CN105693573B - A kind of method and device of by-product production sodium methyl mercaptide using dimethyl sulphide synthesis - Google Patents
A kind of method and device of by-product production sodium methyl mercaptide using dimethyl sulphide synthesis Download PDFInfo
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- CN105693573B CN105693573B CN201610137509.XA CN201610137509A CN105693573B CN 105693573 B CN105693573 B CN 105693573B CN 201610137509 A CN201610137509 A CN 201610137509A CN 105693573 B CN105693573 B CN 105693573B
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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
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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 discloses a kind of method of the by-product production sodium methyl mercaptide using dimethyl sulphide synthesis, specifically using using the accessory substance in dimethyl sulphide building-up process as raw material, unstripped gas is pumped into water extraction tower, soft water is sent into water extraction tower from water extraction tower top, and the methanol in unstripped gas is extracted with soft water；By separating methanol rectifying, the thioether of abjection returns to dimethyl sulfide workshop and used；Thick methyl mercaptan after desulfurization ether is sent into stripper, stripping removes most of hydrogen sulfide in raw material；Micro hydrogen sulfide is removed using ferric oxide desulfurizer, obtains refined methyl mercaptan gas；Refined methyl mercaptan gas is sent into absorption tower, with absorbing by liquid caustic soda, obtains sodium methyl mercaptide solution.The present invention also provides a kind of equipment corresponding with this method, and this method can be effectively using the methyl mercaptan production sodium methyl mercaptide product of dimethyl sulfide synthesis by-product, and realizing turns waste into wealth, and has higher economical and environmentally friendly value.
Description
Technical field
The invention belongs to field of chemical technology, and in particular to one kind uses methyl mercaptan, especially dimethyl sulphide to synthesize
Method of the methyl mercaptan of byproduct in process as raw material production sodium methyl mercaptide solution.
Background technology
Sodium methyl mercaptide is a kind of strong alkaline liquid of water white transparency, there is off-odor, available in agricultural chemicals, medicine, pigment
The raw material of mesosome, such as agricultural chemicals symetryne, Methomyl and organic intermediate raw material；Food additives methionine, vitamin, rubber
The raw material of glue vulcanizing agent；The antidote of hydrogen sulfide poisoning；The odor additive etc. of coal gas, natural gas.
Currently, domestic sodium methyl mercaptide product mostly uses NaHS as raw material, anti-with dimethyl suflfate or chloromethanes
Methyl mercaptan should be generated, then sodium methyl mercaptide product is obtained with absorbing by liquid caustic soda.Wherein, dimethyl suflfate is hypertoxic raw material, use, accumulating
Process has larger potential safety hazard.The yield of dimethyl suflfate-final sodium methyl mercaptide of NaHS technique is only 75%~80%
Left and right, and the largely waste water containing organic matter is produced in production process, have greater environmental impacts.Chloromethanes-NaHS technique pair
Produce thioether and a large amount of sodium chloride-containings, the waste water of organic matter, subsequent treatment are more difficult.
The content of the invention
The invention provides it is a kind of using dimethyl sulphide synthesize by-product methyl mercaptan produce sodium methyl mercaptide solution method and
Device, its raw material used can be achieved to turn waste into wealth, and effectively prevent using sulfuric acid two for the accessory substance of thioether synthetic workshop
Methyl esters-NaHS or environmental problem and safety problem that chloromethanes-NaHS is raw band.
The technical solution adopted in the present invention is：By being used after the dimethyl sulfide material-heat-exchanging containing methyl mercaptan, water extraction is de-
The processing steps such as methanol, rectifying desulfurization ether, pressurization Stripping Desulfuration hydrogen, fixed bed fine de-sulfur, remove methanol, the sulphur in raw material
The impurity such as ether, hydrogen sulfide；Methyl mercaptan after being cleaned with certain density absorbing by liquid caustic soda, obtains sodium methyl mercaptide product.It is specifically walked
Suddenly include：
(1) using the accessory substance in dimethyl sulphide building-up process as raw material, unstripped gas is condensed to after 15~30 DEG C and extracted from water
Bottom of towe is taken to be pumped into water extraction tower, soft water is sent into water extraction tower from water extraction tower top, is extracted with soft water in unstripped gas
Methanol；
(2) material of separating methanol is sent into rectifying column, the rectifying at 0.5~0.9MPa, 55~85 DEG C, the big portion in raw material
Thioether is divided to be removed, the thioether of abjection returns to dimethyl sulfide workshop and used；
(3) the thick methyl mercaptan after desulfurization ether is sent into stripper, at 0.5~1.0MPa, 20~60 DEG C, stripping removing is former
Most of hydrogen sulfide in material, obtains the organic materials using methyl mercaptan as key component；
(4) organic materials of thick depriving hydrogen sulphide is sent into fine de-sulfur reactor, removed using ferric oxide desulfurizer micro
Hydrogen sulfide, until hydrogen sulfide content remains at less than 0.01%, obtain refined methyl mercaptan gas；
(5) refined methyl mercaptan gas is sent into absorption tower, at 40~60 DEG C, pressure is under 0.07~0.25MPa, uses liquid
Alkali absorption, obtain sodium methyl mercaptide solution.
In step (1), the side components in dimethyl sulphide building-up process include 35wt%-45wt% dimethyl sulfides,
50wt%-60wt% methyl mercaptans, 1.2wt%-2.5wt% methanol, 1.8wt%-2.5wt% water, 0.05wt%-0.2wt% sulphur
Change hydrogen.In step (1), the accessory substance in dimethyl sulphide building-up process is with 500-800m3/ h flow is pumped into water extraction tower, soft water
With 200-400m3/ h flow is sent into water extraction tower.
In step (1), after water extracts, with 50~100m3/ h flow extraction partial extraction water, while with identical stream
Amount supplements fresh soft water to keep system balancing.
In step (3), return flow is 1400m in stripper3/ h~1700m3/h。
In step (5), by the liquid caustic soda of concentration 13%~15% with 100~200m3/ h flow is continuously pumped into absorption tower
Top, inversely contacted with methyl mercaptan, methyl mercaptan generates sodium methyl mercaptide by absorbing by liquid caustic soda, from absorb the bottom of the tower with 100~200m3/h
Flow produce to obtain finished product sodium methyl mercaptide solution.
It is a kind of using dimethyl sulphide synthesis by-product production sodium methyl mercaptide device, raw material storage tank be connected with pump after through defeated
Expects pipe is connected with water extraction tower bottom, with being connected at the top of preheater at the top of water extraction tower, in preheater bottom and thioether rectifying column
Portion connects, and is connected at the top of thioether rectifying column with rectifying column condenser, and rectifying column condenser bottom is through conveying pipeline and surge tank top
Connection, buffering pot bottom are connected through conveying pipeline with stripper top, and stripper bottom is connected through conveying pipeline with vaporizer bottom, vapour
Change and be connected at the top of device through conveying pipeline with fine de-sulfur reactor bottom, fine de-sulfur reactor head is through under conveying pipeline and product absorption tower
Portion connects, through conveying pipeline with dividing alkali tank to be connected at the top of product absorption tower.
Water extraction tower bottom is connected through conveying pipeline with water extraction tower top, forms circulation loop；Thioether rectifier bottoms pass through
Conveying pipeline is connected with thioether rectifying column bottom again after being connected with rectifying column reboiler, forms circulation loop；Rectifying column condenser is extremely
It is additionally provided with the conveying pipeline of surge tank to the conveying pipeline of thioether rectifying column；Stripper top is through conveying pipeline and stripper condenser
After connection, then it is connected with stripper top, forms circulation loop；Stripper bottom be connected with stripper reboiler after again with stripping
Tower bottom connects to form circulation loop；It is additionally provided with the top of vaporizer through conveying pipeline to the conveying pipeline on product absorption tower.
Under process conditions of the present invention, the accessory substance methyl mercaptan of thioether synthesis is converted into the conversion ratio of sodium methyl mercaptide
More than 95%, sodium sulfide content is low in its product, and product quality gets a promotion.
Method provided by the present invention, raw material and pilot process utilization of materials are high, and other dirts are not produced in production process
Thing is contaminated, realizing turns waste into wealth, and compared to traditional sodium methyl mercaptide production technology, there is higher economy, safety and environmental protection to be worth.
Brief description of the drawings
Fig. 1 is the simple process figure of sodium methyl mercaptide production technology.In figure：1. the preheater of 2. water extraction tower of raw material storage tank 3.
4. the stripper reboiler of 8. stripper of thioether rectifying column 5. rectifying column reboiler, 6. rectifying column condenser, 7. surge tank 9.
The product absorption tower 14. of stripper condenser 10. (band storage tank) 11. vaporizers (band surge tank) 12. fine de-sulfur reactor 13.
Divide alkali tank.
Embodiment
The present invention is further illustrated with embodiment below in conjunction with the accompanying drawings, but the scope of protection of present invention is not limited to
In the scope of embodiment statement.
1. raw material continuous purification and continuous absorption production sodium methyl mercaptide
(1) water extraction separating methanol：Material is produced as raw material using the tail gas condenser of dimethyl sulfide synthetic workshop, its raw material
Component is as follows：Dimethyl sulfide 40.74% (wt, similarly hereinafter), methyl mercaptan 55.23%, methanol 1.78%, water 2.15%, hydrogen sulfide
0.10%.By unstripped gas condense to after 15 DEG C with 600m3/ h flow, it is continuously pumped into the bottom of water extraction tower 2 from raw material storage tank 1 and enters
Material mouth, tower middle and upper part is with 300m3/ h flow is continuously pumped into soft water, and aqueous phase inversely contacts with raw material containing methyl mercaptan, in raw material
Methanol is extracted into aqueous phase, and the overflow after tower top aggregation of the organic phase containing methyl mercaptan produces.The top of sampling analysis water extraction tower 2
The material containing mercaptan of extraction, its component are as follows：Dimethyl sulfide 40.95%, methyl mercaptan 54.83%, methanol does not detect, water
4.19%, hydrogen sulfide 0.03%.It can be seen that from data, the methanol in raw material has been removed thoroughly.Extracting system runs one section
After time, extraction is gradually increasing with methanol content in water, is now started with 80m3/ h flow extraction partial extraction water, while with
Identical flow supplements fresh soft water to keep system balancing.The extraction water of extraction contains methanol, hydrogen sulfide, is reclaimed after rectification process
Use.
(2) rectifying desulfurization ether：By the material of methanol removal in step (1), preheated device 3 exchange heat after by thioether rectifying column 4
Middle part continuous feed, the rectifying at 0.8MPa, 75 DEG C, methyl mercaptan and a small amount of hydrogen sulfide, thioether in raw material are from overhead extraction, portion
Divide backflow, partly into next step；Bottom of towe is smart thioether, and continuous extraction to dimethyl sulfide workshop uses.Sampled detection,
The methyl mercaptan gas component of overhead extraction is：Methyl mercaptan 97.82%, thioether 2.14%, hydrogen sulfide 0.04%.
(3) by the material of step (2) overhead extraction, after heat exchange, continuously entered from the middle part of stripper 8 in tower, bottom of towe is again
Boil device 9 to heat using hot water or steam, carry out pressurization stripping, at 0.5~1.0MPa, 20~60 DEG C, in stripping removing raw material
Most of hydrogen sulfide, obtain the organic materials using methyl mercaptan as key component.Control stripper top return flow 1500m3/
h.Hydrogen sulfide in thick methyl mercaptan gas is separated, and return to dimethyl sulfide workshop from tower top synthesizes for thioether；Remaining group
Divide and continuously produced from bottom of towe.Sampling detection stripper bottom production material, its component are：Methyl mercaptan:97.85%, thioether
2.15%, hydrogen sulfide 0.002%.
(4) fixed bed fine de-sulfur：The thick mercaptan gas that step (3) is produced by stripper bottom, enters fine de-sulfur after heat exchange
Reactor 12.Iron oxide series desulfurizing agent is housed, the trace hydrogen sulfide not removed completely in step (3) is de- in essence in the reactor
Further removed in reaction of Salmon-Saxl device.Produced and sample from stripper bottom every 2 hours, detection hydrogen sulfide content remains at
Less than 0.01%, illustrate that stripper depriving hydrogen sulphide has produced a desired effect, now close fine de-sulfur reactor feed, no longer carry out
Fine de-sulfur step.In actual production, if need to open fine de-sulfur reactor, can be required according to product quality (sulfide index)
And the specific condition of production determines.
(5) absorbing by liquid caustic soda：The qualified methyl mercaptan gas of desulfurization, by the bottom continuous feed of product absorption tower 13.By concentration
13%~15% liquid caustic soda is with 100~200m3/ h flow is continuously pumped into product absorption tower middle and upper part, at 40~60 DEG C, pressure
Power is that, with absorbing by liquid caustic soda, liquid caustic soda inversely contacts with methyl mercaptan under 0.2MPa.Methyl mercaptan generates sodium methyl mercaptide by absorbing by liquid caustic soda, from
Product absorb the bottom of the tower is with 100~200m3/ h flow produces to obtain finished product sodium methyl mercaptide solution, sampling detection each index of product
For：Sodium methyl mercaptide 21.24%, vulcanized sodium 0.02%, free alkali 0.08%；A small amount of unabsorbed thioether is not soluble in water and proportion
It is small, absorption tower top is gathered in, overflow returns to dimethyl disulfide after standing and dividing alkali lye to alkali tank 14 is divided as smart dimethyl sulfide
Ether workshop uses.
2. raw material continuous purification and batch absorption production sodium methyl mercaptide
Above continuous absorption, the mode of continuous extraction finished product sodium methyl mercaptide are applied to the stable situation of raw material sources, work as life
When production fluctuation range is larger, using continuous feeding and discharging mode, methyl mercaptan deficiency may be caused make it that the free alkali in product is higher；
Or methyl mercaptan it is higher cause absorb saturation, the situation that excessive methyl mercaptan is wasted.To ensure that product quality is stable, when actual life
The mode of batch absorption should be selected when fluctuation range is larger in production.Now, step (1) to (4) purification of raw materials technique is basically unchanged,
Product absorption tower no longer continuously enters liquid caustic soda and continuously produces product, but after adding enough liquid caustic soda, alkali lye in tower with 500~
800m3/ h flow carries out infinite reflux, and the material containing methyl mercaptan entered to product absorption tower after purification carries out batch absorption.It is to be detected
After alkali liquor absorption saturation, wholly or largely solution repeats to absorb as product, the again enough new liquid caustic soda of property supplement for extraction.
Specifically by the way of accomplished continuously or intermittently absorbing, it can be determined by technical staff according to practical condition.
Embodiment 2
A kind of device of by-product production sodium methyl mercaptide using dimethyl sulphide synthesis, raw material storage tank 1 pass through after being connected with pump
Conveying pipeline is connected with the bottom of water extraction tower 2, and the top of water extraction tower 2 is connected with the top of preheater 3, the bottom of preheater 3 and thioether essence
The middle part of tower 4 is evaporated to connect, the top of thioether rectifying column 4 is connected with rectifying column condenser 6, the bottom of rectifying column condenser 6 through conveying pipeline and
The top of surge tank 7 is connected, and the bottom of surge tank 7 is connected through conveying pipeline with the top of stripper 8, and the bottom of stripper 8 is through conveying pipeline and vapour
Change the connection of the bottom of device 11, the top of vaporizer 11 is connected through conveying pipeline with the bottom of fine de-sulfur reactor 12, and fine de-sulfur reactor 12 pushes up
Portion is connected through conveying pipeline with the bottom of product absorption tower 13, and the top of product absorption tower 13 is through conveying pipeline with dividing alkali tank 14 to be connected.
The bottom of water extraction tower 2 is connected through conveying pipeline with the top of water extraction tower 2, forms circulation loop；The bottom of thioether rectifying column 4
It is connected again with the bottom of thioether rectifying column 4 after conveying pipeline is connected with rectifying column reboiler 5, forms circulation loop；Rectifying column condenses
It is additionally provided with device 6 to the conveying pipeline of surge tank 7 to the conveying pipeline of thioether rectifying column 4；The top of stripper 8 is through conveying pipeline and stripping
After tower condenser 10 connects, then be connected with the top of stripper 8, formation circulation loop；The bottom of stripper 8 and stripper reboiler 9
It is connected to form circulation loop with the bottom of stripper 8 again after connection；The top of vaporizer 11 is additionally provided with to product through conveying pipeline to be absorbed
The conveying pipeline of tower 13.
Claims (1)
1. a kind of method of by-product production sodium methyl mercaptide using dimethyl sulphide synthesis, it is characterised in that comprise the following steps：
（1）Water extracts separating methanol：Material is produced as raw material using the tail gas condenser of dimethyl sulfide synthetic workshop, its raw material components
It is as follows：Dimethyl sulfide 40.74wt%, methyl mercaptan 55.23wt%, methanol 1.78wt%, water 2.15wt%, hydrogen sulfide 0.10wt% will
Unstripped gas is condensed to 600m3/h flow, the bottom feed mouth of water extraction tower 2 being continuously pumped into from raw material storage tank 1, in tower after 15 DEG C
Top is continuously pumped into soft water with 300m3/h flow, and aqueous phase is inversely contacted with raw material containing methyl mercaptan, and the methanol in raw material is extracted
Into aqueous phase, the overflow after tower top aggregation of the organic phase containing methyl mercaptan produces, the sulfur-bearing of the top of sampling analysis water extraction tower 2 extraction
Alcohol material, its component are as follows：Dimethyl sulfide 40.95%, methyl mercaptan 54.83%, methanol does not detect, water 4.19%, hydrogen sulfide
0.03%；
（2）Rectifying desulfurization ether：By step（1）The material of middle methanol removal, by the middle part of thioether rectifying column 4 after the preheated heat exchange of device 3
Continuous feed, the rectifying at 0.8MPa, 75 DEG C, methyl mercaptan and a small amount of hydrogen sulfide, thioether in raw material return from overhead extraction, part
Stream, partly into next step；Bottom of towe is smart thioether, and continuous extraction to dimethyl sulfide workshop uses, sampled detection, tower top
The methyl mercaptan gas component of extraction is：Methyl mercaptan 97.82%, thioether 2.14%, hydrogen sulfide 0.04%；
（3）By step（2）The material of overhead extraction, after heat exchange, continuously entered from the middle part of stripper 8 in tower, tower bottom reboiler 9
Heated using hot water or steam, carry out pressurization stripping, at 0.5 ~ 1.0MPa, 20 ~ 60 DEG C, the major part in stripping removing raw material
Hydrogen sulfide, the organic materials using methyl mercaptan as key component is obtained, control stripper top return flow 1500m3/h, thick first sulphur
Hydrogen sulfide in alcohol gas is separated, and return to dimethyl sulfide workshop from tower top synthesizes for thioether；Remaining component is from bottom of towe
Continuous extraction, sampling detection stripper bottom production material, its component are：Methyl mercaptan:97.85%, thioether 2.15%, hydrogen sulfide
0.002%；
（4）Fixed bed fine de-sulfur：Step（3）The thick mercaptan gas produced by stripper bottom, fine de-sulfur reaction is entered after heat exchange
Device 12；Iron oxide series desulfurizing agent, step are housed in the reactor（3）In the trace hydrogen sulfide that does not remove completely it is anti-in fine de-sulfur
Answer and further removed in device, produced and sample from stripper bottom every 2 hours, detection hydrogen sulfide content remains at
Less than 0.01%, illustrate that stripper depriving hydrogen sulphide has produced a desired effect, now close fine de-sulfur reactor feed, no longer carry out
Fine de-sulfur step；
（5）Absorbing by liquid caustic soda：The qualified methyl mercaptan gas of desulfurization, by the bottom continuous feed of product absorption tower 13, by concentration 13% ~ 15%
Liquid caustic soda product absorption tower middle and upper part is continuously pumped into 100 ~ 200m3/h flow, at 40 ~ 60 DEG C, pressure be 0.2MPa under,
With absorbing by liquid caustic soda, liquid caustic soda inversely contacts with methyl mercaptan, and methyl mercaptan generates sodium methyl mercaptide by absorbing by liquid caustic soda, from product absorb the bottom of the tower
Produce to obtain finished product sodium methyl mercaptide solution with 100 ~ 200m3/h flow, sampling detection each index of product is：Sodium methyl mercaptide
21.24%, vulcanized sodium 0.02%, free alkali 0.08%；A small amount of unabsorbed thioether is not soluble in water and proportion is small, is gathered in absorption
Tower top, to alkali tank 14 is divided, returning to dimethyl sulfide workshop as smart dimethyl sulfide after standing and dividing alkali lye uses for overflow；
(6) raw material continuous purification and batch absorption production sodium methyl mercaptide
Step（1）Extremely（4）Purification of raw materials technique is basically unchanged, and product absorption tower no longer continuously enters liquid caustic soda and continuously produces product, and
It is that alkali lye carries out infinite reflux in tower with 500 ~ 800m3/h flow, after entering purification to product absorption tower after adding enough liquid caustic soda
Material containing methyl mercaptan carry out batch absorption, after alkali liquor absorption saturation to be detected, extraction wholly or largely solution as product,
The enough new liquid caustic soda of property supplement repeat to absorb again, that is, obtain sodium methyl mercaptide.
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| CN108250114B (en) * | 2018-03-01 | 2023-12-29 | 贵州兴发化工有限公司 | Sodium methyl mercaptide production process and device |
| CN111718239A (en) * | 2020-07-16 | 2020-09-29 | 福建师范大学福清分校 | Method for separating dimethyl sulfide and methanol aqueous solution by continuous extractive distillation |
| CN112778174A (en) * | 2021-04-12 | 2021-05-11 | 蓝星安迪苏南京有限公司 | Device and method for preparing high-concentration sodium methyl mercaptide solution |
| CN114702420A (en) * | 2022-05-07 | 2022-07-05 | 宁夏紫光天化蛋氨酸有限责任公司 | Method for separating methyl mercaptan and dimethyl sulfide |
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| US4186061A (en) * | 1977-06-24 | 1980-01-29 | Phillips Petroleum Company | Fractionation of methyl-mercaptan reactor effluent |
| CN1033309C (en) * | 1992-07-09 | 1996-11-20 | 湖北省化学研究所 | Organic and inorganic sulfur removing technology at normal temp |
| CN103992253B (en) * | 2014-06-05 | 2016-03-02 | 刘成旭 | A kind of preparation method utilizing industrial gaseous waste to generate electronic-grade dimethyl thioether |
| CN105330577A (en) * | 2015-11-30 | 2016-02-17 | 白国强 | Production technology of high-purity sodium methyl mercaptide |
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Effective date of registration: 20221101 Address after: 843099 Zhejiang Industrial Park (West Park), Aksu economic and Technological Development Zone, Aksu Prefecture, Xinjiang Uygur Autonomous Region Patentee after: Xinjiang Xingfa Chemical Co.,Ltd. Address before: 443711 Hunan Road, Gufu Town, Xingshan County, Yichang City, Hubei Province Patentee before: HUBEI XINGFA CHEMICALS GROUP Co.,Ltd. |