CN107759501A - A kind of device for producing DMDS coproduction dimethyltrisulfide - Google Patents

A kind of device for producing DMDS coproduction dimethyltrisulfide Download PDF

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Publication number
CN107759501A
CN107759501A CN201711283696.3A CN201711283696A CN107759501A CN 107759501 A CN107759501 A CN 107759501A CN 201711283696 A CN201711283696 A CN 201711283696A CN 107759501 A CN107759501 A CN 107759501A
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CN
China
Prior art keywords
delivery pump
connection
dmds
dimethyltrisulfide
reactor
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CN201711283696.3A
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Inventor
李广敏
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Inquiry (shanghai) Technology Co Ltd
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Inquiry (shanghai) Technology Co Ltd
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Priority to CN201711283696.3A priority Critical patent/CN107759501A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C319/00Preparation of thiols, sulfides, hydropolysulfides or polysulfides
    • C07C319/22Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides
    • C07C319/24Preparation of thiols, sulfides, hydropolysulfides or polysulfides of hydropolysulfides or polysulfides by reactions involving the formation of sulfur-to-sulfur bonds
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of method for producing DMDS coproduction dimethyltrisulfide, sulphur is mainly dissolved in DMDS solution by this method enters first reactor, sulphur and DMDS generate dimethyltrisulfide in reactor, dimethyltrisulfide and unreacted DMDS are introduced into first rectifying column and separated, tower top obtains DMDS product, the dimethyltrisulfide of bottom of towe can be used as production marketing, second reactor reaction generation DMDS can also be entered with methyl mercaptan, reaction solution enters the first flash tank removing hydrogen sulfide, liquid phase separates hydrogen sulfide and methyl mercaptan into Second distillation column tower top, materials at bottom of tower enters third distillation column, DMDS product is produced in rectifying column tower top, bottom of towe solution is recycled into first rectifying column isolated DMDS product again.The method that the present invention distinguishes refining spearation using reaction mass twice, two kinds of products of DMDS and dimethyltrisulfide can be obtained, it is reasonable with technological process configuration, equipment investment is small, good reaction selectivity, impurity content is low in reaction product, and refining spearation technique is simple, and product purity is high and easily controllable.

Description

A kind of device for producing DMDS coproduction dimethyltrisulfide
Technical field
The present invention relates to production DMDS coproduction dimethyltrisulfide technical field, more particularly to a kind of production dimethyl The device of two sulphur coproduction dimethyltrisulfides.
Background technology
DMDS DMDS is agricultural chemicals and dyestuff intermediate, is Entex, methiocarb mercaptodimethur, fensulfothion, methyl sulphur Acid, the raw material of methylsufonyl chloride, in the oil industry as catalyst passivator, as ethene splits Jie's furnace coking inhibitor, hydrogenation takes off Sulphur and the activator for giving sulfidation;Rubber liquid vulcanizing agent, curing agent DADMT raw materials and organic solvent.Dimethyltrisulfide master It is used for medicine intermediate, is used on a small quantity as food additives in the food flavors such as gravy, soup class.DMDS and diformazan Base trithio is all that market is well sold and in short supply, the long-term fine chemical product that supply falls short of demand.
In the relevant report and patent of methyl mercaptan vulcanization method production DMDS, mainly there are two kinds of production methods:One Kind reacts generation DMDS for raw material sulphur and methyl mercaptan in vulcanization reaction device, and the material of reaction enters rectifying column Refining spearation, this method methyl mercaptan and DMDS are lost in seriously, and refining spearation system process is complicated, and product yield is low, production Product purity is not high.
One kind is two step vulcanization reactions, i.e. CN103864650A discloses a kind of method of continuous production DMDS, Dimethyltrisulfide reactor is pumped into through charging after the thawing of raw material sulphur, the DMDS reaction generation dimethyl three with circulation Sulphur, dimethyltrisulfide enter DMDS reactor, reaction generation DMDS, DMDS crude product with methyl mercaptan Into knockout drum, most hydrogen sulfide is separated, liquid product enters rectifying column, overhead condensation recovery DMDS production Product, hydrogen sulfide are discharged as fixed gas, and the DMDS and dimethyltrisulfide of tower reactor, which return, to be recycled, this method exist with Lower deficiency:
1st, the material of end reaction enters separate unit rectifying column refining spearation, contains in the DMDS solution of such tower reactor circulation Dimethyltrisulfide concentration it is higher, generate the sulphur of dimethyl four or more sulphur into dimethyltrisulfide reactor solution, cause mesh It is low to mark product yield, refining spearation complex process.
2nd, the product to be reacted in dimethyltrisulfide reactor is the mixture of dimethyltrisulfide and DMDS, Not sulfide hydrogen and methyl mercaptan, not by after mixture elder generation refining spearation, DMDS reactor is entered back into, causes dimethyl Two reaction of Salmon-Saxl devices and refining separation device equipment investment are big, and the catalyst consumption amount of reaction also increases.
3rd, during rectifying tower reactor material Returning reactor, the heavy constituent accumulated in system, metal ion, salt etc. It can not in time exclude, influence the purity and yield of DMDS product.
In presently disclosed patent of invention, not producing DMDS can be reported with the correlation of coproduction dimethyltrisulfide technology Road.
The content of the invention
Present invention seek to address that the problem of above-mentioned technology is present, there is provided one kind production DMDS coproduction dimethyl three The method of sulphur, there is technological process configuration rationally, equipment investment is small, good reaction selectivity, and reaction product impurity content is low, refines The features such as separating technology is simple, and product purity is high and easily controllable.
A kind of device for producing DMDS coproduction dimethyltrisulfide, it is characterised in that including the first reaction mechanism, Two reaction mechanisms and finished product collecting mechanism, in addition to vacuum mechanism, waste gas treatment mechanism, compression mechanism, methyl mercaptan addition mechanism, Methyl mercaptan vulcanization mechanism, burn mechanism and methyl mercaptan combination mechanism, first reaction mechanism have four output ends respectively with institute Stating finished product collecting mechanism, restructuring mechanism, vacuum mechanism and the connection of the second reaction mechanism, second reaction mechanism has four outputs End is connected with the finished product collecting mechanism, burning mechanism, methyl mercaptan vulcanization mechanism and the first reaction mechanism respectively;
Further, first reaction mechanism include first reactor, first rectifying column, the first condenser, the first backflash, First delivery pump, the second delivery pump and the 3rd delivery pump, the first reactor are provided with feed end, and material solution passes through charging End enters in the first reactor, and the first reactor is connected with the first rectifying column, and the first rectifying column has three Individual output end is connected with first condenser, second delivery pump and the 3rd delivery pump respectively, and first condenser has Two output ends are connected with the vacuum mechanism and first backflash respectively, the vacuum mechanism and the exhaust gas processor Structure is connected, and first backflash is connected with first delivery pump, and first delivery pump connects with the finished product collecting mechanism Connect, the 3rd delivery pump is connected with the finished product collecting mechanism;
Further, second reaction mechanism include second reactor, the first flash tank, the 4th delivery pump, Second distillation column, Second condenser, the second backflash, the 5th delivery pump, the second delivery pump, third distillation column, the 3rd backflash, the 3rd condenser, 7th delivery pump and the 8th delivery pump, the feed end of the second reactor are connected with the 3rd delivery pump, and described second is anti- Two delivery ends of device are answered to be connected respectively with the compression mechanism and first flash tank, first flash tank there are two outputs End is connected with the 4th delivery pump and the compression mechanism respectively, and the 4th delivery pump is connected with the Second distillation column, The Second distillation column has two output ends to be connected respectively with second condenser and the 6th delivery pump, and described second is cold Condenser has two output ends to be connected respectively with second backflash and the compression mechanism, second backflash and described the Five delivery pumps are connected, and the 5th delivery pump is connected with the finished product collecting mechanism, the 6th delivery pump and the described 3rd essence Tower connection is evaporated, the third distillation column has two output ends to be connected respectively with the 3rd backflash and the 8th delivery pump, 3rd backflash has two output ends to be connected respectively with the 3rd condenser and the burning mechanism, the 3rd condensation Device is connected with the 7th delivery pump, and the 7th delivery pump is connected with the finished product collecting mechanism, the 8th delivery pump with The first reactor connection;
Further, the methyl mercaptan combination mechanism and the methyl mercaptan addition mechanism be connecteds, the methyl mercaptan addition mechanism and The feed end connection of the second reactor;
Further, second delivery pump is arranged on the first rectifying column bottom connection;
Further, choke valve is provided with the 3rd delivery pump, the 3rd conveying pump duty can be adjusted;
Further, the 8th rear pump is connected with the third distillation column bottom.
Have the advantage that:
The present invention can obtain DMDS and dimethyltrisulfide two using the method for the difference refining spearation of reaction mass twice Kind product, technological process configuration is more reasonable, can be needed enter second reactor by adjusting dimethyltrisulfide according to production Amount, any control obtains the yield of DMDS and dimethyltrisulfide product.It is small with equipment investment, reaction selectivity Well, the features such as impurity content is low in reaction product, and refining spearation technique is simple, and product purity is high and easily controllable.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention.
Wherein, 1 is the first reaction mechanism, and 2 be the second reaction mechanism, and 3 be finished product collecting mechanism, and 4 be vacuum mechanism, and 5 are Waste gas treatment mechanism, 6 be compression mechanism, and 7 be that methyl mercaptan adds mechanism, and 8 be that methyl mercaptan vulcanizes mechanism, and 9 is burn mechanism, and 11 are First reactor, 12 be first rectifying column, and 13 be the first condenser, and 14 be the first backflash, and 15 be the first delivery pump, and 16 be Two delivery pumps, 17 be the 3rd delivery pump, and 21 be second reactor, and 22 be the first flash tank, and 23 be the 4th delivery pump, and 24 be second Rectifying column, 25 be the second condenser, and 26 be the second backflash, and 27 be the 5th delivery pump, and 28 be the 6th delivery pump, and 29 be the 3rd essence Tower is evaporated, 30 be the 3rd backflash, and 31 be the 3rd condenser, and 32 be the 7th delivery pump, and 33 be the 8th delivery pump.
Embodiment
A kind of device for producing DMDS coproduction dimethyltrisulfide, it is characterised in that including the first reaction mechanism 1, Second reaction mechanism 2 and finished product collecting mechanism 3, in addition to vacuum mechanism 4, waste gas treatment mechanism 5, compression mechanism 6, methyl mercaptan add Add mechanism 7, methyl mercaptan vulcanization mechanism 8, burn mechanism 9 and methyl mercaptan combination mechanism 10, first reaction mechanism 1 have four it is defeated Go out end to be connected with the finished product collecting mechanism 3, restructuring mechanism, the reaction mechanism 2 of vacuum mechanism 4 and second respectively, described second is anti- Mechanism 2 is answered there are four output ends anti-with the finished product collecting mechanism 3, burning mechanism 9, methyl mercaptan vulcanization mechanism 8 and first respectively Mechanism 1 is answered to connect.
2nd, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 1, its feature exist In:First reaction mechanism 1 include first reactor 11, first rectifying column 12, the first condenser 13, the first backflash 14, First delivery pump 15, the second delivery pump 16 and the 3rd delivery pump 17, the first reactor 11 are provided with feed end, material solution Entered by feed end in the first reactor 11, the first reactor 11 is connected with the first rectifying column 12, described First rectifying column 12 have three output ends respectively with first condenser 13, the delivery pump 17 of second delivery pump 16 and the 3rd Connection, first condenser 13 have two output ends to be connected respectively with the vacuum mechanism 4 and first backflash 14, institute State vacuum mechanism 4 to be connected with the waste gas treatment mechanism 5, first backflash 14 is connected with first delivery pump 15, institute State the first delivery pump 15 to be connected with the finished product collecting mechanism 3, the 3rd delivery pump 17 connects with the finished product collecting mechanism 3 Connect.
3rd, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 1, its feature exist In:Second reaction mechanism 2 include second reactor 21, the first flash tank 22, the 4th delivery pump 23, Second distillation column 24, Second condenser 25, the second backflash 26, the 5th delivery pump 27, the 6th delivery pump 28, third distillation column 29, the 3rd backflash 30th, the 3rd condenser 31, the 7th delivery pump 32 and the 8th delivery pump 33, the feed end of the second reactor 21 and the described 3rd Delivery pump 17 connects, described 21 two delivery ends of second reactor respectively with the compression mechanism 6 and first flash tank 22 Connection, first flash tank 22 have two output ends to be connected respectively with the 4th delivery pump 23 and the compression mechanism 6, institute State the 4th delivery pump 23 to be connected with the Second distillation column 24, the Second distillation column 24 there are two output ends respectively with described Two condensers 25 and the 6th delivery pump 28 connect, second condenser 25 have two output ends respectively with described second time Chute 26 and the compression mechanism 6 are connected, and second backflash 26 is connected with the 5th delivery pump 27, the 5th conveying Pump 27 is connected with the finished product collecting mechanism 3, and the 6th delivery pump 28 is connected with the third distillation column 29, the 3rd essence Evaporating tower 29 has two output ends to be connected respectively with the 3rd backflash 30 and the 8th delivery pump 33, the 3rd backflash 30 have two output ends to be connected respectively with the 3rd condenser 31 and the burning mechanism 9, the 3rd condenser 31 and institute The 7th delivery pump 32 is stated to connect, the 7th delivery pump 32 is connected with the finished product collecting mechanism 3, the 8th delivery pump 33 with The first reactor 11 connects.
4th, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 1, its feature exist In:The methyl mercaptan combination mechanism 10 and the methyl mercaptan addition mechanism 7 are connected, the methyl mercaptan addition mechanism 7 and described the The feed end connection of two reactors 21.
5th, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 2, its feature exist In:Second delivery pump 16 is arranged on the bottom of first rectifying column 12 connection.
6th, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 2, its feature exist In:Choke valve is provided with 3rd delivery pump 17, the conveying capacity of the 3rd delivery pump 17 can be adjusted.
7th, a kind of device for producing DMDS coproduction dimethyltrisulfide according to claim 3, its feature exist In:8th rear pump is connected with the bottom of third distillation column 29.
By the sulphur that quality is 600Kg, it is in 3525Kg DMDS solution, into first reactor to be dissolved in quality 11 excessive DMDSs and sulfur reaction, reaction generation dimethyltrisulfide quality:2362.5Kg and DMDS matter Amount:1762.5Kg solution enters first rectifying column 12, is separated by the way of rectification under vacuum, top gaseous phase is cold through first The condensation of condenser 13 enters the first backflash 14, and it is 1500Kg to obtain quality, and the DMDS product that purity is more than 99.5% passes through First delivery pump 15 is sent into finished product stowage mechanism, and bottom of towe is by the restructuring lease making second containing metal ion, salt and other impurities Delivery pump 16 is excluded in time, and the dimethyltrisulfide product that purity is 98% is obtained in the middle and lower part of first rectifying column 12, and quality is 2362.5Kg is sent into finished product collecting mechanism 3 or second reactor 21 through the pressure-raising of the 3rd delivery pump 17, is passed through according to production needs The amount that dimethyltrisulfide enters second reactor 21 is adjusted, controls the production ratio of DMDS and dimethyltrisulfide product. It is molten with the methyl mercaptan total overall reaction that quality is 1800Kg, reaction if DMDS product is fully entered in second reactor 21 Liquid enters the hydrogen sulfide 580Kg of the first flash tank 22 removing dissolving, and the solution after flash distillation enters the second essence through the 4th delivery pump 23 The top of tower 24, removed overhead hydrogen sulfide and micro methyl mercaptan are evaporated, bottom of towe solution enters third distillation column 29 through the 6th delivery pump 28 Middle part, top gaseous phase condense into the 3rd condenser 31, and fixed gas enters burning mechanism 9 and burned, and condensate liquid enters the 3rd backflow Groove 30, the DMDS product purity that the 3rd backflash 30 comes out are sent into finished product through the 7th delivery pump 32 more than 99.5% and received Collecting mechanism 3, bottom of towe solution are recycled into first rectifying column 12 through the 8th delivery pump 33 and separated again.
The invention is not limited in above-described embodiment, on the basis of technical scheme disclosed by the invention, the skill of this area Art personnel are according to disclosed technology contents, it is not necessary to which performing creative labour can makes one to some of which technical characteristic A little to replace and deform, these are replaced and deformation is within the scope of the present invention.

Claims (7)

1. a kind of device for producing DMDS coproduction dimethyltrisulfide, it is characterised in that including the first reaction mechanism(1)、 Second reaction mechanism(2)With finished product collecting mechanism(3), in addition to vacuum mechanism(4), waste gas treatment mechanism(5), compression mechanism (6), methyl mercaptan addition mechanism(7), methyl mercaptan vulcanization mechanism(8), burn mechanism(9)With methyl mercaptan combination mechanism(10), it is described First reaction mechanism(1)Have four output ends respectively with the finished product collecting mechanism(3), restructuring mechanism, vacuum mechanism(4)With Two reaction mechanisms(2)Connection, second reaction mechanism(2)Have four output ends respectively with the finished product collecting mechanism(3), burn Burn mechanism(9), methyl mercaptan vulcanization mechanism(8)With the first reaction mechanism(1)Connection.
A kind of 2. device for producing DMDS coproduction dimethyltrisulfide according to claim 1, it is characterised in that:Institute State the first reaction mechanism(1)Including first reactor(11), first rectifying column(12), the first condenser(13), the first backflash (14), the first delivery pump(15), the second delivery pump(16)With the 3rd delivery pump(17), the first reactor(11)Be provided with into Expect end, material solution enters the first reactor by feed end(11)It is interior, the first reactor(11)With described first Rectifying column(12)Connection, the first rectifying column(12)Have three output ends respectively with first condenser(13), described Two delivery pumps(16)With the 3rd delivery pump(17)Connection, first condenser(13)Have two output ends respectively with the vacuum Mechanism(4)With first backflash(14)Connection, the vacuum mechanism(4)With the waste gas treatment mechanism(5)Connection, it is described First backflash(14)With first delivery pump(15)Connection, first delivery pump(15)With the finished product collecting mechanism (3)Connection, the 3rd delivery pump(17)With the finished product collecting mechanism(3)Connection.
A kind of 3. device for producing DMDS coproduction dimethyltrisulfide according to claim 1, it is characterised in that:Institute State the second reaction mechanism(2)Including second reactor(21), the first flash tank(22), the 4th delivery pump(23), Second distillation column (24), the second condenser(25), the second backflash(26), the 5th delivery pump(27), the 6th delivery pump(28), third distillation column (29), the 3rd backflash(30), the 3rd condenser(31), the 7th delivery pump(32)With the 8th delivery pump(33), described second is anti- Answer device(21)Feed end and the 3rd delivery pump(17)Connection, the second reactor(21)Two delivery ends respectively with institute State compression mechanism(6)With first flash tank(22)Connection, first flash tank(22)Have two output ends respectively with institute State the 4th delivery pump(23)With the compression mechanism(6)Connection, the 4th delivery pump(23)With the Second distillation column(24) Connection, the Second distillation column(24)Have two output ends respectively with second condenser(25)With the 6th delivery pump (28)Connection, second condenser(25)Have two output ends respectively with second backflash(26)With the compression mechanism (6)Connection, second backflash(26)With the 5th delivery pump(27)Connection, the 5th delivery pump(27)With it is described into Product collecting mechanism(3)Connection, the 6th delivery pump(28)With the third distillation column(29)Connection, the third distillation column (29)Have two output ends respectively with the 3rd backflash(30)With the 8th delivery pump(33)Connection, the 3rd backflow Groove(30)Have two output ends respectively with the 3rd condenser(31)With the burning mechanism(9)Connection, the 3rd condensation Device(31)With the 7th delivery pump(32)Connection, the 7th delivery pump(32)With the finished product collecting mechanism(3)Connection, institute State the 8th delivery pump(33)With the first reactor(11)Connection.
A kind of 4. device for producing DMDS coproduction dimethyltrisulfide according to claim 1, it is characterised in that:Institute State methyl mercaptan combination mechanism(10)Mechanism is added with the methyl mercaptan(7)Connection, the methyl mercaptan add mechanism(7)With described Two reactors(21)Feed end connection.
A kind of 5. device for producing DMDS coproduction dimethyltrisulfide according to claim 2, it is characterised in that:Institute State the second delivery pump(16)It is arranged on the first rectifying column(12)Bottom connects.
A kind of 6. device for producing DMDS coproduction dimethyltrisulfide according to claim 2, it is characterised in that:Institute State the 3rd delivery pump(17)It is interior to be provided with choke valve, the 3rd delivery pump can be adjusted(17)Conveying capacity.
A kind of 7. device for producing DMDS coproduction dimethyltrisulfide according to claim 3, it is characterised in that:Institute State the 8th rear pump and the third distillation column(29)Bottom connects.
CN201711283696.3A 2017-12-07 2017-12-07 A kind of device for producing DMDS coproduction dimethyltrisulfide Pending CN107759501A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116651020A (en) * 2023-07-31 2023-08-29 民勤县鑫达化工有限公司 Separation device for dimethyl disulfide production and manufacturing and application method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1153160A (en) * 1995-12-27 1997-07-02 西安近代化学研究所 Production process of 1, 1, 1, 2-tetrafluoroethane
CN103864650A (en) * 2014-03-20 2014-06-18 中国海洋石油总公司 Method for continuously producing dimethyl disulfide
CN104592070A (en) * 2015-01-13 2015-05-06 湖北兴发化工集团股份有限公司 Preparation method of dimethyl disulfide
CN104610106A (en) * 2015-01-13 2015-05-13 湖北兴发化工集团股份有限公司 Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method
CN107652159A (en) * 2017-10-18 2018-02-02 山东华安新材料有限公司 A kind of device and method for preparing 2,3,3,3 tetrafluoropropenes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1153160A (en) * 1995-12-27 1997-07-02 西安近代化学研究所 Production process of 1, 1, 1, 2-tetrafluoroethane
CN103864650A (en) * 2014-03-20 2014-06-18 中国海洋石油总公司 Method for continuously producing dimethyl disulfide
CN104592070A (en) * 2015-01-13 2015-05-06 湖北兴发化工集团股份有限公司 Preparation method of dimethyl disulfide
CN104610106A (en) * 2015-01-13 2015-05-13 湖北兴发化工集团股份有限公司 Method for producing dimethyl disulfide by using methyl mercaptan and sulfur vaporization method
CN107652159A (en) * 2017-10-18 2018-02-02 山东华安新材料有限公司 A kind of device and method for preparing 2,3,3,3 tetrafluoropropenes

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116651020A (en) * 2023-07-31 2023-08-29 民勤县鑫达化工有限公司 Separation device for dimethyl disulfide production and manufacturing and application method thereof
CN116651020B (en) * 2023-07-31 2023-09-19 民勤县鑫达化工有限公司 Separation device for dimethyl disulfide production and manufacturing and application method thereof

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Application publication date: 20180306