CN114591205A - Process for joint production of methyl mercaptan and methyl sulfide - Google Patents
Process for joint production of methyl mercaptan and methyl sulfide Download PDFInfo
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- CN114591205A CN114591205A CN202210308232.8A CN202210308232A CN114591205A CN 114591205 A CN114591205 A CN 114591205A CN 202210308232 A CN202210308232 A CN 202210308232A CN 114591205 A CN114591205 A CN 114591205A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/02—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
- C07C319/08—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by replacement of hydroxy groups or etherified or esterified hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/14—Preparation of thiols, sulfides, hydropolysulfides or polysulfides of sulfides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
Abstract
The invention relates to the technical field of production of methyl mercaptan and methyl sulfide, in particular to a process for jointly producing methyl mercaptan and methyl sulfide, which comprises the steps of S101, circularly heating a reaction system; step S102, feeding materials into a reaction system; step S103, extracting reaction products; and S104, rectifying the oil phase after treatment. The beneficial effects of the invention are as follows: the production process of the methyl mercaptan and the methyl sulfide shares a set of device to carry out combined safe and environment-friendly production; the device has the advantages of high yield, high equipment utilization rate, low production cost, no side reaction, high safety, high raw material conversion rate and the like, is favorable for energy conservation and consumption reduction, improves the competitiveness of the device, can effectively control the yield of the methyl mercaptan and the methyl sulfide by adjusting the raw material feeding proportion according to market conditions, and flexibly adjusts the product yield, thereby realizing the long, stable, safe, reliable and continuous production of the device at the same time.
Description
Technical Field
The invention relates to the technical field of production of methyl mercaptan and methyl sulfide, in particular to a combined production process of methyl mercaptan and methyl sulfide.
Background
Methyl mercaptan is used as an important organic synthesis intermediate and is mainly used for synthesizing materials, pesticides, medicines and the like. Such as methionine, fenthion, bifenthrin, propaphos, prometryn, etc., and also for the production of methane sulfonyl chloride, methylthiopropanol, etc., intermediates. Particularly for synthesizing methionine, the demand of methionine is continuously increased along with the development and rise of the feed additive industry in recent years, and the production development of methyl mercaptan is stimulated;
the dimethyl sulfide is colorless to light yellow transparent volatile liquid, is an important organic intermediate, solvent and edible spice, belongs to fine chemical products, and has wide application. When used as the raw material of an intermediate compound, the compound can be used for producing dimethyl sulfoxide, dimethyl sulfone, methionine and pesticides; when used as a solvent, the solvent is organic compounds, resin, inorganic compounds, solvents of polymerization reaction and cyanidation reaction, analytical reagents, polyacrylonitrile and other synthetic fiber spinning and hydraulic oil;
the synthetic method of methyl mercaptan mainly comprises the following steps: the method comprises a sodium hydrosulfide-dimethyl sulfate method, a methyl chloride-sodium hydrosulfide method, a thiourea-dimethyl sulfate method and the like, wherein when the sodium hydrosulfide-dimethyl sulfate method is adopted for production, the process is simple, the operation is easy, the investment cost is low, but equipment and pipeline blockage faults are easy to occur in the production process, the sodium sulfate waste liquid is discharged more, the environmental pollution is serious, when the methyl chloride-sodium hydrosulfide method is adopted for production, the production is simple, the equipment quantity is small, the investment is low, but the production cost is high, the product yield is low, the side reactions are more, the pollution is serious, and when the thiourea-dimethyl sulfate method is adopted for production, the product yield is high, the pollution is small, but the raw materials are expensive and the product cost is higher;
the synthetic method of the dimethyl sulfide mainly comprises the following steps: the carbon disulfide method and the sodium sulfide method have the disadvantages of low product yield, high energy consumption, serious pollution and incapability of continuous production in the production process.
In conclusion, the production process can only carry out independent production on the methyl mercaptan and the dimethyl sulfide, and the conditions of serious environmental pollution, low yield, high cost and the like exist in the production process.
Therefore, a process for the co-production of methyl mercaptan and methyl sulfide is needed to overcome the above problems.
Disclosure of Invention
In order to solve the problems, the invention provides a process for coproducing methyl mercaptan and methyl sulfide, which solves the problem that methyl mercaptan and methyl sulfide cannot be produced simultaneously and continuously in the prior art, and achieves the purpose of solving the problems in the background art.
In order to achieve the purpose, the invention specifically adopts the following technical scheme:
the method comprises the following steps:
step S101, introducing molten salt with the temperature of 170 ℃ into the shell pass of a synthesis reaction tower to heat the synthesis reaction tower to 320 ℃, and simultaneously adding hydrogen sulfide with the pressure of 1.0Mpa and the temperature of 85 +/-5 ℃ to vulcanize a catalyst in the synthesis reaction tower, so that the temperature of the reaction tower is raised to 290 ℃ and the pressure is 1.0 Mpa; step S102, after the methanol is vaporized, adjusting the molar ratio of hydrogen sulfide to methanol entering the reaction raw material feed to be 1.1: 1, entering a synthesis reaction tower to generate a reaction product under the action of a catalyst; step S103, cooling the reaction product to 40 ℃, separating the reaction product through a three-phase separation tank under the pressure of 0.8Mpa, and introducing an oil phase obtained after separation into a water extraction tower to obtain a treated oil phase; wherein the oil phase after treatment contains crude methyl mercaptan and crude methyl sulfide; and S104, rectifying the treated oil phase to obtain a methyl mercaptan product and a methyl sulfide product.
As a further explanation of the above technical solution:
step S101 specifically includes: the molten salt is heated to 170 ℃ by an electric heater of a molten salt tank, and then the synthesis reaction tower is circularly heated to 320 ℃ with the temperature rise not more than 30 ℃/h.
Step S101 specifically includes: hydrogen sulfide at 40 deg.c and 0.5MPa is fed into the hydrogen sulfide inlet tank and fed via the hydrogen sulfide compressor into the hydrogen sulfide outlet tank to stabilize pressure to 1.0MPa and 85 deg.c +/-5 deg.c.
Step S102 specifically includes: the methanol feed pump pressurizes methanol to 1.2MPa, and the methanol is then fed to a methanol vaporizer to vaporize the methanol.
Step S103 specifically includes: cooling the reaction product to 140 ℃ through a reaction raw material/product heat exchanger, then cooling to 40 ℃ through a double-stage reaction product cooler, adding the reaction product into a three-phase separation tank after the pressure is 0.8Mpa, and then separating oil phase, water phase and gas phase; and absorbing the methanol in the oil phase through a water extraction tower to obtain a treated oil phase.
Step S104 specifically includes: firstly, rectifying and recovering methyl mercaptan by a methyl mercaptan rectifying tower to obtain a methyl mercaptan product, and then rectifying and recovering methyl sulfide by a methyl sulfide rectifying tower to obtain a methyl sulfide product.
The invention has the beneficial effects that:
1. the production device jointly produces two products of methyl mercaptan and methyl sulfide, and can realize the simultaneous production with long device period, stability, safety, reliability and continuity;
2. the conversion rate of the raw materials is as high as 94%, the amount of the circulating raw materials is small, and the operation cost is low;
3. the yield of the product is realized by adjusting the proportion of the reaction raw materials, and the product is flexibly adjusted and has strong adaptability according to market conditions;
4. the investment and the production cost are low, no other pollution by-products are generated in the production, the safety and the environmental protection are realized, and the environmental pollution is avoided.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a schematic flow chart of the present invention.
In the figure: 1. a molten salt bath electric heater; 2. a molten salt pump; 3. a synthesis reaction tower; 4. a hydrogen sulfide compressor; 5. hydrogen sulfide enters the gas tank; 6. discharging the gas tank; 7. a regulating valve; 8. a methanol feed tank; 9. a methanol feed pump; 10. a methanol vaporizer; 11. two regulating valves; 12. three regulating valves; 13. a reaction feed/product heat exchanger; 14. an electric heater for reaction raw materials; 15. a three-phase separation tank; 16. a gas phase regulating valve; 17. a two-stage reaction product cooler; 18. four regulating valves; 19. five regulating valves; 20. a water extraction column; 21. a methyl mercaptan rectification column; 22. a bottom reboiler; 23. a tower top condenser; 24. a methyl mercaptan overhead reflux tank; 25. six regulating valves; 26. a methyl mercaptan product cooler; 27. a methyl sulfide rectifying tower; 28. a second tower bottom reboiler; 29. a second tower top condenser; 30. a dimethyl sulfide reflux tank; 31. seven regulating valves; 32. a feed buffer tank; 33. a tower bottom kettle; 34. a heavies vaporizer; 35. and (4) a collection tank.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and are not intended to limit the scope of the present invention.
Referring to fig. 1 to 2, the invention discloses a process for jointly producing methyl mercaptan and methyl sulfide, which comprises the following steps:
step S101, adding molten salt with the temperature of 170 ℃ into a synthesis reaction tower 3 to heat the synthesis reaction tower 3 to 320 ℃, and simultaneously adding hydrogen sulfide with the pressure of 1.0Mpa and the temperature of 85 +/-5 ℃ to vulcanize a catalyst in the synthesis reaction tower 3, so that the temperature of the synthesis reaction tower 3 is raised to 320 ℃ and the pressure is 1.0 Mpa;
step S101 specifically includes: after the molten salt is heated to 170 ℃ by the electric heater 1 of the molten salt tank, circularly heating the synthesis reaction tower 3 to 320 ℃ with the temperature rise not more than 30 ℃/h;
step S101 specifically includes: feeding hydrogen sulfide with the temperature of 40 ℃ and the pressure of 0.5Mpa into a hydrogen sulfide inlet tank 5, adding the hydrogen sulfide into a hydrogen sulfide outlet tank 6 through a hydrogen sulfide compressor 4, stabilizing the pressure to 1.0Mpa, and controlling the temperature to be 85 ℃ +/-5 ℃;
step S102, after the methanol is vaporized, adjusting the molar ratio of hydrogen sulfide to methanol to be 1.1: 1, entering a reaction raw material electric heater 14 and then entering a synthesis reaction tower 3 to generate a reaction product;
step S102 specifically includes: pressurizing methanol to 1.2Mpa by methanol feeding pump 9, adding into methanol vaporizer 10, and vaporizing the methanol;
step S103, cooling the reaction product to 40 ℃, separating the reaction product through a three-phase separation tank 15 under the pressure of 0.8Mpa, and introducing the oil phase obtained after separation into a water extraction tower 20 to obtain an oil phase after methanol treatment; wherein the oil phase after treatment contains crude methyl mercaptan and crude methyl sulfide;
step S103 specifically includes: cooling the reaction product to 170 ℃ through a reaction raw material/product heat exchanger 13, then cooling to 40 ℃ through a bipolar reaction product cooler, adding the reaction product into a three-phase separation tank 15 after the pressure is 0.8Mpa, and then performing oil phase, water phase and gas phase separation; absorbing the methanol in the oil phase through a water extraction tower 20 to obtain a treated oil phase;
step S104, rectifying the treated oil phase to obtain a methyl mercaptan product and a methyl sulfide product;
step S104 specifically includes: firstly, the methyl mercaptan is rectified and recovered by a methyl mercaptan rectifying tower 21 to obtain a methyl mercaptan product, and then the methyl sulfide is rectified and recovered by a methyl sulfide rectifying tower 27 to obtain a methyl sulfide product.
As shown in figure 1 of the drawings, in which,
step S101 is that the reaction system circularly heats up; firstly, starting a molten salt tank electric heater 1, controlling the temperature of molten salt to be 170 ℃, starting a molten salt pump 2 with the pressure of 0.3Mpa to enter a shell pass of a synthesis reaction tower 3 to heat up, vulcanizing a catalyst in the synthesis reaction tower 3, starting a hydrogen sulfide compressor 4 to carry out system circulation heating, preparing hydrogen sulfide with the supply temperature of 40 ℃ and the pressure of 0.5Mpa from hydrogen sulfide, entering a hydrogen sulfide inlet tank 5, pressurizing the hydrogen sulfide to the pressure of 1.0Mpa through the hydrogen sulfide compressor 4 and the temperature of 85 +/-5 ℃, then entering an outlet tank 6 to stabilize the pressure, entering the synthesis reaction tower 3 to carry out circulation heating, and regulating and controlling the outlet pressure of the hydrogen sulfide compressor 4 through a regulating valve 7; when the temperature of the synthesis reaction tower 3 is raised to 320 ℃ and the pressure is 1.0Mpa, the stable temperature and pressure enter the next reaction for feeding;
step S102 is feeding a reaction system; normal temperature methanol in a methanol storage tank is sent into a methanol feeding tank 8, then the methanol is pressurized to 1.2Mpa by a methanol feeding pump 9 and then enters a methanol vaporizer 10 for methanol vaporization, the shell side of the methanol vaporizer 10 is heated by steam of 0.8Mpa, and the outlet temperature of the methanol vaporizer 10 is controlled to be 100 +/-5 ℃ by a two-regulating valve 11; the reaction methanol passes through a methanol vaporizer 10, and the molar ratio of the methanol to the hydrogen sulfide entering the synthesis reaction tower 3 is regulated to be 1.1: 1 (according to market conditions, the feeding amount of reaction raw materials, namely methanol and hydrogen sulfide, can be adjusted, the yield of methyl mercaptan and methyl sulfide can be controlled, the product is flexible to adjust, strong in adaptability and convenient for actual production), then reaction heat is recycled through a reaction raw material/product heat exchanger 13, then the reaction heat is heated and heated through a reaction raw material electric heater 14 and enters a synthesis reaction tower 3, the inlet temperature of the synthesis reaction tower 3 is controlled to be 290 +/-5 ℃, the outlet temperature is controlled to be 320 +/-5 ℃, the pressure is 1.0-1.1MPa, the pressure controls the pressure of a reaction system through a gas phase regulating valve 16 arranged on a three-phase separation tank 15, a reaction product is obtained after the reaction tower 3, and the methanol and hydrogen sulfide can continuously carry out feeding work, so that continuous production is realized;
step S103, extracting a reaction product; the reaction product is cooled to 140 ℃ after heat is recovered by a reaction raw material/product heat exchanger 13, then enters a two-stage reaction product cooler 17, is cooled to 40 ℃ and enters a three-phase separation tank 15 under the pressure of 0.8Mpa to be separated into an oil phase, a water phase and a gas phase, the gas phase is adjusted by a four-regulating valve 18 and is merged into a hydrogen sulfide gas inlet tank 5, then returns to a reaction system to continue to react, the water phase contains trace methanol, the water phase is sent to a wastewater recovery system through a five-regulating valve 19, the water phase is recycled, the water in the water phase is treated to be used as process water supplement, the methanol in the water phase is recovered and returned to a methanol inlet tank 8, the oil phase enters a water extraction tower 20, the methanol is dissolved in the water, the methyl mercaptan and the methyl sulfide are not dissolved in the water, the methyl mercaptan and the methyl sulfide are separated by a liquid-liquid extraction method, the alcohol-containing wastewater at the bottom of the water extraction tower 20 is pumped out by a tower kettle pump 33 and divided into two ways, one way is sent to the water extraction tower 20 to reflux and absorb the methanol, the other path is subjected to steam stripping separation and recycling, so that a treated oil phase is obtained;
step S104 is the rectification of the oil phase after the treatment, the separation and purification are carried out by adopting the rectification principle according to the difference of the boiling points of the methyl mercaptan and the methyl sulfide (as shown in Table 1), the crude methyl mercaptan and the crude methyl sulfide at the top of the water extraction tower 20 enter a feeding buffer tank 32, (the material treated by the water extraction tower 20 contains a small amount of alcohol-containing wastewater, the alcohol-containing wastewater is brought to the rear system and cannot be removed, and the product quality is influenced, so the alcohol-containing wastewater is cut off, and the alcohol-containing wastewater is collected by a collecting tank 35), the material completely removed of the alcohol-containing wastewater enters the middle lower part of a methyl mercaptan rectification tower 21, a tower bottom reboiler 22 is heated to control the temperature of the methyl mercaptan rectification tower 21 to be 55 ℃, the pressure to be 0.6MPa, the methyl mercaptan in the tower is completely vaporized, the top of the methyl mercaptan is condensed by a tower top condenser 23 and then enters a methyl mercaptan tower top reflux tank 24, the temperature is 40 ℃, and the pressure is regulated by a six-regulating valve 25 and is merged into a tail gas system, one path is extracted by a methyl mercaptan tower top reflux tank 24 to be used as methyl mercaptan tower top reflux, and the other path is cooled by a methyl mercaptan product cooler 26 and then is sent to a methyl mercaptan product storage tank at the temperature of 20 ℃; crude methyl sulfide at the bottom of a methyl mercaptan rectifying tower 21 is pressed to the middle lower part of a methyl sulfide rectifying tower 27, a reboiler 28 at the bottom of a second tower of the methyl sulfide rectifying tower 27 is subjected to steam heating and steam stripping, the temperature of a tower kettle is controlled at 120 ℃ and the pressure is 0.35Mpa, methyl sulfide in the tower is completely vaporized, a condenser 29 at the top of the second tower is cooled by low-temperature water at 7 ℃, the condensed methyl sulfide enters a methyl sulfide reflux tank 30 at 20 ℃, the pressure is regulated by a seven-regulating valve 31 and is merged into a tail gas system, the methyl sulfide product is pumped out to be taken as reflux at the top of the tower, the other path is sent to a methyl sulfide product storage tank, a small amount of polythiol component is arranged at the bottom of the methyl sulfide rectifying tower 27, because the polythiol component is heavier than methyl sulfide and has a higher boiling point, when the temperature at the bottom of the tower is controlled to be too high, the quality of the methyl sulfide product cannot be vaporized at the top of the polythiol vaporized at the bottom of the tower, when a large amount of heavy components is accumulated, the methyl sulfide is indirectly heated and vaporized by steam through a heavy component vaporizer 34, sending the mixture into an incinerator for treatment;
as shown in figure 1, the production of the methyl mercaptan and the methyl sulfide shares a set of production device to carry out combined safe and environment-friendly production, the investment and the production cost are low, the long-period, stable, safe, reliable and continuous simultaneous production of the methyl mercaptan and the methyl sulfide can be realized, no other pollution byproducts are produced in the production, the safety and the environment protection are realized, and the environmental pollution is avoided.
TABLE 1
As further illustration of the present application:
the reaction equation of the present application is:
methyl mercaptan CH3OH+H2S-CH3SH+H2O
Dimethyl sulfide 2CH3OH+H2S-CH3SCH3+2H2O；
The method adopts a methanol-hydrogen sulfide catalytic synthesis process, and according to different characteristics of methyl mercaptan and methyl sulfide molecules, a catalyst of a reaction tower is a noble metal catalyst, has wide selectivity on methyl mercaptan and methyl sulfide, and can meet the requirement of simultaneous production of methyl mercaptan and methyl sulfide, and is characterized in that the components in the synthesis process are 45 wt% -50 wt% of methyl sulfide, 45 wt% -50 wt% of methyl mercaptan, 1.2 wt% -2.5 wt% of methanol, 1.8 wt% -2.5 wt% of water and 0.05 wt% -0.2 wt% of hydrogen sulfide; the conversion rate of the raw materials is up to 94 percent, and the method has the characteristics of small amount of circulating raw materials and low operation cost;
the synthesis reaction tower 3 is a shell-and-tube constant temperature reaction tower, the reaction speed is high, the reaction process of the process belongs to exothermic reaction, and reaction heat is taken away through molten salt circulation to reach stable reaction temperature; mixing the raw materials, and introducing the mixture into a synthesis reaction tower 3, wherein the reaction pressure is 1.0-1.1Mpa, the inlet temperature of the reaction tower is controlled by 290 ℃ by a raw material electric heater in the reaction tower, and the reaction temperature of 320-325 ℃ is kept by two groups of electric heaters in a molten salt tank; hydrogen sulfide is excessive in the reaction process, and the yield of the product is selectively adjusted by controlling the feeding amount of methanol; the reaction raw materials are processed by a high-temperature catalyst to generate methyl mercaptan, methyl sulfide and water, alcohol-containing wastewater is removed by extraction, and an industrial-grade methyl mercaptan product and an industrial-grade methyl sulfide product are obtained by rectification and purification.
A raw material distribution area is arranged in the synthesis reaction tower 3, the raw material distribution area is a porous container, and materials are uniformly distributed; the synthetic reaction tower 3 is also provided with ceramic ball fillers which are divided into five layers of fillers, and the fillers comprise phi 8, phi 5, phi 3, phi 5 and phi 8 respectively, so that reaction materials can be fully mixed, the catalyst can be protected from being impacted, and the service life of the catalyst is prolonged.
As further illustration of the present application: the method adopts hydrogen sulfide and methanol as production raw materials to realize the combined production of methyl mercaptan and dimethyl sulfide; specifically, hydrogen sulfide and methanol react with a catalyst in a synthesis reaction tower to obtain a reaction product, the reaction product is separated by a three-phase separation tank, and then an oil phase is treated, wherein the oil phase is firstly treated by a water extraction tower and then rectified to obtain a methyl mercaptan product and a methyl sulfide product.
It should be noted that in the description of the present invention, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicating the directions or positional relationships are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The terms "comprises," "comprising," or any other similar term are intended to cover a non-exclusive inclusion, such that a process, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, article, or apparatus.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
Claims (6)
1. The process for jointly producing the methyl mercaptan and the methyl sulfide adopts hydrogen sulfide and methanol as raw materials to jointly produce a methyl mercaptan product and a methyl sulfide product, and is characterized by comprising the following steps of:
step S101, adding molten salt with the temperature of 170 ℃ into a synthesis reaction tower to heat the synthesis reaction tower to 320 ℃, and simultaneously adding hydrogen sulfide with the pressure of 1.0Mpa and the temperature of 85 +/-5 ℃ to vulcanize a catalyst in the synthesis reaction tower, so that the temperature of the reaction tower is raised to 320 ℃ and the pressure is 1.0 Mpa;
step S102, after the methanol is vaporized, adjusting the molar ratio of hydrogen sulfide to methanol entering into the reaction raw material feed to be 1.1: 1, entering a synthesis reaction tower to generate a reaction product;
step S103, cooling the reaction product to 40 ℃, separating the reaction product through a three-phase separation tank under the pressure of 0.8Mpa, and introducing the oil phase obtained after separation into a water extraction tower to obtain a treated oil phase; wherein the oil phase after treatment contains crude methyl mercaptan and crude methyl sulfide;
and S104, rectifying the treated oil phase to obtain a methyl mercaptan product and a methyl sulfide product.
2. The process for the joint production of methyl mercaptan and methyl sulfide as claimed in claim 1, wherein step S101 specifically comprises:
and heating the molten salt to 170 ℃ through an electric heater of a molten salt tank, and then circularly heating the synthesis reaction tower to 320 ℃ with the temperature not higher than 30 ℃/h.
3. The process for the joint production of methyl mercaptan and methyl sulfide as claimed in claim 2, wherein step S101 specifically comprises:
hydrogen sulfide at 40 ℃ +/-10 ℃ and 0.5Mpa is fed into a hydrogen sulfide inlet tank, and is added into a hydrogen sulfide outlet tank through a hydrogen sulfide compressor to be stabilized to 1.0Mpa and at 85 ℃ +/-5 ℃.
4. The process for the joint production of methyl mercaptan and methyl sulfide as claimed in claim 1, wherein step S102 specifically comprises:
the methanol feed pump pressurizes methanol to 1.2MPa, and the methanol is then fed to a methanol vaporizer to vaporize the methanol.
5. The process for the joint production of methyl mercaptan and methyl sulfide as claimed in claim 1, wherein step S103 specifically comprises:
the temperature of a reaction product discharged from the reaction tower is 320 ℃, the temperature of the reaction raw material is raised to 210 ℃ through a reaction raw material/product feeding and discharging heat exchanger, the temperature of the reaction product is lowered to 140 ℃, then the temperature is lowered to 40 ℃ through a two-stage reaction product cooler, the pressure is 0.8Mpa, and then the reaction product is added into a three-phase separation tank for oil phase, water phase and gas phase separation;
and absorbing the methanol in the oil phase through a water extraction tower to obtain a treated oil phase.
6. The process for the joint production of methyl mercaptan and methyl sulfide as claimed in claim 1, wherein step S104 specifically comprises:
firstly, rectifying and recovering methyl mercaptan by a methyl mercaptan rectifying tower to obtain a methyl mercaptan product, and then rectifying and recovering methyl sulfide by a methyl sulfide rectifying tower to obtain a methyl sulfide product.
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| JP2000219673A (en) * | 1999-01-29 | 2000-08-08 | Toray Fine Chemical Kk | Production of methyl mercaptan and/or dimethyl sulfide |
| US6198003B1 (en) * | 1999-04-20 | 2001-03-06 | Albemarle Corporation | Method for producing alkyl mercaptans and/or dialkyl monosulfides |
| CN1579617A (en) * | 2003-08-13 | 2005-02-16 | 中国科学院大连化学物理研究所 | Active alumina catalyst, and its preparation method and use |
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| CN104974066A (en) * | 2014-04-01 | 2015-10-14 | 中国石油化工股份有限公司 | Preparation method of dimethyl sulfide |
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| CN113316567A (en) * | 2019-01-18 | 2021-08-27 | 安迪苏法国联合股份有限公司 | Process for preparing compounds of formula RSH by hydrosulfurization |
| CN113149877A (en) * | 2021-04-26 | 2021-07-23 | 新疆兴发化工有限公司 | Production process of dimethyl sulfide |
| CN113578312A (en) * | 2021-06-30 | 2021-11-02 | 浙江大学 | Coordinated site catalyst, preparation method thereof and application thereof in preparation of mercaptan and thioether |
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