CN102949976A - Sulfur chlorinated isobutylene production equipment and method - Google Patents
Sulfur chlorinated isobutylene production equipment and method Download PDFInfo
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- CN102949976A CN102949976A CN2012104462176A CN201210446217A CN102949976A CN 102949976 A CN102949976 A CN 102949976A CN 2012104462176 A CN2012104462176 A CN 2012104462176A CN 201210446217 A CN201210446217 A CN 201210446217A CN 102949976 A CN102949976 A CN 102949976A
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Abstract
The invention provides sulfur chlorinated isobutylene production equipment, comprising an enamel gas liquid reaction kettle and a falling film absorption tower. According to the technical main points, the enamel gas liquid reaction kettle comprises an upper sealing head, a kettle body and a stirring shaft; a stirring blade is arranged on the stirring shaft; a jacket is arranged outside the kettle body; a cooling liquid inlet and a liquid outlet are arranged on the jacket; the upper sealing head is connected with the kettle body together; a feeding opening and an air exhaust opening are arranged at the upper part of the kettle body; the air exhaust opening is communicated with the falling film absorption tower; a discharging opening is arranged at the center of the bottom of the kettle body; an air inlet pipe is arranged at the bottom of the kettle body; and three to five air inlet pipes are uniformly and coaxially distributed on the rim of the discharging opening. The sulfur chlorinated isobutylene production equipment provided by the invention has the advantages that single sulfur chloride and isobutylene can be subjected to multipoint reaction, so that the reaction process tends to be stable, the reaction temperature is easy to control, side product amount can be reduced, the reaction time is shortened, the yield can be improved, and the production cost can be reduced; the isobutylene has sufficient reaction time, so that the raw materials can be prevented from being wasted; and the defects that the enamel has low toughness, is easy to break and the like can be overcome without arranging an individual air exhaust annular pipe, so that the occurrence of the safe accident can be avoided.
Description
Technical field
The present invention relates to a kind of gas liquid reaction still, relating in particular to a kind of autoclave body bottom is the gas liquid reaction still of loose structure, and it is mainly used in the consersion unit of sulfur monochloride and isobutene under the normal temperature.
Background technology
Sulfide isobutene (T321) is a kind of sulfur-containing additive single dose, and it is widely used in the main extreme pressure anti-wear additives of the high-grade gear oil of modulation, antiwear hydraulic oil, cutting oil, lubricating grease and industry oil.Its production technology is mainly carried out through addition reaction and sulfurizing dechlorination reaction take isobutene, sulfur monochloride and alkali metal or alkaline earth sulfide as raw material in the world wide.
Generate byproduct hydrogen chloride, hydrogen sulfide in the reaction.Wherein, be light yellow oily liquid under sulfur monochloride (having another name called disulphur dichloride, the single sulfur chloride) normal temperature and pressure, and have the specific stimulation smell; It easily is fuming in air, and mucous membrane is had extremely strong excitant; Stable under the room temperature, easily be decomposed into corresponding simple substance during 100 ° of C, then decompose fully during 300 ° of C; Can be chloride and sulfide by metallic reducing; Generate sulfur dichloride with chlorine reaction.Can generate metal chloride with metal oxide or sulfide reaction.For gas, it has many adverse effects such as teratogenesis, carcinogenic, mutagenesis to human body under isobutene (the having another name called the 2-metering system) normal temperature and pressure.In sum, the gas liquid reaction of sulfur monochloride and isobutene must be carried out under the closed environment, and avoids using hardware, prevents the chlorination corrosion of sulfur monochloride.
In many chemical products are produced, gaseous phase materials and liquid phase material carry out in the gas liquid reaction still, with reference to a kind of gas liquid reaction still described in the patent CN2635202 shown in Figure 4, comprise upper cover, kettle, upper cover and kettle are fixed together, be provided with agitator in the kettle, kettle is outer with chuck.Liquid phase material is entered by the upper cover top, and gaseous phase materials enters the ring-type gas port by the gas distributor that arranges in the kettle, then with kettle in liquid phase feed reaction.
Although the Multipoint synchronous of above-mentioned patent energy high efficiency smooth carries out most gas liquid reaction, but it is obviously undesirable that it is applied in the production of sulfide isobutene, the reasons are as follows: 1. use enamel instead as the consersion unit material, because the low toughness of enamel self, the characteristics such as frangible, only by the single-point fixed form of air inlet and kettle, under the strong effect that stirs eddy current, very easily break away from kettle and cause security incident; 2. because reaction kettle body must adopt hermetically-sealed construction, can cause being difficult to sealing if set up the gas distributor reinforced liner at kettle; 3. existing gas liquid reaction still draw ratio is difficult to meet the process conditions of sulfide isobutene, cause isobutene fully to react in the cavity that just has been discharged into kettle top with sulfur monochloride, cause gas to be detained in a large number, pressure is increased be difficult for reaction pressure, and affected reaction efficiency and wasted large content of starting materials; 4. sulfur monochloride and isobutene reaction process are very violent, course of reaction is emitted large calorimetric, easily cause excess Temperature in the kettle if can not well control air inflow, reaction temperature is difficult to be effectively controlled, high temperature easily causes sulfur monochloride to decompose simultaneously, amount of by-products increases, and has reduced yield, has improved production cost; 5. the air inflow of isobutene is difficult to be effectively controlled, and causes in the reaction solution local temperature too high, and accessory substance increases.
Summary of the invention
Be difficult to control for solving sulfur monochloride and isobutene reaction condition, the prior art consersion unit is difficult to the problems such as application, a kind of multiple spot reactor and a kind of production method of using the sulphur chlorination isobutene of this equipment of providing of the present invention.
The invention provides following technical scheme: a kind of sulphur chlorination isobutene production equipment, comprise enamel gas liquid reaction still and film-falling absorption tower, its technical essential is: described enamel gas liquid reaction still comprises upper cover, kettle, shaft, shaft is provided with paddle, kettle is provided with chuck outward, chuck is provided with cooling agent inlet and liquid outlet, upper cover and kettle link together, kettle top is provided with charging aperture, exhaust outlet, exhaust outlet is connected with film-falling absorption tower, the autoclave body bottom center is provided with discharging opening, and autoclave body bottom is provided with air inlet pipe, three to five air inlet pipe of coaxial even distribution around discharging opening; The kettle draw ratio is 2 ~ 3.5:1.
The volume of described kettle is 3000L.
A kind of production method of using the sulphur chlorination isobutene of above-mentioned consersion unit, its technical essential be, comprises the steps: to open cooling circulating water, and the sulfur monochloride of 2500L ~ 2800L is joined in the reactor, opens agitating device; Then pass into isobutene by air inlet pipe in reactor, intake is 10kg/h first, regulates total throughput between 10-90kg/h, keeps reactor internal reaction liquid slight boiling condition, increases gradually total throughput of air inlet pipe; After reacting completely, stop ventilation, close agitating device, open bleeder valve, by discharging opening sulphur chlorination isobutene solution is discharged.
Compared with prior art, beneficial effect of the present invention is as follows:
(1) loose structure is adopted in the reactor bottom, makes single sulfur chloride and isobutene carry out the multiple spot reaction, and course of reaction is tended to be steady, and reaction temperature is easy to control, and amount of by-products reduces, and has shortened the reaction time, has improved productive rate, has reduced production cost;
(2) adopt specific length-width ratio, make isobutene that the sufficient reaction time be arranged, avoid the waste of raw material;
(3) overcome the low toughness of enamel, the defective such as frangible, need not to arrange independent exhaust endless tube, avoided the generation of security incident.
Description of drawings
Fig. 1 is the structural representation of a kind of multiple spot reactor of the present invention.
Fig. 2 is that Fig. 1 is along A-A line profile.
Fig. 3 is consersion unit annexation schematic diagram of the present invention.
Fig. 4 is existing a kind of gas liquid reaction still cross-sectional view.
Main symbol description in the accompanying drawing: 1. air inlet pipe; 2. chuck inlet; 3. chuck; 4. charging aperture; 5. shaft; 6. exhaust outlet; 7. chuck liquid outlet; 8. paddle; 9. discharging opening; 10. gas liquid reaction still; 11. film-falling absorption tower; A. single sulfur chloride; B. isobutene; C. hydrogen sulfide gas.
The below will be described in further detail the present invention by drawings and Examples, but following example only is the present invention's example wherein, not represent the rights protection scope that the present invention limits, and the scope of the present invention is as the criterion with claims.
The specific embodiment
Embodiment 1
Referring to figs. 1 to Fig. 3, a kind of sulphur chlorination isobutene production equipment of the present invention, comprise enamel gas liquid reaction still 10 and film-falling absorption tower 11, described enamel gas liquid reaction still comprises upper cover, kettle, shaft 5, shaft 5 is provided with paddle 8, kettle is provided with chuck 3 outward, chuck 3 is provided with cooling agent inlet 2 and liquid outlet 7, upper cover and kettle link together, kettle top is provided with charging aperture 4, exhaust outlet 6, exhaust outlet 6 is connected with film-falling absorption tower 11, and the autoclave body bottom center is provided with discharging opening, autoclave body bottom is provided with air inlet pipe 1, three air inlet pipe 1 of coaxial even distribution around discharging opening 9; The kettle draw ratio is 2 ~ 3.5:1, and the volume of kettle is 3000L.
The using method of this production equipment is as follows:
Open cooling circulating water, the sulfur monochloride of 2500L is joined in the reactor, open agitating device; Then pass into isobutene by air inlet pipe 1 in reactor, intake is 10kg/h first, regulates total throughput between 10-90kg/h, keeps reactor internal reaction liquid slight boiling condition, increases gradually total throughput of air inlet pipe; After reacting completely, stop ventilation, close agitating device, open bleeder valve, by discharging opening sulphur chlorination isobutene solution is discharged, be transported in the dechlorination reaction still.
Claims (3)
1. sulphur chlorination isobutene production equipment, comprise enamel gas liquid reaction still and film-falling absorption tower, it is characterized in that: described enamel gas liquid reaction still comprises upper cover, kettle, shaft, shaft is provided with paddle, kettle is provided with chuck outward, chuck is provided with cooling agent inlet and liquid outlet, upper cover and kettle link together, kettle top is provided with charging aperture, exhaust outlet, exhaust outlet is connected with film-falling absorption tower, the autoclave body bottom center is provided with discharging opening, and autoclave body bottom is provided with air inlet pipe, three to five air inlet pipe of coaxial even distribution around discharging opening; The kettle draw ratio is 2 ~ 3.5:1.
2. production equipment according to claim 1, it is characterized in that: the volume of described kettle is 3000L.
3. a right to use requires the production method of the sulphur chlorination isobutene of 1 or 2 described consersion units, it is characterized in that, comprises the steps: to open cooling circulating water, and the sulfur monochloride of 2500L ~ 2800L is joined in the reactor, opens agitating device; Then pass into isobutene by air inlet pipe in reactor, intake is 10kg/h first, regulates total throughput between 10-90kg/h, keeps reactor internal reaction liquid slight boiling condition, increases gradually total throughput of air inlet pipe; After reacting completely, stop ventilation, close agitating device, open bleeder valve, by discharging opening sulphur chlorination isobutene solution is discharged.
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| CN2012104462176A CN102949976A (en) | 2012-11-09 | 2012-11-09 | Sulfur chlorinated isobutylene production equipment and method |
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| CN2012104462176A CN102949976A (en) | 2012-11-09 | 2012-11-09 | Sulfur chlorinated isobutylene production equipment and method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240048A (en) * | 2013-05-06 | 2013-08-14 | 南通金陵农化有限公司 | Chloromethane through pipe for alkylating pot |
| CN103467444A (en) * | 2013-08-31 | 2013-12-25 | 沈阳广达化工有限公司 | Method for increasing utilization ratio of isobutene in sulfurized isobutene production |
| CN103894133A (en) * | 2014-03-24 | 2014-07-02 | 苏州润弘贸易有限公司 | Reaction device for printing and dyeing chemical industry |
| CN104001466A (en) * | 2014-03-24 | 2014-08-27 | 苏州润弘贸易有限公司 | Temperature-controllable refining agent reaction kettle |
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| US4563302A (en) * | 1983-12-01 | 1986-01-07 | Edwin Cooper, Inc. | Sulfurized olefin process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240048A (en) * | 2013-05-06 | 2013-08-14 | 南通金陵农化有限公司 | Chloromethane through pipe for alkylating pot |
| CN103467444A (en) * | 2013-08-31 | 2013-12-25 | 沈阳广达化工有限公司 | Method for increasing utilization ratio of isobutene in sulfurized isobutene production |
| CN103894133A (en) * | 2014-03-24 | 2014-07-02 | 苏州润弘贸易有限公司 | Reaction device for printing and dyeing chemical industry |
| CN104001466A (en) * | 2014-03-24 | 2014-08-27 | 苏州润弘贸易有限公司 | Temperature-controllable refining agent reaction kettle |
| CN103894133B (en) * | 2014-03-24 | 2015-12-23 | 苏州润弘贸易有限公司 | A kind of printing and dyeing chemical industry reaction unit |
| CN104001466B (en) * | 2014-03-24 | 2015-12-23 | 苏州润弘贸易有限公司 | Can the scouring agent reactor of temperature control |
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Application publication date: 20130306 |