparatus for producing technical field. The device comprises a synthesis reaction kettle, a rectifying kettle, an oxidation kettle, a premixing tank, a dehydration filter, a re-crystallizer and a dryer; temperature regulating systems are respectively arranged on the synthesis reaction kettle and the rectifying kettle and are connected with a vacuum pumping system; the synthesis reaction kettle is connected with the rectifying kettle, the oxidation kettle, the dehydration filter, the re-crystallizer and the dryer in sequence through a discharge pipeline; the oxidation kettle is connected with the premixing tank through a discharge pipeline and a circulating pipeline; and switch valves are respectively arranged on the feeding pipeline, the discharging pipeline and the circulating pipeline of each section connected with the synthesis reaction kettle, the rectifying kettle, the oxidation kettle, the premixing tank, the dehydration filter, the re-crystallizer and the dryer. The utility model provides a water washing and neutralization reaction after the apparatus for producing can avoid reacting reduces the three wastes and handles, and the reaction product of oxidation reaction unit is difficult for hydrolysising simultaneously.
Description
Technical Field
The utility model relates to an electrolyte additive apparatus for producing technical field, concretely relates to apparatus for producing of sulphuric acid vinyl ester.
Background
The Ethylene Sulfate (ES) can be used as an additive of the electrolyte of the lithium ion battery. The addition of the vinyl sulfate into the lithium ion battery electrolyte can effectively inhibit the reduction of the initial capacity of the lithium ion battery, increase the initial discharge capacity, reduce the expansion of the battery after high-temperature placement, improve the charge and discharge performance of the battery and prolong the cycle life of the battery.
The current methods for producing vinyl sulfate mainly comprise a direct addition method of sulfur trioxide and ethylene oxide, and a synthesis method of ethylene glycol and thionyl chloride. The direct addition of sulfur trioxide and ethylene oxide to prepare vinyl sulfate is to add sulfuric anhydride and ethylene oxide into dioxane at the same time for reaction, and to improve the yield to 80-90% by adjusting the material ratio and the reaction conditions. However, the raw materials used in the method are highly toxic and volatile, the pressure in the production process is high, and the measures for production facilities and safety are high. In contrast, the ethylene glycol and thionyl chloride react to prepare the ethylene sulfite, and then the ethylene sulfite is oxidized to obtain the vinyl sulfate, so that the reaction condition is mild, the process is simple, the production cost is low, and the method is an industrial mainstream process for producing the vinyl sulfate at present. However, in the production process, because the acid value of the intermediate product needs to be washed for many times, the yield is low, the waste water is high, the purity is not high, and the separated water phase needs to be extracted for many times, so that the process is complicated. Meanwhile, the oxidation reaction unit has the conditions of poor reaction effect and easy hydrolysis of reaction products.
Disclosure of Invention
The utility model discloses to the technical problem that preparation ethylene sulfate in-process need wash many times, extract and easily hydrolyze at the reaction product that the oxidation reaction unit obtained to the intermediate product among the above-mentioned background art, the utility model provides a production device of ethylene sulfate can avoid washing and neutralization reaction after the reaction, reduces the three wastes and handles, and the reaction product of oxidation reaction unit is difficult for hydrolysising simultaneously, and product yield is high, purity is good.
In order to solve the technical problem, the utility model provides a production device of vinyl sulfate, which comprises a synthesis reaction kettle, a rectifying kettle, an oxidation kettle, a premixing tank, a dehydration filter, a re-crystallizer and a dryer;
the synthesis reaction kettle and the rectifying kettle are respectively provided with a temperature regulating system and a stirrer, and are connected with a vacuum pumping system;
the synthesis reaction kettle is sequentially connected with the rectifying kettle, the oxidizing kettle, the dehydration filter, the re-crystallizer and the dryer through discharge pipelines; the oxidation kettle is connected with the premixing tank through a discharge pipeline and a circulating pipeline;
and switch valves are respectively arranged on the feeding pipeline, the discharging pipeline and the circulating pipeline of each section connected with the synthesis reaction kettle, the rectifying kettle, the oxidation kettle, the premixing tank, the dehydration filter, the re-crystallizer and the dryer.
Preferably, the device also comprises an intermediate product reflux tank; the intermediate product reflux tank is respectively connected with the rectifying kettle and the oxidation kettle through discharge pipelines.
Preferably, the device also comprises a heat exchanger; the heat exchanger is connected with the rectifying still through a discharge pipeline and a circulating pipeline and is connected with the intermediate product reflux tank through a discharge pipeline.
Preferably, the temperature regulating system comprises a steam pipeline, a circulating water feeding pipeline, a circulating water discharging pipeline and a cooling water pipeline, and the temperature in the synthesis reaction kettle and the temperature in the rectifying kettle are regulated through water circulation.
Preferably, a discharge pipeline between the oxidation kettle and the dehydration filter is connected with a sewage discharge system.
Preferably, the acid absorption system is connected with the vacuum-pumping system.
Preferably, the vacuum-pumping system comprises a vacuum tank and a vacuum pump.
Preferably, a kettle bottom viewing mirror is arranged at the kettle bottom of the oxidation kettle.
Preferably, the stirrer is a propeller-type or gate-type stirrer.
The utility model discloses compare in prior art and obtained following technological effect:
the utility model provides a vinyl sulfate's apparatus for producing, synthetic reation kettle and rectifying still all are connected with evacuation system, carry out the vacuum treatment operation to the intermediate product (the reaction liquid that contains the ethylene sulfite ester) that generates, have avoided the washing and neutralization reaction after the reaction, have saved the cost that the three wastes were handled, have improved the yield of intermediate product, the effectual economic nature that enlarges whole equipment.
The utility model discloses set up rectifying still, the raw materials carries out the back at synthetic reation kettle, carries out the rectification purification to intermediate product (the reaction liquid that contains ethylene sulfite), has improved the quality of intermediate product, has reduced the influence of impurity to follow-up workshop section, the effectual utilization ratio that has improved is favorable to improving the purity of ethylene sulfate product.
The utility model discloses set up the oxidation kettle and mix jar in advance, carry out the rectification purification back to intermediate product (the reaction solution that contains ethylene sulfite ester), the ethylene sulfite ester that the purity that will obtain is greater than 99.2% changes over to the oxidation kettle, and add dichloroethane in the oxidation kettle, dropwise add sodium hypochlorite solution and mix in the mixed liquid that obtains in advance, make aqueous phase and organic phase separation after mixing the completion in advance, change over to the jar in advance earlier organic phase, get rid of behind the aqueous phase, change over to the oxidation kettle into over to rethread circulation line, adopt and mix the technology in advance, make the intermediate product in organic phase by oxidation, thereby realize that the product is difficult to be hydrolyzed, the reaction process mole yield is high.
Drawings
Fig. 1 is a schematic structural diagram of a production device provided by the present invention;
FIG. 2 is a schematic structural view of a temperature regulating system in the middle synthesis reaction kettle of the present invention;
FIG. 3 is a schematic structural view of a temperature regulating system in a middle rectifying still of the present invention;
FIG. 4 is a schematic view of the connection between the oxidation kettle and the cooling water supply line and the cooling water drain line;
FIG. 5 is a schematic diagram of the novel vacuum pumping system;
wherein, the method comprises the following steps of 1-a synthesis reaction kettle, 2-a rectifying kettle, 3-an oxidation kettle, 4-a premixing tank, 5-a dehydration filter, 6-a re-crystallizer, 7-a dryer, 8-an intermediate product reflux tank, 9-a heat exchanger, 10, a kettle bottom sight glass, 11-a stirrer, 12-a sewage discharge system, 13-an acid absorption system, 14-a temperature regulation system, 141-a cooling water pipeline, 142-a circulating water supply pipeline, 143-a circulating water discharge pipeline, 144-a steam pipeline, 145-a cooling water supply pipeline, 146-a cooling water discharge pipeline, 15-a vacuum pumping system, 151-a vacuum tank and 152-a vacuum pump.
Detailed Description
The utility model provides a production device of vinyl sulfate, which comprises a synthesis reaction kettle 1, a rectifying still 2, an oxidation kettle 3, a premixing tank 4, a dehydration filter 5, a heavy crystallizer 6 and a dryer 7; the synthesis reaction kettle 1 and the rectifying kettle 2 are respectively provided with a temperature regulating system 14 and a stirrer 11, and the synthesis reaction kettle 1 and the rectifying kettle 2 are both connected with a vacuum pumping system 15; the synthesis reaction kettle 1 is sequentially connected with a rectifying kettle 2, an oxidation kettle 3, a dehydration filter 5, a heavy crystallizer 6 and a dryer 7 through discharge pipelines; the oxidation kettle 3 is connected with the premixing tank 4 through a discharge pipeline and a circulating pipeline; switch valves are respectively arranged on the feeding pipeline, the discharging pipeline and the circulating pipeline of each section connected with the synthesis reaction kettle 1, the rectifying kettle 2, the oxidation kettle 3, the premixing tank 4, the dehydration filter 5, the heavy crystallizer 6 and the dryer 7.
When the reactor works, raw materials of ethylene glycol and thionyl chloride enter a synthesis reaction kettle 1 to react to obtain reaction liquid containing vinyl sulfite, the obtained reaction liquid containing the vinyl sulfite is transferred into a rectifying kettle 2 through a discharge pipeline to be rectified and purified, the obtained ES with the purity of more than 99.2% is transferred into an oxidation kettle 3 through the discharge pipeline, dichloroethane is added into the oxidation kettle 3, sodium hypochlorite solution is dripped for premixing, stirring and standing are carried out after dripping is finished, a water phase and an organic phase are layered through standing, the organic phase is transferred into a premixing tank 4 through the discharge pipeline, the water phase in the oxidation kettle 3 is removed, and the organic phase in the premixing tank 4 is transferred into the oxidation kettle 3 through a circulating pipeline. Adjusting the pH value of an organic phase in the oxidation kettle 3 to 7-8, adding a catalyst, and dropwise adding a sodium hypochlorite solution for oxidation reaction to obtain a vinyl sulfate crude product; and transferring the obtained vinyl sulfate crude product into a dehydration filter 5, a recrystallization device 6 and a dryer 7 in sequence through a discharge pipeline for dehydration, recrystallization and drying in sequence to obtain the vinyl sulfate.
In order to make the reaction fully proceed, the internal stirrer 11 of the synthesis reaction kettle 1 is preferably a push type or frame type stirrer.
In order to facilitate the control of the reaction temperature, in the present invention, the temperature control system 14 preferably includes a steam line 144, a circulating water supply line 142, a circulating water discharge line 143, and a cooling water line 141, and the temperature in the synthesis reaction kettle 1 and the rectifying still 3 is controlled by water circulation.
To facilitate the evacuation, the evacuation system 15 of the present invention preferably includes a vacuum tank 151 and a vacuum pump 152.
In order to facilitate the absorption of hydrochloric acid by-products generated in the reaction, the present invention preferably further comprises an acid absorption system 13, wherein the acid absorption system 13 is connected to the vacuum pumping system 15.
In order to facilitate separation and storage of the ES with the purity of more than 99.2 percent, the utility model preferably also comprises an intermediate product reflux tank 8; the intermediate product reflux tank 8 is respectively connected with the rectifying still 2 and the oxidation still 3 through discharge pipelines, and after rectification and purification are carried out, the obtained ES with the purity of more than 99.2 percent is firstly transferred into the intermediate product reflux tank 8 and then transferred into the oxidation still. The utility model discloses in, the preferred filler formula rectifying still that adopts stainless wire net filler of rectifying still 2.
In order to rapidly cool the ES with the purity of more than 99.2 percent after rectification and purification and facilitate the subsequent oxidation reaction, the utility model preferably further comprises a heat exchanger 9; the heat exchanger 9 is connected with the rectifying still 2 through a discharge pipeline and a circulating pipeline, and is connected with the intermediate product reflux tank 8 through a discharge pipeline.
In order to conveniently observe the separation condition of the water phase and the organic phase obtained by the standing separation after the oxidation reaction is finished, the utility model discloses in the bottom of the kettle of the oxidation kettle 3 is preferably installed with the kettle bottom viewing mirror 10. In order to make the reaction proceed sufficiently, the stirrer 11 inside the oxidation reactor 3 is preferably a propeller-type or frame-type stirrer.
In order to facilitate the cooling of the oxidation kettle 3, the utility model discloses in, oxidation kettle 3 is preferred to be connected with cooling water supply line 145 and cooling sewer line 146.
In order to facilitate the treatment of the water phase obtained by the standing separation and the wastewater obtained after the dehydration, the utility model discloses the discharge pipeline between the oxidation kettle 3 and the dehydration filter 5 is preferably connected with the sewage system 12.
In order to dry quickly and sufficiently, in the present novel usage, the dryer 7 is preferably a vacuum dryer.
In order to further illustrate the present invention, the following embodiments are described in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
Before starting up, purging the whole system to test density, starting an acid absorption system, adding thionyl chloride into a synthesis reaction kettle, dropwise adding industrial-grade ethylene glycol, controlling the temperature of the system to be not more than 30 ℃, continuing stirring for 2 hours after dropwise adding, then heating to 50 ℃, carrying out heat preservation reaction until no raw material ethylene glycol remains after gas chromatography detection, reducing pressure at constant temperature, and vacuumizing under the condition of-0.1 Mpa to prepare the reaction liquid containing the ethylene sulfite.
And transferring the reaction liquid containing the ethylene sulfite into a rectifying still, keeping the pressure in the rectifying still at-0.1 MPa, controlling the reflux ratio to be 5:1, continuously extracting front fraction, switching to an intermediate product reflux tank when the ES content reaches more than 99.2 percent, stopping extraction until the material in the rectifying still is less than 50kg, cooling, and balancing the pressure by nitrogen.
Adding ethylene sulfite and dichloroethane with the purity of more than 99.2 percent in an intermediate product reflux tank into an oxidation kettle as solvents, starting cooling water, controlling the temperature of the oxidation kettle at 0-10 ℃, starting dropwise adding a sodium hypochlorite solution with the available chlorine of 12 percent under normal pressure, and dropwise adding for 1h (the reaction temperature is not more than 10 ℃). After the dropwise addition, stirring is continued for 1h, and standing is carried out for 0.5 h. Slowly separating liquid through a kettle bottom sight glass, flowing the lower layer organic phase into a premixing tank by gravity, and pressing the organic phase into an oxidation kettle after the upper layer wastewater is treated.
Adjusting the pH value of an organic phase in an oxidation kettle to 7 by adding sodium bicarbonate solid, adding a catalyst of ruthenium trichloride, cooling the temperature of the reaction kettle to 3 ℃, then dropwise adding a sodium hypochlorite solution with 12% of available chlorine into the oxidation kettle, controlling the reaction temperature not to exceed 10 ℃, sampling, carrying out gas chromatography detection and analysis on a sample without the ethylene sulfite, finishing dropwise adding, preserving heat for 1h, and standing for liquid separation to obtain a crude ethylene sulfate product.
And dehydrating the crude product of the vinyl sulfate, and recrystallizing and drying the dehydrated crude product of the vinyl sulfate in vacuum to obtain the high-purity vinyl sulfate.
The purity, water content, acid value and molar yield of the obtained high-purity vinyl sulfate were measured, and the specific results were 99.61% in purity, 45ppm in water content, 45ppm in acid value and 92.18% in molar yield.
The utility model discloses a concrete example is applied to explain the principle and the implementation mode of the utility model, and the explanation of the above example is only used to help understand the method and the core idea of the utility model; meanwhile, for the general technical personnel in the field, according to the idea of the present invention, there are changes in the concrete implementation and the application scope. In summary, the content of the present description should not be construed as a limitation of the present invention.
Claims (9)
1. A production device of vinyl sulfate is characterized by comprising a synthesis reaction kettle, a rectifying kettle, an oxidation kettle, a premixing tank, a dehydration filter, a re-crystallizer and a dryer;
the synthesis reaction kettle and the rectifying kettle are respectively provided with a temperature regulating system and a stirrer, and are connected with a vacuum pumping system;
the synthesis reaction kettle is sequentially connected with the rectifying kettle, the oxidizing kettle, the dehydration filter, the re-crystallizer and the dryer through discharge pipelines; the oxidation kettle is connected with the premixing tank through a discharge pipeline and a circulating pipeline;
and switch valves are respectively arranged on the feeding pipeline, the discharging pipeline and the circulating pipeline of each section connected with the synthesis reaction kettle, the rectifying kettle, the oxidation kettle, the premixing tank, the dehydration filter, the re-crystallizer and the dryer.
2. The production apparatus according to claim 1, further comprising an intermediate product return tank; the intermediate product reflux tank is respectively connected with the rectifying kettle and the oxidation kettle through discharge pipelines.
3. The production device of claim 2, further comprising a heat exchanger; the heat exchanger is connected with the rectifying still through a discharge pipeline and a circulating pipeline and is connected with the intermediate product reflux tank through a discharge pipeline.
4. The production plant according to claim 1, wherein the temperature regulation system comprises a steam line, a recycle water supply line, a recycle water drain line and a cooling water line, and the temperature in the synthesis reaction kettle and the rectification kettle is regulated by water circulation.
5. The production device according to claim 1, wherein a discharge line between the oxidation kettle and the dehydration filter is connected to a sewage system.
6. The production apparatus according to claim 1, further comprising an acid absorption system connected to the vacuum pumping system.
7. The production apparatus as claimed in claim 1, wherein the vacuum pumping system comprises a vacuum tank and a vacuum pump.
8. The production device of claim 1, wherein the bottom of the oxidation kettle is provided with a kettle bottom sight glass.
9. The production device according to claim 1, wherein the agitator is a pusher-type or gate-type agitator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021317259.6U CN211226975U (en) | 2020-07-08 | 2020-07-08 | Production device of vinyl sulfate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021317259.6U CN211226975U (en) | 2020-07-08 | 2020-07-08 | Production device of vinyl sulfate |
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| CN211226975U true CN211226975U (en) | 2020-08-11 |
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| CN202021317259.6U Active CN211226975U (en) | 2020-07-08 | 2020-07-08 | Production device of vinyl sulfate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022007259A1 (en) * | 2020-07-08 | 2022-01-13 | 山东海科新源材料科技股份有限公司 | Method for preparing ethylene sulfate |
| CN117903109A (en) * | 2023-12-29 | 2024-04-19 | 江苏瀚康新材料有限公司 | Process for preparing vinyl sulfate by micro-channel reaction |
-
2020
- 2020-07-08 CN CN202021317259.6U patent/CN211226975U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022007259A1 (en) * | 2020-07-08 | 2022-01-13 | 山东海科新源材料科技股份有限公司 | Method for preparing ethylene sulfate |
| CN117903109A (en) * | 2023-12-29 | 2024-04-19 | 江苏瀚康新材料有限公司 | Process for preparing vinyl sulfate by micro-channel reaction |
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Address after: 257000 23 Zoucheng Road, Shengli Industrial Park, Dongying District, Dongying City, Shandong Province Patentee after: Shandong Haike Xinyuan material technology Co., Ltd Address before: No. 23, Zoucheng Road, Shengli Industrial Park, Dongying City, Shandong Province Patentee before: DONGYING HI-TECH SPRING CHEMICAL INDUSTRY Co.,Ltd. |