CN205653375U - Dimethyl disulfide ether apparatus for producing - Google Patents
Dimethyl disulfide ether apparatus for producing Download PDFInfo
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- CN205653375U CN205653375U CN201620380339.3U CN201620380339U CN205653375U CN 205653375 U CN205653375 U CN 205653375U CN 201620380339 U CN201620380339 U CN 201620380339U CN 205653375 U CN205653375 U CN 205653375U
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Abstract
The utility model relates to a dimethyl disulfide ether apparatus for producing. It just leads to these cross connection of each other that cross the multiple arrangement including alkali preparation tank (8), phase splitter (9), precision filter (11), one -level static mixer (1), second grade static mixer (2), one -level cauldron (3), second grade cauldron (4), one -level blender (5), second grade blender (6) and autoclave multiple arrangements such as (7), has realized a lot of cross circulation process of material in the device, has improved reaction product's yield greatly.
Description
Technical field
This utility model relates to the production of dimethyl disulfide, particularly relates to a kind of Methyl disulfide ether production equipment.
Background technology
It is presently used for the conventional equipment that dimethyl disulfide (DMDS) produces and is mainly batch tank reactor.Inventionbriefly, it is with sodium sulfide, sulfur, dimethyl sulfate as raw material, reacts in batch tank reactor, obtains metabisulfite solution (in lower floor), and dimethyl disulfide and water (on upper strata).But when using conventional equipment to produce according to existing technique, but also exist: 1, methanthiol reaction is not exclusively, has obvious abnormal flavour；2, conveying pipeline can crystallize because of sodium methyl mercaptide, and then block pipeline, affect many unfavorable factors such as reaction；3, the yield of product dimethyl disulfide is low, and yield is only 70%～85%.
Utility model content
The purpose of this utility model is to provide a kind of Methyl disulfide ether production equipment, this process units is when the production of dimethyl disulfide, methanthiol reaction can be made completely, also be avoided that the crystallization of methanthiol salt, and then block pipeline, affect many unfavorable factors such as reaction.
The purpose of this utility model is achieved through the following technical solutions:
A kind of Methyl disulfide ether production equipment, it is characterised in that: it includes alkali-prepared tank and autoclave, still and static mixer；Described static mixer connects with feeding line, described still and described alkali-prepared tank respectively；Described still connects with waste line, described autoclave the most respectively.
When using said apparatus to produce, liquid methanthiol direct gasification in feeding line joins static mixer, fast reaction is carried out with by the liquid caustic soda come in alkali-prepared tank, the methanthiol salt that reaction generates caches in still, to be detected qualified after, extraction enters oxidation in autoclave and generates dimethyl disulfide.Waste gas is then discharged by waste line.This device production is used to prepare dimethyl disulfide, it is to avoid methanthiol salt-pepper noise, and then blocking pipeline, impact reaction.
In order to realize unreacted liquid caustic soda circulating reflux, and the liquid caustic soda added with liquid caustic soda tank mixes participation reaction, and as optimizing further, above-mentioned Methyl disulfide ether production equipment, it also has additional blender；Described blender is serially connected between above-mentioned static mixer and above-mentioned alkali-prepared tank, and described blender also connects with described still.
As optimizing further, above-mentioned Methyl disulfide ether production equipment, it is provided with alkali-prepared tank, autoclave, one-level static mixer, two grades of static mixers, one-level still, two grades of stills, one-level blender and secondary mixer；Described one-level static mixer connects with feeding line, described one-level still and described one-level blender respectively；Described one-level still connects with described two grades of static mixers, described one-level blender and described autoclave the most respectively；Described one-level blender also connects with described two grades of stills；Described two grades of static mixers connect with described two grades of stills and described secondary mixer the most respectively；Described two grades of stills connect with described secondary mixer and waste line the most respectively；Described secondary mixer also connects with described alkali-prepared tank.
As optimizing further, above-mentioned Methyl disulfide ether production equipment, it also includes phase separator and accurate filter；Above-mentioned autoclave connects with catalyst feed line, oxidant feed pipeline, described phase separator and waste line the most respectively；Described phase separator connects with described accurate filter and waste liquid pipeline the most respectively.
For improving the yield of product dimethyl disulfide further, and more efficiently by the aqueous phase material recycleds such as methanthiol salt complete for unreacted and strong base solution, above-mentioned Methyl disulfide ether production equipment, also have additional liquid caustic soda enrichment facility；Described liquid caustic soda enrichment facility is connected with above-mentioned alkali-prepared tank, above-mentioned phase separator, steam pipe line and waste line respectively.
As optimizing further, above-mentioned Methyl disulfide ether production equipment, also have additional gas-liquid separator；Described gas-liquid separator can be serially connected between above-mentioned two grades of stills and the waste line being connected on above-mentioned two grades of stills, or/and can be serially connected between above-mentioned autoclave and the waste line being connected on above-mentioned autoclave, and described gas-liquid separator is connected with between above-mentioned two grades of stills, above-mentioned autoclave respectively and has reflux pipeline.
As optimizing further, above-mentioned Methyl disulfide ether production equipment, also have additional multiphase flow reaction pump；Above-mentioned autoclave is provided with the pipeloop connected with autoclave, to realize the circulation of material in still；Described multiphase flow reaction pump is connected on described pipeloop；Above-mentioned catalyst feed line, above-mentioned oxidant feed pipeline, and the connection pipeline of above-mentioned one-level still and above-mentioned autoclave, be connected to the feed end of described multiphase flow reaction pump respectively.By setting up multiphase flow reaction pump, gas phase can be beaten to micron order, strengthen gas-liquid two-phase contact surface, and shorten the response time, improve reaction efficiency.
This utility model has the advantages that
This utility model provides a kind of Methyl disulfide ether production equipment, it is by the connection that crosses one another of multiple devices, achieve the material repeatedly cross-circulation process in device, substantially increase the yield of product, when being applied to associating absorbing by liquid caustic soda method and oxidizing process specifically to prepare dimethyl disulfide, methanthiol is reacted and free from extraneous odour completely, the yield of product dimethyl disulfide may be up to few 93%, and achieve effective control of methanthiol salt in pipeline, avoid the crystallization of methanthiol salt, and then blocking pipeline, affect many unfavorable factors such as reaction, be suitable to industrialized production promote.
Accompanying drawing explanation
Fig. 1 is the attachment structure schematic diagram of Methyl disulfide ether production equipment described in this utility model embodiment 1.
Fig. 2 is the attachment structure schematic diagram of Methyl disulfide ether production equipment described in this utility model embodiment 2.
Fig. 3 is the attachment structure schematic diagram of Methyl disulfide ether production equipment described in this utility model embodiment 3.
Detailed description of the invention
Below by specific embodiment, this utility model is specifically described; it is pointed out here that following example are served only for being further described this utility model; it is not intended that the restriction to its protection domain, this utility model can be made some nonessential improvement and adjustment according to foregoing by the person skilled in the art of this area.
Embodiment 1
As shown in Figure of description 1, a kind of Methyl disulfide ether production equipment, it includes 1, two grades of static mixers 2 of one-level static mixer, 3, two grades of stills 4 of one-level still, one-level blender 5, secondary mixer 6, autoclave 7, alkali-prepared tank 8, phase separator 9, liquid caustic soda enrichment facility 10, accurate filter 11 and gas-liquid separator 12；One-level static mixer 1 connects with feeding line, one-level still 3 and one-level blender 5 respectively；One-level still 3 connects with two grades of static mixers 2, one-level blender 5 and autoclave 7 the most respectively；One-level blender 5 also connects with two grades of stills 4；Two grades of static mixers 2 connect with two grades of stills 4 and secondary mixer 6 the most respectively；Two grades of stills 4 connect with secondary mixer 6 and waste line the most respectively；Secondary mixer 6 also connects with alkali-prepared tank 8；Autoclave 7 connects with catalyst feed line, oxidant feed pipeline, phase separator 9 and waste line the most respectively；Phase separator 9 connects with accurate filter 11 and waste liquid pipeline the most respectively；Liquid caustic soda enrichment facility 10 is connected with alkali-prepared tank 8, phase separator 9, steam pipe line and waste line respectively；Gas-liquid separator 12 is two, one of them is serially connected between two grades of stills 4 and the waste line being connected on two grades of stills 4, another is serially connected between autoclave 7 and the waste line being connected on autoclave 7, and gas-liquid separator 12 respectively and is respectively connected with reflux pipeline between two grades of stills 4, autoclaves 7.
When using the Methyl disulfide ether production equipment in this example to produce, by liquid methanthiol direct gasification in feeding line joins one-level static mixer 1, fast reaction is carried out with the liquid caustic soda come in one-level blender 5, the methanthiol salt that reaction generates caches in one-level still 3, and a part of material extraction enters and generates dimethyl disulfide in autoclave 7.The methyl mercaptan gas not absorbed is overflowed by one-level still 3 top, enters two grades of static mixers 2, and the liquid caustic soda come with secondary mixer 6 in two grades of static mixers 2 carries out absorbing reaction, and the low concentration methanthiol salt that reaction generates enters in two grades of stills 4 and caches.Reactant liquor in two grades of stills 4 is low methanthiol salt height aqueous slkali, and part extraction enters one-level blender 5, is partially into secondary mixer 6；Alkali-prepared tank 8 reclaims the liquid caustic soda come by liquid caustic soda enrichment facility 10, and is configured to certain concentration entrance secondary mixer 6, then loops to two grades of static mixers 2 and participates in the absorption reaction of methanthiol.The gas-liquid mixture externally to discharge separates via gas-liquid separator 12, and waste gas enters exhaust-gas treatment operation, and liquid then flows in two grades of stills 4.
Qualified methanthiol salt is by one-level still 3 extraction, it is sent directly in autoclave 7 and carries out reaction under high pressure with oxidant, catalyst, waste gas also enters gas-liquid separator 12, waste gas removes exhaust treatment system, reactant liquor carries out two-phase laminated flow through phase separator 9, upper oil phase dimethyl disulfide carries out catalyst separation through accurate filter 11, and catalyst can be with reuse, and the product dimethyl disulfide filtered out is certified products.Split-phase liquid caustic soda out is owing to there being water to generate in course of reaction, so to carry out distillation process through liquid caustic soda enrichment facility 10, waste gas frowzy enters exhaust-gas treatment operation.Liquid caustic soda after concentration is carried out methanthiol salt by liquid caustic soda enrichment facility 10 dozens to alkali-prepared tank 8 to be prepared.
By the regulation of the materials such as liquid caustic soda in multiple devices such as liquid caustic soda enrichment facility is controlled, it is achieved that to effective control of methanthiol salt in pipeline, it is to avoid crystallize because of it, and then blocking pipeline, affect many unfavorable factors such as reaction；When using the device in this example to produce after testing, the yield of its product dimethyl disulfide is up to 96.5%.
Embodiment 2
As shown in Figure of description 2, a kind of Methyl disulfide ether production equipment, it includes 1, two grades of static mixers 2 of one-level static mixer, 3, two grades of stills 4 of one-level still, one-level blender 5, secondary mixer 6, autoclave 7, alkali-prepared tank 8, phase separator 9, liquid caustic soda enrichment facility 10 and accurate filter 11；One-level static mixer 1 connects with feeding line, one-level still 3 and one-level blender 5 respectively；One-level still 3 connects with two grades of static mixers 2, one-level blender 5 and autoclave 7 the most respectively；One-level blender 5 also connects with two grades of stills 4；Two grades of static mixers 2 connect with two grades of stills 4 and secondary mixer 6 the most respectively；Two grades of stills 4 connect with secondary mixer 6 and discharging pipeline the most respectively；Secondary mixer 6 also connects with alkali-prepared tank 8；Autoclave 7 connects with catalyst feed line, oxidant feed pipeline, phase separator 9 and discharging pipeline the most respectively；Phase separator 9 connects with accurate filter 11 and discharging pipeline the most respectively；Liquid caustic soda enrichment facility 10 is connected with alkali-prepared tank 8, phase separator 9, steam pipe line and discharging pipeline respectively.
Methyl disulfide ether production equipment using method in this example is with embodiment 1, and when using the device in this example to produce after testing, the yield of its product dimethyl disulfide is up to 93.2%.
Embodiment 3
As shown in Figure of description 3, a kind of Methyl disulfide ether production equipment, it includes 1, two grades of static mixers 2 of one-level static mixer, 3, two grades of stills 4 of one-level still, one-level blender 5, secondary mixer 6, autoclave 7, alkali-prepared tank 8, phase separator 9, liquid caustic soda enrichment facility 10, accurate filter 11, gas-liquid separator 12 and multiphase flow reaction pump 13；One-level static mixer 1 connects with feeding line, one-level still 3 and one-level blender 5 respectively；One-level still 3 connects with two grades of static mixers 2, one-level blender 5 and autoclave 7 the most respectively；One-level blender 5 also connects with two grades of stills 4；Two grades of static mixers 2 connect with two grades of stills 4 and secondary mixer 6 the most respectively；Two grades of stills 4 connect with secondary mixer 6 and waste line the most respectively；Secondary mixer 6 also connects with alkali-prepared tank 8；Autoclave 7 connects with catalyst feed line, oxidant feed pipeline, phase separator 9 and waste line the most respectively；Phase separator 9 connects with accurate filter 11 and waste liquid pipeline the most respectively；Liquid caustic soda enrichment facility 10 is connected with alkali-prepared tank 8, phase separator 9, steam pipe line and waste line respectively；Gas-liquid separator 12 is two, one of them is serially connected between two grades of stills 4 and the waste line being connected on two grades of stills 4, another is serially connected between autoclave 7 and the waste line being connected on autoclave 7, and gas-liquid separator 12 respectively and is respectively connected with reflux pipeline between two grades of stills 4, autoclaves 7；Autoclave 7 is provided with the pipeloop 14 that connect internal with autoclave 7；Multiphase flow reaction pump 13 is connected on pipeloop 14；Catalyst feed line, oxidant feed pipeline, and one-level still 3 and the connection pipeline of autoclave 7, be connected to the feed end of multiphase flow reaction pump 13 respectively.
Methyl disulfide ether production equipment using method in this example is with embodiment 1, wherein, catalyst, oxidant, and connect, through one-level still 3 and autoclave 7, the qualified methanthiol salt that pipeline is passed through, mixing is more fully contacted in multiphase flow reaction pump 13, significantly shorten the response time, improve reaction efficiency.
Claims (6)
1. a Methyl disulfide ether production equipment, it is characterised in that: it is provided with alkali-prepared tank (8), autoclave (7), one-level static mixer (1), two grades of static mixers (2), one-level still (3), two grades of stills (4), one-level blender (5) and secondary mixer (6)；Described one-level static mixer (1) connects with feeding line, described one-level still (3) and described one-level blender (5) respectively；Described one-level still (3) connects with described two grades of static mixers (2), described one-level blender (5) and described autoclave (7) the most respectively；Described one-level blender (5) also connects with described two grades of stills (4)；Described two grades of static mixers (2) connect with described two grades of stills (4) and described secondary mixer (6) the most respectively；Described two grades of stills (4) connect with described secondary mixer (6) and waste line the most respectively；Described secondary mixer (6) also connects with described alkali-prepared tank (8).
2. Methyl disulfide ether production equipment as claimed in claim 1, it is characterised in that: it also includes phase separator (9) and accurate filter (11)；Described autoclave (7) connects with catalyst feed line, oxidant feed pipeline, described phase separator (9) and waste line the most respectively；Described phase separator (9) connects with described accurate filter (11) and waste liquid pipeline the most respectively.
3. Methyl disulfide ether production equipment as claimed in claim 1 or 2, it is characterised in that: it also has additional phase separator (9) and liquid caustic soda enrichment facility (10)；Described liquid caustic soda enrichment facility (10) is connected with described alkali-prepared tank (8), described phase separator (9), steam pipe line and waste line respectively.
4. Methyl disulfide ether production equipment as claimed in claim 1 or 2, it is characterised in that: it also has additional gas-liquid separator (12)；Described gas-liquid separator (12) is serially connected between described two grades of stills (4) and the waste line being connected on described two grades of stills (4), or/and be serially connected between described autoclave (7) and the waste line being connected on described autoclave (7), and described gas-liquid separator (12) is connected with between described two grades of stills (4), described autoclave (7) respectively and has reflux pipeline.
5. Methyl disulfide ether production equipment as claimed in claim 3, it is characterised in that: it also has additional gas-liquid separator (12)；Described gas-liquid separator (12) is serially connected between described two grades of stills (4) and the waste line being connected on described two grades of stills (4), or/and be serially connected between described autoclave (7) and the waste line being connected on described autoclave (7), and described gas-liquid separator (12) is connected with between described two grades of stills (4), described autoclave (7) respectively and has reflux pipeline.
6. Methyl disulfide ether production equipment as claimed in claim 2, it is characterised in that: it also has additional multiphase flow reaction pump (13)；Described autoclave (7) is provided with the pipeloop (14) that connect internal with autoclave (7)；Described multiphase flow reaction pump (13) is connected on described pipeloop (14)；Described catalyst feed line, described oxidant feed pipeline, and the connection pipeline of described one-level still (3) and described autoclave (7), be connected to the feed end of described multiphase flow reaction pump (13) respectively.
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| CN2016201164713 | 2016-02-05 | ||
| CN201620116471 | 2016-02-05 |
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| CN205653375U true CN205653375U (en) | 2016-10-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152585A (en) * | 2019-07-01 | 2019-08-23 | 扬州市职业大学(扬州市广播电视大学) | A kind of reaction kettle for dimethyl disulfide production |
| CN114570319A (en) * | 2022-03-23 | 2022-06-03 | 扬州市职业大学(扬州开放大学) | A reation kettle for dimethyl disulfide production |
-
2016
- 2016-04-28 CN CN201620380339.3U patent/CN205653375U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110152585A (en) * | 2019-07-01 | 2019-08-23 | 扬州市职业大学(扬州市广播电视大学) | A kind of reaction kettle for dimethyl disulfide production |
| CN114570319A (en) * | 2022-03-23 | 2022-06-03 | 扬州市职业大学(扬州开放大学) | A reation kettle for dimethyl disulfide production |
| CN114570319B (en) * | 2022-03-23 | 2023-09-29 | 扬州市职业大学(扬州开放大学) | Reaction kettle for producing dimethyl disulfide |
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| Date | Code | Title | Description |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A dimethyl disulfide production unit Effective date of registration: 20200904 Granted publication date: 20161019 Pledgee: Chongqing chemical medicine holding (Group) Co.,Ltd. Pledgor: NINGXIA UNISPLENDOUR TIANHUA METHIONINE Co.,Ltd. Registration number: Y2020500000011 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20230711 Granted publication date: 20161019 Pledgee: Chongqing chemical medicine holding (Group) Co.,Ltd. Pledgor: NINGXIA UNISPLENDOUR TIANHUA METHIONINE Co.,Ltd. Registration number: Y2020500000011 |
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| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of utility model: A dimethyl disulfide production device Effective date of registration: 20230725 Granted publication date: 20161019 Pledgee: Chongqing chemical medicine holding (Group) Co.,Ltd. Pledgor: NINGXIA UNISPLENDOUR TIANHUA METHIONINE Co.,Ltd. Registration number: Y2023500000053 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |