CN112979516A - Energy-saving methyl mercaptan synthesizing device - Google Patents

Energy-saving methyl mercaptan synthesizing device Download PDF

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Publication number
CN112979516A
CN112979516A CN202110427023.0A CN202110427023A CN112979516A CN 112979516 A CN112979516 A CN 112979516A CN 202110427023 A CN202110427023 A CN 202110427023A CN 112979516 A CN112979516 A CN 112979516A
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China
Prior art keywords
preheater
gas
reactor
refrigerator
methyl mercaptan
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CN202110427023.0A
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CN112979516B (en
Inventor
张一可
张强
郭锐
蒋松
范留伟
马海燕
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Chadu Hainan Technology Co ltd
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Chadu Hainan Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/02Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols
    • C07C319/08Preparation of thiols, sulfides, hydropolysulfides or polysulfides of thiols by replacement of hydroxy groups or etherified or esterified hydroxy groups
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/26Separation; Purification; Stabilisation; Use of additives
    • C07C319/28Separation; Purification
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25BREFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
    • F25B15/00Sorption machines, plants or systems, operating continuously, e.g. absorption type
    • F25B15/02Sorption machines, plants or systems, operating continuously, e.g. absorption type without inert gas
    • F25B15/06Sorption machines, plants or systems, operating continuously, e.g. absorption type without inert gas the refrigerant being water vapour evaporated from a salt solution, e.g. lithium bromide
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28DHEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D7/00Heat-exchange apparatus having stationary tubular conduit assemblies for both heat-exchange media, the media being in contact with different sides of a conduit wall
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency

Abstract

The invention discloses an energy-saving methyl mercaptan synthesis device which comprises a mixer, a first preheater, a second preheater, a third preheater, a reactor, a heat collector, a multistage condenser, a compressor, a tail gas washer, a methanol precooler, a refrigerator and a gas-liquid separator. Pre-cooling methanol, washing part of circulating gas, emptying non-condensable gas after gas-liquid separation, mixing absorption liquid with hydrogen sulfide, sequentially preheating by a first preheater, a second preheater and a third preheater, and then entering a reactor; the heat medium enters from the lower part of the reactor and is discharged after heat exchange of the first preheater; the synthesis gas produced by the reactor sequentially passes through a second preheater, a first preheater and a heat collector for heat exchange and then enters a multistage condenser for separating crude mercaptan, the uncondensed gas phase is pressurized by a compressor, then one part of the uncondensed gas phase enters a tail gas washing device, and the other part of the uncondensed gas phase and hydrogen sulfide enter a mixer together; the heat from the heat collector is made into chilled water by a refrigerator and then precooled into methanol. The device has the advantages of full heat utilization, reasonable inert gas and hydrogen sulfide separation process and obvious energy consumption reduction.

Description

Energy-saving methyl mercaptan synthesizing device
Technical Field
The invention belongs to the field of chemical production, and particularly relates to an energy-saving methyl mercaptan synthesis device.
Background
Methyl mercaptan belongs to a mercaptan organic substance which has the smallest relative molecular mass and is very active and is easy to react with other substances to form a sulfur-containing substance, so that the methyl mercaptan has wide application and is a main raw material for synthesizing pesticides, medicines, foods, synthetic materials and the like.
CN 1186067a discloses a process for the continuous production of methyl mercaptan by catalytic reaction of methanol and hydrogen sulfide, with significant improvements in the pretreatment of the feed gas mixture and the utilization of the heat of reaction and heat in the product gas mixture. The heat of the synthesis gas is only used for methanol evaporation and preheating, the temperature of the synthesis gas after methanol evaporation and preheating is still 100-150 ℃, the temperature is higher in actual production, the heat of the synthesis gas is taken away by cooling water of multi-stage condensation, and the heat and circulating water are wasted.
CN 202415415U discloses a device for preparing methyl mercaptan by adopting hydrogen sulfide-methanol catalytic reaction, wherein the heat of synthesis gas is only used for methanol evaporation and preheating, the preheating of raw materials to the reaction temperature in a catalyst bed layer is difficult to realize in the actual production, the heat of the synthesis gas is taken away by cooling water of multi-stage condensation, and the heat and circulating water are wasted.
CN 1189487A discloses a separation method of a product gas mixture for catalytic synthesis of methyl mercaptan, wherein a residual gas flow enters into secondary washing and distillation after product gas at 100-150 ℃ is subjected to secondary condensation. The waste heat of the synthesis gas is not fully utilized; the content of inert gas components in the mercaptan synthesis reaction is very low (less than 5%), and the total washing of the residual gas is uneconomical, since the reaction requires the amount of recycle gas to be adequate.
CN 111167267A discloses a recycle system of hydrogen sulfide in methyl mercaptan synthesis tail gas, uses methanol to absorb hydrogen sulfide in synthesis tail gas, and the residual gas is emptied after passing through a first cooler and a gas-liquid separation tank. Small liquid drops in the residual gas are removed in a condensation mode, so that the consumption of a cooling medium is increased, and the investment is increased.
Disclosure of Invention
In order to solve the problems, the invention aims to provide an energy-saving methyl mercaptan synthesis device, which has the advantages of full utilization of heat, reasonable inert gas removal process and obvious reduction of energy consumption.
The purpose of the invention is realized as follows:
an energy-saving methyl mercaptan synthesizing device is characterized in that: comprises a mixer 1, a first preheater 2, a second preheater 3, a third preheater 4, a reactor 5, a heat collector 6, a multi-stage condenser 7, a compressor 8, a tail gas scrubber 9, a methanol precooler 10, a refrigerator 11 and a gas-liquid separator 12; the inlet of the mixer 1 is respectively connected with the bottom of the tail gas scrubber 9 and the outlet of the compressor 8, and the outlet of the mixer is sequentially connected with the upper part of the reactor 5 through the tube passes of the first preheater 2, the second preheater 3 and the third preheater 4; the shell side of the preheater III 4 is connected with the upper part of the shell side of the reactor 5; the lower part of the reactor 5 sequentially passes through a second preheater 3 and a first preheater 2; the first preheater 2 is sequentially connected with a heat collector 6 and a multi-stage condenser 7; the multistage condenser 7 is respectively connected with a compressor 8 and a methyl mercaptan separation device 13; the outlet of the compressor 8 is connected with a tail gas scrubber 9; the other side of the heat collector 6 is connected with a refrigerator 11 and a methanol preheater 10 in sequence; the upper part of the tail gas scrubber 9 is connected with the shell pass of a methanol precooler 10, and the gas phase at the top part is sent to H after passing through a gas-liquid separator 122An S recovery unit or a tail gas incineration unit 14.
The further design is that: the reactor 5 is a tubular reactor.
The further design is that: the heat collector 6 is a shell-and-tube heat exchanger.
The further design is that: the refrigerator 11 may be a lithium bromide refrigerator, an organic refrigerator, or an ammonia refrigerator.
The further design is that: the tail gas scrubber 9 is provided with a self-circulation spraying pipeline, and the spraying position of the self-circulation spraying pipeline is arranged at the middle upper part.
The further design is that: the gas-liquid separator 12 is a double-baffle gas-liquid separator.
Compared with the prior art, the invention has the beneficial effects that:
the invention has reasonable process, reasonable inert gas and hydrogen sulfide separation flow, no redundant working procedures, full heat utilization and low cooling water consumption, and is suitable for newly-built devices and the reconstruction and upgrading of the existing devices.
Drawings
FIG. 1 is a schematic structural view of the present invention;
the system comprises a mixer 1, a mixer 2, a first preheater 3, a second preheater 4, a third preheater 5, a reactor 6, a heat collector 7, a multistage condenser 8, a compressor 9, a tail gas scrubber 10, a methanol precooler 11, a refrigerator 12, a gas-liquid separator 13, a methyl mercaptan separation device 14, and H2S recovery or tail gas incineration device, 15, methanol tank, 16, hydrogen sulfide compressor;
FIG. 2 is a schematic diagram of a tail gas scrubber.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
An energy-saving methyl mercaptan synthesis device comprises a mixer 1, a first preheater 2, a second preheater 3, a third preheater 4, a reactor 5, a heat remover 6, a multistage condenser 7, a compressor 8, a tail gas scrubber 9, a methanol precooler 10, a refrigerator 11 and a gas-liquid separator 12; the mixer 1The inlet is respectively connected with the bottom of the tail gas scrubber 9 and the outlet of the compressor 8, and the outlet is sequentially connected with the upper part of the reactor 5 through the tube passes of the first preheater 2, the second preheater 3 and the third preheater 4; the shell side of the preheater III 4 is connected with the upper part of the shell side of the reactor 5; the reactor 5 is a tubular reactor, and the lower part of the reactor passes through the shell pass of a second preheater 3 and a first preheater 2 in sequence; the first preheater 2 is sequentially connected with a heat collector 6 and a multi-stage condenser 7; the multistage condenser 7 is respectively connected with a compressor 8 and a methyl mercaptan separation device 13; the outlet of the compressor 8 is connected with a tail gas scrubber 9; the other side of the heat collector 6 is connected with a refrigerator 11 and a methanol preheater 10 in sequence; the upper part of the tail gas scrubber 9 is connected with the shell pass of a methanol precooler 10, and the gas phase at the top part is sent to H after passing through a gas-liquid separator 122S recovery or tail gas incineration unit 14.
The further design is that: the heat collector 6 is a heat exchanger commonly used in the chemical process.
The further design is that: the heat collector 6 is a shell-and-tube heat exchanger.
The further design is that: the refrigerator 11 may be a lithium bromide refrigerator, an organic refrigerator, or an ammonia refrigerator.
The further design is that: the tail gas scrubber 9 is provided with a self-circulation spraying pipeline, and the spraying position is at the middle upper part.
Further, the reactor is a tubular reactor;
the methanol in the methanol tank 15 is pre-cooled to-5 ℃ to 5 ℃ through a methanol pre-cooler 10, enters the upper part of a tail gas scrubber 9 and sprays and absorbs part of the recycle gas, the absorption liquid is sent to a mixer 1 to be mixed with the other recycle gas (containing hydrogen sulfide from a hydrogen sulfide compressor 16), then is subjected to heat exchange with the synthesis gas in a first preheater 2 to 70 ℃ to 90 ℃, is subjected to heat exchange with the synthesis gas in a second preheater 3 to 140 ℃ to 200 ℃, is subjected to heat exchange with a heating medium in a third preheater 4 to 250 ℃ to 300 ℃ and then enters a reactor 5, and the components of the synthesis gas produced by the reactor 5 are about 88% of methyl mercaptan, 9% of methyl sulfide and 3% of inert components. The temperature of the synthesis gas is about 150 ℃ after heat exchange through the first preheater 2, the second preheater 3 and the third preheater 4.
The synthesis gas with the temperature of 120 ℃ and 150 ℃ exchanges heat with hot water in a heat remover 6 to obtain the temperature of about 100 DEG CThe hot water enters the refrigerator 11, the chilled water produced in the refrigerator 11 supplies cold for the methanol preheater 10, and the insufficient part can be supplied by the chilled water in the battery limits. The synthesis gas after heat exchange enters a multistage condenser 7 for separating a gas phase and a liquid phase, the liquid phase is sent to a separation device for purifying methyl mercaptan, the gas phase is pressurized by a compressor, then a part of the gas phase is sent to a tail gas scrubber 9 for absorption, the absorbed inert gas is sent to a gas-liquid separator 12 for recycling the liquid phase and then sent to a H2S recovery unit or tail gas burning unit; the other part of the circulating gas and the supplemented hydrogen sulfide and the absorption liquid enter a mixer together to form a closed loop.
The gas-liquid separator 12 is a multi-gear gas-liquid separator, and has no public engineering consumption.
The gas flow ratio from the compressor 8 to the mixer 1 and the tail gas scrubber 9 is 1-10, usually 4.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.

Claims (6)

1. An energy-saving methyl mercaptan synthesizing device is characterized in that: comprises a mixer (1), a first preheater (2), a second preheater (3), a third preheater (4), a reactor (5), a heat collector (6), a multi-stage condenser (7), a compressor (8), a tail gas scrubber (9), a methanol precooler (10), a refrigerator (11) and a gas-liquid separator (12); the inlet of the mixer (1) is respectively connected with the bottom of the tail gas scrubber (9) and the outlet of the compressor (8), and the outlet of the mixer is connected with the upper part of the reactor (5) through the tube passes of the first preheater (2), the second preheater (3) and the third preheater (4) in sequence; the shell side of the preheater III (4) is connected with the upper part of the shell side of the reactor (5); the lower part of the reactor (5) sequentially passes through the shell pass of a second preheater (3) and a first preheater (2); the first preheater (2) is sequentially connected with the heat collector (6) and the multistage condenser (7); the multistage condenser (7) is respectively provided with a compressor (8) and a crude mercaptan separation device(13) Connecting; the outlet of the compressor (8) is connected with a tail gas scrubber (9); the other side of the heat collector (6) is connected with a refrigerator (11) and a methanol preheater (10) in sequence; the upper part of the tail gas scrubber (9) is connected with the shell side of the methanol precooler (10), and the top gas phase is sent to H after passing through a gas-liquid separator (12)2S recovery or tail gas incineration device (14).
2. An energy-saving methyl mercaptan synthesis plant according to claim 1, wherein: the reactor (5) is a tubular reactor.
3. An energy-saving methyl mercaptan synthesis plant according to claim 1, wherein: the heat collector (6) is a shell-and-tube heat exchanger.
4. An energy-saving methyl mercaptan synthesis plant according to claim 1, wherein: the refrigerator (11) can be a lithium bromide refrigerator, an organic refrigerator or an ammonia refrigerator.
5. An energy-saving methyl mercaptan synthesis plant according to claim 1, wherein: the tail gas scrubber (9) is provided with a self-circulation spraying pipeline, and the spraying position of the self-circulation spraying pipeline is arranged at the middle upper part.
6. An energy-saving methyl mercaptan synthesis plant according to claim 1, wherein: the gas-liquid separator (12) is a double-baffle gas-liquid separator.
CN202110427023.0A 2021-04-20 2021-04-20 Energy-saving methyl mercaptan synthesis device Active CN112979516B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113623895A (en) * 2021-07-01 2021-11-09 华电电力科学研究院有限公司 Combined cooling heating and power system for cooling data center and control method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1186067A (en) * 1996-12-27 1998-07-01 底古萨股份公司 Process for continuous production of methyl mercaptan
CN1189487A (en) * 1996-12-27 1998-08-05 底古萨股份公司 Process for separating product gas mixture from catalytic synthesis of methyl mercaptan
US5847223A (en) * 1995-06-23 1998-12-08 Rhone-Poulenc Nutrition Animale Process for the preparation of methyl mercaptan
CN202415415U (en) * 2011-12-21 2012-09-05 天津市泰旭物流有限公司 Device for preparing methanethiol by use of hydrogen sulfide-methanol gas-phase catalytic reaction method
CN107501049A (en) * 2017-09-19 2017-12-22 天津大学 A kind of extracting rectifying removing low-temp methanol washes the device and method of sulfide in recycle methanol
CN215162271U (en) * 2021-04-20 2021-12-14 查都(海南)科技有限公司 Energy-saving methyl mercaptan synthesizing device

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5847223A (en) * 1995-06-23 1998-12-08 Rhone-Poulenc Nutrition Animale Process for the preparation of methyl mercaptan
CN1186067A (en) * 1996-12-27 1998-07-01 底古萨股份公司 Process for continuous production of methyl mercaptan
CN1189487A (en) * 1996-12-27 1998-08-05 底古萨股份公司 Process for separating product gas mixture from catalytic synthesis of methyl mercaptan
CN202415415U (en) * 2011-12-21 2012-09-05 天津市泰旭物流有限公司 Device for preparing methanethiol by use of hydrogen sulfide-methanol gas-phase catalytic reaction method
CN107501049A (en) * 2017-09-19 2017-12-22 天津大学 A kind of extracting rectifying removing low-temp methanol washes the device and method of sulfide in recycle methanol
CN215162271U (en) * 2021-04-20 2021-12-14 查都(海南)科技有限公司 Energy-saving methyl mercaptan synthesizing device

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113623895A (en) * 2021-07-01 2021-11-09 华电电力科学研究院有限公司 Combined cooling heating and power system for cooling data center and control method thereof
CN113623895B (en) * 2021-07-01 2022-11-01 华电电力科学研究院有限公司 Combined cooling heating and power system for cooling data center and control method thereof

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