CN202490608U - Safety production device of dimethyl sulfide oxidizing reaction - Google Patents
Safety production device of dimethyl sulfide oxidizing reaction Download PDFInfo
- Publication number
- CN202490608U CN202490608U CN2012200546873U CN201220054687U CN202490608U CN 202490608 U CN202490608 U CN 202490608U CN 2012200546873 U CN2012200546873 U CN 2012200546873U CN 201220054687 U CN201220054687 U CN 201220054687U CN 202490608 U CN202490608 U CN 202490608U
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- China
- Prior art keywords
- feed pipe
- nitrogen dioxide
- thioether
- oxidizing tower
- tower
- Prior art date
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Abstract
The utility model relates to a safety production device of dimethyl sulfide oxidizing reaction. A precision flowmeter, a feed regulating valve and a stop valve are respectively arranged on a nitrogen dioxide feed pipe, an oxygen feed pipe and a refined thioether feed pipe of the safety production device. A tail gas emptying valve is positioned on the top of an oxidizing tower. A detecting device used for measuring temperature and pressure is disposed in the oxidizing tower. The detecting device, the stop valve and the tail gas emptying valve are respectively connected with a programmable logic controller (PLC) interlocking protection system. Tail gas of the oxidizing tower is led to a neutralizing treatment device. Use level of nitrogen dioxide, oxygen and refined thioether is strictly controlled. feeding is done according to the standards that thioether feed flow is 300 to 400 kg/h, oxygen feed flow is 60-80 Nm<3>/h, and nitrogen dioxide feed flow is 10-30 Nm<3>/h. Nitrogen dioxide is added first, then, oxygen is added, and refined thioether is added at last. Temperature of each tower section of the oxidizing tower is controlled. The safety production device effectively prevents thioether from being excessive, also enables an oxidizing reaction area to be concentrated and enables reaction to be full, and ensures safety production state of the oxidizing tower.
Description
Technical field
The utility model relates to a kind of process units of dimethyl sulfide oxidation reaction, belongs to chemical production technical field.
Background technology
The technology of existing sulfide oxidation mainly contains following steps:
1) nitrogen dioxide vaporization flow process
The liquid dinitrogen tetroxide that stores in the raw material dinitrogen tetroxide storage tank; Measure through Liquid level adjusting valve control and flowmeter through the nitrogen oxide pump; Squeeze in the nitrogen oxide surge tank; The liquid level of control nitrogen oxide surge tank feeds hot water to the nitrogen oxide surge tank dinitrogen tetroxide is heated vaporization, through the pressure of pressure-regulating valve control nitrogen oxide surge tank; The nitrogen dioxide gas of vaporization after the control and regulation of control valve and a metal pipe float flowmeter metering, entering oxidizing tower in the middle part of second tower joint at the bottom of the oxidizing tower.
2) oxygen flow process
About 1.0MPa oxygen that system pipe network is come gets into the oxygen surge tank after pressure-regulating valve decompression, the oxygen that the oxygen surge tank comes out saves the entering oxidizing tower from oxidizing tower first tower after control valve control and regulation and a metal pipe float flow meter metering.
3) sulfide oxidation flow process
Smart thioether is through the convey materials pump; Respectively through Flux Valve Control regulate with a metal pipe float flow meter metering after more respectively by three the thioethers inlets in upper, middle and lower (selecting one of them entry position) second and third tower joint entering oxidizing tower at the bottom of the oxidizing tower; At a certain temperature; In the dimethyl sulfoxide (DMSO) mother liquor that has absorbed nitrogen dioxide, oxygen in advance, carry out the liquid phase emulsion reaction with a certain proportion of nitrogen dioxide, oxygen and generate thick dimethyl sulfoxide (DMSO), the extraction at the bottom of the tower of the thick sulfoxide of generation gets into thick sulfoxide storage tank.
The reaction principle of sulfide oxidation:
Thioether is under 60～75 ℃ the condition in temperature, under the catalytic action of nitrogen dioxide, generates thick dimethyl sulfoxide (DMSO) with oxygen reaction.Oxygen in the course of reaction, nitrogen dioxide are excessive, and excess of oxygen and nitrogen dioxide are delivered to tail gas absorber from the oxidizing tower top with the form of tail gas and carried out tail gas and absorb and handle, and the thick sulfoxide of generation gets into thick sulfoxide storage tank.Its reaction mechanism is following:
Main reaction: (CH
3)
2S+NO
2=(CH
3)
2SO+NO ↑+Q
Put
2NO+O
2=2NO
2↑+Q
Put
Side reaction: 3NO
2+ H
2O=2HNO
3+ NO+Q
Put
(CH
3)
2SO+2HNO
3=(CH
3)
2SO
2+ H
2O+2NO
2+ Q
Put
Main reaction after the merging is: 2 (CH
3)
2S+O
2=2 (CH
3)
2SO+Q
Put
The weak point that prior art exists mainly contains:
1) the sulfoxide device does not prevent the robust techniques measure of the excessive entering oxidizing tower of thioether.The flow-meter that has only a low precision on three kinds of material feeding lines of oxidizing tower; In case wrong being presented under the condition that does not have other flowmeters to do reference occur; Make operating personnel be difficult to the authenticity that judgment data shows; The as easy as rolling off a log proportioning of three kinds of materials that causes is improper, causes thioether excessive and accidents caused.
2) the sulfoxide device is not stopped the robust techniques measure that thioether gets into the exhaust emissions pipeline yet.
Contain excessive nitrogen dioxide gas in the tail gas of oxidizing tower, former technical flow design reclaims drainer for reclaiming the nitrogen dioxide in the oxidizing tower tail gas through a nitrogen oxide condenser and nitrogen oxide.Contact with oxygen and together get into when gathering certain equivalent in the oxidizing tower exhaust pipe, very easily explosion caused accident if thioether is excessive.
3) design of the feed distributor of two materials of oxidizing tower is unreasonable: (distributor designs of oxygen is reasonable)
The distributor of oxygen: rich font distributor
The distributor of nitrogen oxide: straight arm type distributor
The distributor of smart thioether: straight arm type distributor
The problem that exists: the distributor of thioether is the straight arm type distributor, just begins to distribute near tower wall place, and has been covered with distributed holes on the surface; Material is distributed not to be concentrated; Make thioether to around and near tower wall place diffusion profile, and in (sulfoxide is than great and extraction at the bottom of the tower) under the thick sulfoxide effect that generates, the liquid thioether that distributes near the tower wall moves down easily thereupon; Thereby cause oxidation main reaction region position to move down, thereby the safety that jeopardizes oxidizing tower.The distributor of nitrogen oxide also is the straight arm type distributor, and project organization is with the thioether feed distributor, exists equally material to be distributed do not concentrate, make nitrogen oxide to around and near tower wall place diffusion profile.In a word, do not concentrate and the bad control in position that irrational distribution effect causes the oxidation main reaction region easily, make that simultaneously reaction mass also is not easy to react completely.
4) oxidizing tower harmfulness is bigger, but lacks the safety interlocking protection system, also lacks the reliable and secure measure of under abnormal conditions, cutting off the oxidizing tower charging rapidly.
Summary of the invention
The purpose of the utility model is to overcome above-mentioned deficiency; A kind of safety in production device of dimethyl sulfide oxidation reaction is provided; This kind device has an accident in the time of preventing the oxidizing tower operation, reduces the risk of operation, makes oxidizing tower itself be in a kind of comparatively safe operating condition and state.
The technical scheme that the utility model is taked is:
A kind of safety in production device of dimethyl sulfide oxidation reaction; Comprise nitrogen dioxide feed pipe, oxygen feed pipe, nitrogen feed pipe, smart thioether feed pipe, oxidizing tower; Be respectively equipped with accurate flowmeter, material control valve and stop valve on nitrogen dioxide feed pipe, oxygen feed pipe, the smart thioether feed pipe; The tail gas atmospheric valve is arranged at the oxidizing tower top; Be provided with the checkout gear of measuring temperature, pressure in the oxidizing tower, checkout gear, stop valve, tail gas atmospheric valve connect PLC interlock protection system, and the tail gas of oxidizing tower is connected into the neutralisation treatment device.
Described smart thioether feed pipe, nitrogen dioxide feed pipe put in and partly are connected with distributor in the oxidizing tower; The distributor of smart thioether feed pipe is a sleeve-like straight arm type distributor; Inner core one end opening and opening surface are upwards; The distributor of nitrogen dioxide feed pipe is a sleeve-like straight arm type distributor, and inner core one end opening and opening surface are downward.
Described accurate flowmeter is provided with a plurality of on every feed pipe.
Described stop valve is for cutting off ball valve.
Described nitrogen dioxide feed pipe is provided with the nitrogen dioxide gas-liquid separator, and nitrogen dioxide gas-liquid separator both sides are respectively equipped with a nitrogen dioxide stop valve.The nitrogen dioxide stop valve connects PLC interlock protection system.Because the very corrosive of nitrogen oxide; The nitrogen oxide table of sulfide oxidation system all has corrosion in various degree; Influenced ordinary production, increased gas-liquid separator, prevented that effectively the nitrogen oxide of liquefaction from getting into oxidizing tower; Cause acid number higher, stop valve is positioned at two ends when having prevented flow in respect of leak source effectively, and a large amount of nitrogen oxides leaks.
Described oxidizing tower is looked handleless cup at cat head liquid level gauge, tower bottom flow amount meter and cat head tail gas camera has been installed respectively, and camera connects monitoring system, and the control room is monitored color and state constantly.
A plurality of long-range points for measuring temperature are set in the described oxidizing tower, and the temperature of test shows that in monitoring system the control room operating personnel are very favourable to state of temperature and the variation tendency of holding whole oxidizing tower.
Sulfide oxidation system exhaust pipe is separated and transforms, avoid pipeline to connect each other, prevent that material from gathering, and prevents similar accident in exhaust pipe.Nitrogen oxide tail gas on the equipment such as oxidizing tower, stripping tower, neutralizing tank, nitrogen oxide surge tank, thick sulfoxide storage tank, neutral sulfoxide groove, neutral sulfoxide head tank is all separated and introduces the absorption tower separately; Avoid pipeline to connect each other; Prevent that material from mixing, gathering, and tries to avert accidents in exhaust pipe.
The tail gas of two sulfide oxidation towers gets into absorption tower separately, and thick sulfoxide gas is carried tail gas and got into the absorption tower separately, and the tail gas that produces with part in the thick sulfoxide gets into the absorption tower separately.
The beneficial effect of the utility model is:
(1) the PLC interlock protection system of oxidizing tower connection can be from guaranteeing the safe and stable operation of oxidizing tower in essence.In case the main reaction region temperature of oxidizing tower, the pressure of oxidizing tower and liquid level, when situation such as three kinds of material feed rates are unusual occurred, the chain program of oxidizing tower was carried out immediately, and two stop valves on the thioether feeding line cut out immediately, open the cat head nitrogen valve.Strict feeding sequence and the charge ratio of carrying out the oxidizing tower absorption, driving thrown nitrogen dioxide earlier, throws oxygen again, throws thioether at last again, improves still strict this program of carrying out when loading.Guarantee material proportion, prevented the excessive of thioether effectively.
(2) tail gas of oxidizing tower is former is designed to reclaim nitrogen dioxide gas; Has certain danger owing to reclaim; After technological transformation, nitrogen dioxide is not reclaimed, adopt the method for neutralisation treatment to carry out harmless treatment; Fundamentally prevented to cause because of thioether is excessive combustible etc. in exhaust pipe, assemble the accident of blasting maybe, accomplished essential safety.
(3) superiority transformed of distributor, the distribution of nitrogen oxide and thioether have been avoided that part of near tower body, and the distributor opening of thioether makes progress, thus the possibility of having avoided thioether to move down.Open Side Down for the distributor of nitrogen oxide, and purpose is in order to reach better diffusion effect, thereby nitrogen oxide gas upwards stirs and makes the sulfide oxidation reaction more cmpletely, has reduced the occurrence probability that oxidation reaction moves down, and helps the safe and stable operation of oxidizing tower.
(4) oxidizing tower cat head liquid level and the tower bottom flow amount handleless cup of looking of taking into account cat head tail gas blow-down pipe has camera head monitor respectively; Signal is introduced to the control room; The control room personnel can monitor constantly, and color and state are if unusual personnel occurring can in time find, this is a kind of reliable intuitively surveillance and control measure.
(5) behind charging control valve on three material feeding lines of oxidizing tower, increase by two simultaneously and cut off ball valves, cut off charging rapidly when being in an emergency, oxidizing tower is guaranteed at a comparatively safe state.
Description of drawings
Fig. 1 is the safety in production apparatus structure of the utility model;
Fig. 2 is the process units structure before transforming;
Fig. 3 is the structure of distributor of smart thioether feed pipe before transforming;
Fig. 4 is the structure of distributor of the smart thioether feed pipe of the utility model;
Fig. 5 is the structure of distributor of nitrogen dioxide feed pipe before transforming;
Fig. 6 is the structure of distributor of the nitrogen dioxide feed pipe of the utility model;
Wherein, 1. oxidizing tower, 2. tail gas neutralisation treatment device, 3. nitrogen dioxide feed pipe, 4. oxygen feed pipe; 5. nitrogen feed pipe, 6. smart thioether feed pipe, material feed rate meter, 8. material control valve, 9. oxidation cat head pressure tap before 7. transforming; 10. liquid level gauge, 11. temperature control valve (TCV)s, 12. magnetic valves, 13. thick sulfoxide storage tanks, 14. nitrogen oxide condensers; 15. the nitrogen oxide drainer, 16. accurate flowmeters, 17. cut off ball valve, 18. flow control valves; 19. long-range point for measuring temperature, 20. long-range liquid levels show point, 21. tail gas atmospheric valves, 22. neutralization ponds; A. gas phase zone, b. uptake zone, the surplus reaction zone of c., d. side reaction district, e. main reaction region, the f. thermal treatment zone.
The specific embodiment
Further specify the utility model below in conjunction with the specific embodiment.
A kind of safety in production device of dimethyl sulfide oxidation reaction; Comprise nitrogen dioxide feed pipe 3, oxygen feed pipe 4, nitrogen feed pipe 5, smart thioether feed pipe 6, oxidizing tower 1; Be respectively equipped with accurate flowmeter 16, material control valve 8 on nitrogen dioxide feed pipe 3, oxygen feed pipe 4, the smart thioether feed pipe 6 and cut off ball valve 17; Tail gas atmospheric valve 21 is arranged at oxidizing tower 1 top; Be provided with the checkout gear of measuring temperature, pressure in the oxidizing tower 1, checkout gear, cut-out ball valve 17, tail gas atmospheric valve 21 connect PLC interlock protection systems, and the tail gas of oxidizing tower 1 is connected into tail gas neutralisation treatment device 2.
Essence thioether feed pipe 6, nitrogen dioxide feed pipe 3 put in and partly are connected with distributor in the oxidizing tower; The distributor of smart thioether feed pipe 6 is that sleeve-like straight arm type distributor and open surface make progress, and the distributor of nitrogen dioxide feed pipe is that sleeve-like straight arm type distributor and open surface are downward.Accurate flowmeter 16 is provided with a plurality of on every feed pipe.17 for cutting off ball valve.
Nitrogen dioxide feed pipe 3 is provided with the nitrogen dioxide vapour liquid separator, and nitrogen dioxide vapour liquid separator both sides are respectively equipped with a nitrogen dioxide stop valve.The nitrogen dioxide stop valve connects PLC interlock protection system.Also be provided with magnetic valve on the nitrogen feed pipe 5.
A plurality of long-range points for measuring temperature 19 are set in the oxidizing tower, and the temperature of test shows that in monitoring system the control room operating personnel are very favourable to state of temperature and the variation tendency of holding whole oxidizing tower.
Nitrogen oxide tail gas on the equipment such as oxidizing tower, stripping tower, neutralizing tank, nitrogen oxide surge tank, thick sulfoxide storage tank 13, neutral sulfoxide groove, neutral sulfoxide head tank is all separated and introduces the absorption tower separately; Avoid pipeline to connect each other; Prevent that material from mixing, gathering, and tries to avert accidents in exhaust pipe.
The tail gas of two sulfide oxidation towers gets into absorption tower separately, and thick sulfoxide gas is carried tail gas and got into the absorption tower separately, and the tail gas that produces with part in the thick sulfoxide gets into the absorption tower separately.
A kind of safety in production technology of dimethyl sulfide oxidation reaction with nitrogen dioxide, oxygen, the strict control of smart thioether consumption, is pressed thioether feed rate 300kg/h, oxygen feed flow 60Nm
3/ h, nitrogen dioxide feed rate 15Nm
3Nitrogen dioxide is thrown in/h charging earlier, throws oxygen again, throws smart thioether at last again, each tower joint temperature of control oxidizing tower; The thermal treatment zone is 40～50 ℃ at the bottom of the tower, 60～75 ℃ of main reaction region, 55～65 ℃ in side reaction district; 40～60 ℃ of surplus reaction zones, 25～35 ℃ of uptake zones, 20～30 ℃ of gas phase zone; The tail gas that oxidation reaction is produced carries out the processing of water neutralization reaction.
Oxygen entrance pressure 0.3MPa, nitrogen dioxide entrance pressure 0.3MPa, oxidizing tower internal pressure≤3KPa.The oxidizing tower liquid level is 50%.The oxidizing tower liquid color is yellow～light green color, and the oxidized tail gas color is yellow.Thick sulfoxide acid number is 40～60mg (KOH)/g.
Embodiment 2
A kind of safety in production technology of dimethyl sulfide oxidation reaction with nitrogen dioxide, oxygen, the strict control of smart thioether consumption, is pressed thioether feed rate 400kg/h, oxygen feed flow 80Nm
3/ h, nitrogen dioxide feed rate 30Nm
3Nitrogen dioxide is thrown in/h charging earlier, throws oxygen again, throws smart thioether at last again, each tower joint temperature of control oxidizing tower; The thermal treatment zone is 40～50 ℃ at the bottom of the tower, 60～75 ℃ of main reaction region, 55～65 ℃ in side reaction district; 40～60 ℃ of surplus reaction zones, 25～35 ℃ of uptake zones, 20～30 ℃ of gas phase zone; The tail gas that oxidation reaction is produced carries out the processing of water neutralization reaction.
Oxygen entrance pressure 0.3MPa, nitrogen dioxide entrance pressure 0.3MPa, oxidizing tower internal pressure≤3KPa.The oxidizing tower liquid level is 60%.The oxidizing tower liquid color is yellow～light green color, and the oxidized tail gas color is yellow.Thick sulfoxide acid number is 40～60mg (KOH)/g.
As stated, the embodiment of the utility model has been carried out explanation at length, but as long as break away from the utility model point and the effect of the utility model in fact a lot of distortion can not arranged, this will be readily apparent to persons skilled in the art.Therefore, such variation also all is included within the protection domain of the utility model.
Claims (6)
1. the safety in production device of a dimethyl sulfide oxidation reaction; Comprise nitrogen dioxide feed pipe, oxygen feed pipe, nitrogen feed pipe, smart thioether feed pipe, oxidizing tower; It is characterized in that; Be respectively equipped with accurate flowmeter, material control valve and stop valve on nitrogen dioxide feed pipe, oxygen feed pipe, the smart thioether feed pipe, the tail gas atmospheric valve is arranged at the oxidizing tower top, is provided with the checkout gear of measuring temperature, pressure in the oxidizing tower; Checkout gear, stop valve, tail gas atmospheric valve connect PLC interlock protection system, and the tail gas of oxidizing tower is connected into the neutralisation treatment device.
2. the safety in production device of dimethyl sulfide oxidation reaction according to claim 1; It is characterized in that; Described smart thioether feed pipe, nitrogen dioxide feed pipe put in and partly are connected with distributor in the oxidizing tower; The distributor of smart thioether feed pipe is that sleeve-like straight arm type distributor and open surface make progress, and the distributor of nitrogen dioxide feed pipe is that sleeve-like straight arm type distributor and open surface are downward.
3. the safety in production device of dimethyl sulfide oxidation reaction according to claim 1 is characterized in that, described accurate flowmeter is provided with a plurality of on every feed pipe.
4. the safety in production device of dimethyl sulfide oxidation reaction according to claim 1 is characterized in that, described stop valve is for cutting off ball valve.
5. the safety in production device of dimethyl sulfide oxidation reaction according to claim 1 is characterized in that, described nitrogen dioxide feed pipe is provided with the nitrogen dioxide vapour liquid separator, and nitrogen dioxide vapour liquid separator both sides are respectively equipped with a nitrogen dioxide stop valve.
6. the safety in production device of dimethyl sulfide oxidation reaction according to claim 1 is characterized in that, described oxidizing tower is looked handleless cup at cat head liquid level gauge, tower bottom flow amount meter and cat head tail gas camera has been installed respectively, and camera connects monitoring system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200546873U CN202490608U (en) | 2012-02-20 | 2012-02-20 | Safety production device of dimethyl sulfide oxidizing reaction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012200546873U CN202490608U (en) | 2012-02-20 | 2012-02-20 | Safety production device of dimethyl sulfide oxidizing reaction |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN202490608U true CN202490608U (en) | 2012-10-17 |
Family
ID=46996852
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012200546873U Withdrawn - After Issue CN202490608U (en) | 2012-02-20 | 2012-02-20 | Safety production device of dimethyl sulfide oxidizing reaction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN202490608U (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527300A (en) * | 2012-02-20 | 2012-07-04 | 兖矿鲁南化肥厂 | Safety production device and process for dimethyl sulfide oxidation reaction |
| CN104275132A (en) * | 2014-10-21 | 2015-01-14 | 武汉江汉化工设计有限公司 | Thioether oxidation tower for producing dimethyl sulfoxide |
-
2012
- 2012-02-20 CN CN2012200546873U patent/CN202490608U/en not_active Withdrawn - After Issue
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102527300A (en) * | 2012-02-20 | 2012-07-04 | 兖矿鲁南化肥厂 | Safety production device and process for dimethyl sulfide oxidation reaction |
| CN104275132A (en) * | 2014-10-21 | 2015-01-14 | 武汉江汉化工设计有限公司 | Thioether oxidation tower for producing dimethyl sulfoxide |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20121017 Effective date of abandoning: 20141224 |
|
| RGAV | Abandon patent right to avoid regrant |