CN211755023U - Equipment for continuously producing ethylene sulfide - Google Patents
Equipment for continuously producing ethylene sulfide Download PDFInfo
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- CN211755023U CN211755023U CN201921616557.2U CN201921616557U CN211755023U CN 211755023 U CN211755023 U CN 211755023U CN 201921616557 U CN201921616557 U CN 201921616557U CN 211755023 U CN211755023 U CN 211755023U
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Abstract
The utility model provides a serialization production ethylene sulfide's equipment, equipment includes: the device comprises a continuous reactor, a feeding tank and a heat preservation storage tank which are connected with the upper end of the continuous reactor, a solid waste collector which is connected with the lower end of the continuous reactor, and a condenser and a gas-liquid separator which are connected with a gas outlet hole at the upper end of the continuous reactor, wherein a scraper plate which is contacted with the inner wall of the continuous reactor is arranged in the continuous reactor. The utility model discloses a continuous reaction improves the intermittent type cauldron formula among the prior art reaction for continuous reactor, and the raw materials is instantaneous reaction under reaction temperature, and the episulfide ethane that generates separates rapidly with other materials, and the cyanate powder of generation is discharged from the reactor bottom under scraping wall screw propulsion at gravity and agitator. The method is clean, pollution-free, stable in production index, less in manpower and beneficial to industrial scale production.
Description
Technical Field
The utility model relates to a continuous production episulfide ethane's equipment.
Background
At present, the main flow process route for producing diethylaminoethanethiol in China is to react ethylene carbonate and thiocyanate to generate thiirane, and then react diethylamine and thiirane to generate the diethylaminoethanethiol.
The same improvement is made on the method for preparing the ethylene sulfide in two patents of CN201710497589 and CN201710497588, and the yield of the ethylene sulfide is improved by adopting an intermittent feeding mode and controlling the reaction speed and the effective separation of a product and carbon dioxide. The ethylene carbonate reacts with thiocyanate to generate ethylene sulfide, the ethylene carbonate is liquid during the reaction, the thiocyanate is solid, the ethylene carbonate is both a reaction raw material and a solvent phase, and the thiocyanate and the ethylene carbonate are fully mixed for reaction through continuous stirring.
The applicant has found through research that the methods of the two patents still have certain technical defects. Cyanate has certain commercial value, but in the production process of the ethylene sulfide, the byproduct cyanate forms greasy dirt-like hard blocks at the bottom of the tank due to high temperature and is difficult to treat. The current industrialized treatment mode is to add water for high-temperature dissolution and repeatedly clean the reaction tank. The cyanate is further decomposed into carbonate, ammonium carbonate and the like in the process of adding water and heating for dissolution to form high-salt, high-COD and high-ammonia nitrogen wastewater, and the dissolving process is accompanied by pungent smell, so that the odor pollution is serious, the production site environment is very poor, the wastewater is extremely difficult to treat and is not beneficial to clean production, and meanwhile, the cyanate decomposition treatment with commercial value is contrary to the development concept of circular economy. In addition, the yield and quality of the product fractions still fluctuate due to manual batch operation, and the batch feeding causes high labor cost, which is not favorable for large-scale production.
Therefore, the development of clean, pollution-free and stable production index ethylene sulfide production equipment which requires less manpower and is beneficial to industrial scale amplification is urgently needed.
SUMMERY OF THE UTILITY MODEL
Therefore, the utility model aims at having the by-product cyanate difficult processing to present ethylene sulfide production facility to because the intermittent type throws the problem that product yield, quality fluctuation and the cost of labor are high that the material leads to, provide a clean, pollution-free, production index is stable, the personnel selection is few, be favorable to the enlarged ethylene sulfide production facility of industrialization scale.
The invention provides a device for continuously producing ethylene sulfide, which comprises the following components by referring to figure 1:
the continuous reaction is carried out in a reactor 1,
a feeding tank 2 and a heat preservation storage tank 3 which are connected with the upper end of the continuous reactor 1,
a solid waste collector 4 connected with the lower end of the continuous reactor 1,
a condenser and a gas-liquid separator which are connected with an air outlet at the upper end of the continuous reactor 1,
wherein, a scraper type stirrer (5) which is contacted with the inner wall of the continuous reactor (1) and extends to the outlet at the bottom end is arranged in the continuous reactor.
In a preferred embodiment of the present invention, the outer surface of the lower end of the continuous reactor 1 may be further provided with an oscillator 6; and a liquid atomizer 7 can be arranged between the heat-preservation storage tank 3 and the continuous reactor 1.
According to the equipment provided by the invention, the continuous reactor 1 is cylindrical or is in an inverted frustum shape with the diameter of the lower surface smaller than that of the upper surface, preferably, the continuous reactor 1 is in the inverted frustum shape, and the ratio of the radius of the upper top of the inverted frustum shape to the height can be 1: 5-10, preferably 1: 8-9. Wherein, the radius of the upper top refers to: maximum radius of the upper end of the continuous reactor 1. The continuous reactor 1 is in an inverted frustum shape, the diameter of the lower surface is smaller than that of the upper surface, and solid byproducts generated in the reaction can be continuously discharged from the bottom end of the reactor.
Preferably, a liquid delivery pump may be provided between the holding tank 3 and the liquid atomizer 7.
In order to achieve a better cyanate scraping effect and at the same time to provide a stirring effect for the reactants, the scraper 5 is preferably a screw type scraper. Preferably, a meter is arranged on the connecting pipeline of the feeding tank 2 and the heat preservation storage tank 3 which are respectively connected with the continuous reactor 1.
In a specific embodiment of the present invention, referring to fig. 1, thiocyanate and ethylene carbonate are charged into a continuous reactor 1 from a charge tank 2 and a holding tank 3, respectively. Preferably, the molar ratio of thiocyanate to ethylene carbonate is controlled to be about 1:1, for example, 1:0.9 to 1.1, preferably 1:0.95 to 1.05, more preferably 1:0.98 to 1.02, and most preferably 1: 1. Ethylene carbonate and thiocyanate are respectively continuously injected into a continuous reactor in a small drop shape and a small particle shape for rapid reaction, generated gases (ethylene sulfide and carbon dioxide) are continuously discharged through an outlet at the upper end of the reactor, the ethylene sulfide is separated and condensed to a storage tank, and generated solid by-product cyanate is continuously discharged through an outlet at the lower end of the reactor under the action of gravity and stirring and collected to the storage tank. Preferably, the connecting pipelines of the feeding tank 2 of thiocyanate and the heat-preservation storage tank 3 of ethylene carbonate respectively connected with the continuous reactor 1 are provided with one-way valves, and the solid waste collector 4 for receiving cyanate adopts a sealing device to prevent generated gas from leaking.
Preferably, the ethylene carbonate holding tank 3 and the continuous reactor 1 are provided with jacketed heating means. The solid waste collecting tank 4 is provided with a cooling device with a clamping sleeve, and the collecting tank 4 keeps the temperature below 30 ℃ in the process of continuously collecting the solid waste. In the apparatus, a vibrator 6 is used to continuously vibrate the outlet of the continuous reactor 1 to prevent solid waste powder from clogging the outlet.
Because of the danger of ethylene sulfide, the safe use mode in the actual production is that the ethylene sulfide is produced and used immediately, and a large amount of long-time storage is avoided. Therefore, the continuous production equipment designed by the invention can control the yield of the ethylene sulfide by reducing or adding the number of the ethylene sulfide continuous reactors connected with the liquid collector according to the actual production requirement, thereby realizing the instant production and use of the ethylene sulfide.
The equipment and the method of the invention carry out reaction according to the theoretical molar ratio, thereby reducing the material cost; the method avoids the generation of wastewater with three high contents, avoids the production fluctuation (quality, yield and cost), is easy to enlarge and scale, improves the production environment, reduces the labor cost and the like.
Drawings
Embodiments of the present invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a schematic diagram of the apparatus for continuously producing ethylene sulfide provided by the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, which are given for the purpose of illustration only and are not intended to limit the scope of the invention.
Example 1
This example uses the continuous reaction apparatus and process of the present invention to prepare ethylene sulfide.
Referring to the apparatus for continuously producing ethylene sulfide shown in FIG. 1, the continuous reactor 1 has an inverted conical shape (the ratio of the radius of the upper end to the height is 1: 8). The ethylene sulfide continuous production equipment comprises: the continuous reactor comprises a continuous reactor 1, a feeding tank 2 and a heat preservation storage tank 3 which are connected with the upper end of the continuous reactor 1, a solid waste collector 4 which is connected with the lower end of the continuous reactor 1, a condenser which is connected with an air outlet hole at the upper end of the continuous reactor 1, and a gas-liquid separator which is connected with the condenser.
Preheating a continuous reactor 1 to 130 ℃, starting a spiral scraper 5 for stirring, simultaneously starting an oscillator 6, feeding sodium thiocyanate into the continuous reactor 1 from a feeding tank 2, atomizing ethylene carbonate into the continuous reactor 1 through a liquid atomizer 7, and adjusting a meter to ensure that the sodium thiocyanate and the ethylene carbonate enter the continuous reactor 1 according to a molar ratio of 1: 1. The generated ethylene sulfide is condensed and collected in a liquid collector through a gas-liquid separator for further preparing the diethylaminoethanethiol.
After the reaction entered steady state, continuous 8 hour production data were collected: the dosage of ethylene carbonate is 2100kg, the dosage of sodium thiocyanate is 1875kg, the total yield of the ethylene sulfide is 1360kg, and the yield of solid waste is 500 kg.
The purity of the produced ethylene sulfide gas phase detection is 99.6%, and the yield is 97.8%.
This production line uses artifical 1 people.
The solid waste is powdery, 500kg of the solid waste is extracted by methanol and then is recovered by two-step crystallization, the crude product amount of the first crystallization is 441kg, the refined product amount is 406kg, the refined product purity is 96.1 percent, and the yield is 81.2 percent.
Example 2
This example uses the continuous reaction apparatus and process of the present invention to prepare ethylene sulfide.
Referring to example 1 and FIG. 1, there is shown an apparatus for continuously producing ethylene sulfide in which a continuous reactor has a reverse conical frustum shape having a ratio of an upper vertex radius to a height of 1: 8.5.
Preheating a continuous reactor 1 to 110 ℃, starting a spiral scraper 5 for stirring, simultaneously starting an oscillator 6, feeding sodium thiocyanate into the continuous reactor 1 from a feeding tank 2, atomizing ethylene carbonate into the continuous reactor 1 through a liquid atomizer 7, and adjusting a meter to ensure that the sodium thiocyanate and the ethylene carbonate enter the continuous reactor 1 according to a molar ratio of 1: 1. The generated ethylene sulfide is condensed and collected in a liquid collector through a gas-liquid separator for further preparing the diethylaminoethanethiol.
After the reaction entered steady state, continuous 8 hour production data were collected: the dosage of ethylene carbonate is 2100kg, the dosage of sodium thiocyanate is 1875kg, the yield of ethylene sulfide is 1357.5kg, and the yield of solid waste is 500 kg. The purity of the produced ethylene sulfide gas phase detection is 99.6%, and the yield is 97.6%. This production line uses artifical 1 people.
Comparative example 1
This comparative example used the existing batch tank reaction to prepare ethylene sulfide.
Adding 220kg of ethylene carbonate (0.52 time of the total feeding amount of the ethylene carbonate) into a reaction tank, heating to 55 ℃ for melting, stirring, adding 375kg of sodium thiocyanate, directly heating to 85 ℃ by starting steam, separating and collecting fractions by a coil heat exchanger and a cyclone gas-liquid separator after fractions are discharged, simultaneously dropwise adding 200kg of the remaining ethylene carbonate with the temperature of 75 ℃, and controlling the temperature in the dropwise adding process to be 100 ℃. After the ethylene sulfide is dripped, the temperature is continuously raised to 138 ℃, and the reaction is ended until no fraction is distilled out. The reaction and operation took 2 hours to give 270.8kg of ethylene sulfide, the purity by gas phase detection was 99.6%, and the yield was 97.5%.
The reaction takes 4 hours in total, 5 workers are used, the solid waste is oil-contaminated hard blocks, the production amount is 100kg, the solid waste is not recycled, the solid waste is directly and repeatedly soaked and cleaned by water with the temperature of more than 90 ℃, the cleaning process has heavy odor pollution, and the reaction takes 3 hours for treating the solid waste.
It can be seen through comparing embodiment 1 and 2 with comparative example 1, compare with the batch reactor among the prior art, the utility model discloses a continuous reactor has realized the effect clean, pollution-free, that the production index is stable, the personnel selection is few, be favorable to the large-scale production of industrialization.
Claims (11)
1. An apparatus for the continuous production of ethylene sulfide, the apparatus comprising:
a continuous reactor (1) for the continuous reaction,
a feeding tank (2) and a heat-preservation storage tank (3) which are connected with the upper end of the continuous reactor (1),
a solid waste collector (4) connected with the lower end of the continuous reactor (1),
a condenser and a gas-liquid separator which are connected with an air outlet at the upper end of the continuous reactor (1),
wherein, a scraper type stirrer (5) which is contacted with the inner wall of the continuous reactor (1) and extends to the outlet at the bottom end is arranged in the continuous reactor.
2. The apparatus according to claim 1, characterized in that the lower outer surface of the continuous reactor (1) is provided with an oscillator (6).
3. The apparatus according to claim 1, characterized in that a liquid atomizer (7) is arranged between the holding tank (3) and the continuous reactor (1).
4. The plant according to claim 1, wherein the continuous reactor (1) has an inverted frustum or cylindrical shape.
5. The apparatus of claim 4, wherein the ratio of the radius of the upper apex of the inverted frustum or cylinder to the height is 1: 8-9.
6. The apparatus of claim 1, wherein the scraper agitator (5) is a helical scraper.
7. The plant according to any one of claims 1 to 6, wherein meters are provided on the connection pipes of the feed tank (2) and the holding tank (3) to the continuous reactor (1), respectively.
8. The apparatus according to any one of claims 1 to 6, wherein a liquid delivery pump may be provided between the holding tank (3) and the liquid atomizer (7).
9. The plant according to any one of claims 1 to 6, wherein the connection lines of the feed tank (2) and the holding tank (3) to the continuous reactor (1) are equipped with one-way valves.
10. The apparatus according to any one of claims 1 to 6, wherein the solid waste collector (4) is a sealed device and has a jacketed temperature reduction device.
11. The apparatus according to any one of claims 1 to 6, wherein the holding tank (3) and the continuous reactor (1) each have a jacket heating apparatus.
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| CN201921616557.2U CN211755023U (en) | 2019-09-26 | 2019-09-26 | Equipment for continuously producing ethylene sulfide |
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| CN201921616557.2U CN211755023U (en) | 2019-09-26 | 2019-09-26 | Equipment for continuously producing ethylene sulfide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665449A (en) * | 2019-09-26 | 2020-01-10 | 保定加合精细化工有限公司 | Equipment for continuously producing ethylene sulfide |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665449A (en) * | 2019-09-26 | 2020-01-10 | 保定加合精细化工有限公司 | Equipment for continuously producing ethylene sulfide |
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