CN101412502A - Method for using gas unidirectional conveying apparatus in thionyl chloride cycle production process - Google Patents
Method for using gas unidirectional conveying apparatus in thionyl chloride cycle production process Download PDFInfo
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- CN101412502A CN101412502A CNA2008100011994A CN200810001199A CN101412502A CN 101412502 A CN101412502 A CN 101412502A CN A2008100011994 A CNA2008100011994 A CN A2008100011994A CN 200810001199 A CN200810001199 A CN 200810001199A CN 101412502 A CN101412502 A CN 101412502A
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Abstract
The invention relates to a method for applying a one-way gas conveying device in a thionyl chloride circulating production process, in particular to a method which comprises the following steps: the one-way gas conveying device is arranged at a gas outlet of a condenser of crude thionyl chloride product; and simultaneously two gas flows are merged and sent into a thionyl chloride synthesis kettle for reutilization through the method of regulating the heating temperature of a crude product deaeration purification kettle for convenience in regulating the pressure at the outlet, thereby forming the totally closed circulating production process thionyl chloride. The process can reduce raw material consumption and make the whole device basically emit no waste liquid or gas. Moreover, the method brings about an enlarged production scale and easy production.
Description
Invention field
What the present invention relates to is the application method of a kind of gas unidirectional conveying apparatus in thionyl chloride cycle production process, concretely, what the present invention relates to is that a kind of gas discharge outlet at the sulfur oxychloride condenser is provided with a gas unidirectional conveying apparatus, Heating temperature by regulating crude product degassing purification still is so that regulate the mode of its top hole pressure simultaneously, and two strands of gases are merged the method that the sulfur oxychloride synthesis reactor utilizes again of sending into, thereby form the totally-enclosed cyclic production process of sulfur oxychloride.
Background technology
The synthetic method of sulfur oxychloride has tens kinds, and still, large-scale industrial production is following three kinds of operational paths basically:
(1) phosphorus pentachloride and sulfurous gas reaction, technology is simple, but SOCl
2With POCl
3Be difficult to separate, be difficult to obtain high purity SOCl
2
(2) be catalyzer with antimony chloride etc., sulfur subchloride and chlorsulfonic acid reaction, domestic extensive employing at present, complex process is invested bigger;
(3) the synthesizing chlorinated sulfoxide of gas-phase catalysis is a catalyzer with the gac, sulfur subchloride and sulfurous gas, chlorine reaction, abroad generally adopt, technology is simple, less investment and product purity height, can adopt closed internal circulation apparatus production, non-environmental-pollution, the primitive reaction formula is as follows:
As typical case's representative of above-mentioned prior art (3), US2431823 discloses and has utilized disulphur dichloride (S
2Cl
2) and chlorine reaction, the sulfur dichloride (SCl of generation
2) and excessive chlorine and chlorine gas-phase reaction under activated carbon catalysis of sulfurous gas and importing, obtain sulfur oxychloride through distillation; The document also discloses that will reaction after the being mainly sulfur monochloride mixture that comprises sulphur after over cure bed and the distillation adds preheater A after through the chlorinator chlorination, begin new reaction.
But, in the document of the disclosure, utilize fan to be transported to the sulfur oxychloride synthesis reactor after the gas merging from condenser and de-gassing vessel, this mode is brought a lot of problems, for example, the set-up mode of the document may be under the pressure surge of synthesis reactor, cause to enter synthesis reactor from the gas of condenser and de-gassing vessel, perhaps cause the pressure surge of de-gassing vessel or condenser, though in another patent application of researchist of the present invention, proposed one return line to be set, but still may cause quantity-produced to be difficult to carry out in the front and back of fan.
In view of this, special proposition the present invention.
Summary of the invention
The object of the present invention is to provide a kind of gas discharge outlet that one gas unidirectional conveying apparatus is set at sulfur oxychloride crude product condenser, Heating temperature by regulating crude product degassing purification still is so that regulate the mode of its top hole pressure simultaneously, and two strands of gases are merged the method that the sulfur oxychloride synthesis reactor utilizes again of sending into, thereby form the totally-enclosed cyclic production process of sulfur oxychloride.
Purpose of the present invention can be achieved in the following manner:
Describe bright technical scheme of the present invention for clear, below the building-up process of sulfur oxychloride is described below, that is:
1, synthetic sulfur monochloride (S
2Cl
2);
2, synthetic sulfur dichloride (SCl
2);
3, synthesizing chlorinated sulfoxide (SOCl
2);
4, sulfur oxychloride rectifying.
In the sulfur oxychloride synthetic process, but there is several means can produce reuse gas, the one, the crude product sulfur oxychloride is after condensing works cooling, and the lower boiling gas of part can reuse; The 2nd, crude product degassing purification still, in order further to improve the content of sulfur oxychloride, in crude product degassing purification still, with the lower boiling unreacted of a part completely material deviate from, this part gas also can be got back to reuse in the sulfur oxychloride synthesis reactor; Certainly, device such as similar rectifying tower also has the portion gas can reuse.
If these mixed gass are emitted, just may waste and pollute, more importantly be, what the present invention relates to is the totally-enclosed recycle to extinction production technique of a kind of sulfur oxychloride, in order almost completely there not to be the emptying of unnecessary waste material in feasible the production, promptly no longer enter production cycle, the reuse amount that needs conscious increase liquid or gas, therefore, the reuse of gas and in reuse, how to keep sulfur oxychloride synthesis reactor, crude product condenser and interference that the pressure of crude product degassing purification still is not subjected to mutually each other becomes an important problem.
The solution that the present invention proposes is that the gas discharge outlet at sulfur oxychloride crude product condenser is provided with a gas unidirectional conveying apparatus, concrete, be that gas discharge outlet at sulfur oxychloride crude product condenser is provided with a pneumatic diaphragm pump, Heating temperature by regulating crude product degassing purification still is so that regulate the mode of its top hole pressure simultaneously, and two strands of gases are merged send into the method that the sulfur oxychloride synthesis reactor utilizes again, thereby form the totally-enclosed cyclic production process of sulfur oxychloride of the present invention.
Specifically, the invention provides the application method of a kind of gas unidirectional conveying apparatus in thionyl chloride cycle production process, the cycle production process of described sulfur oxychloride comprises the synthetic of sulfur oxychloride, condensation, the degassing and rectifying, the device of described thionyl chloride cycle production process comprises the sulfur dichloride synthesis reactor, the sulfur oxychloride synthesis reactor, the crude product condenser, crude product degassing purification still, the crude product sulfur still, the rectifying condenser, rectifying tower and tower still, characteristics of the present invention are that the gas discharge outlet at the crude product condenser is provided with a gas unidirectional conveying apparatus, and the gas discharge outlet of the outlet of described gas unidirectional conveying apparatus by pipeline and crude product degassing purification still merges and lead to corresponding opening for feed at the bottom of the sulfur oxychloride synthesis reactor still.
Among the present invention, described gas unidirectional conveying apparatus is a surge pump, preferred pneumatic diaphragm pump or electric diaphragm pump, more preferably pneumatic diaphragm pump.
Wherein, described pneumatic diaphragm pump is unidirectional delivering gas.Among the present invention, in order to keep the circulation of gas in whole process of production, gas from the crude product condenser has formed unidirectional delivering gas owing to gas unidirectional conveying apparatus, therefore, the top hole pressure of only regulating crude product degassing purification still and corresponding inlet pressure at the bottom of the sulfur oxychloride synthesis reactor still promptly can be kept the pressure dependence between the synthesizing of sulfur oxychloride, condensation and the de-gassing vessel.The variation of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still is that the Heating temperature of regulating crude product degassing purification still forms.
Further, in order to finish circulation, top hole pressure P1 and the sulfurous gas pressure P 2 of injecting sulfur oxychloride synthesis reactor of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still at the bottom of more than or equal to sulfur dichloride synthesis reactor still.Among the present invention, the pressure P 5 of the gas discharge outlet of crude product degassing purification still should also be greater than or equal the pressure P 2 of sulfurous gas injection sulfur oxychloride synthesis reactor post chlorization sulfoxide synthesis reactor more than or equal to the top hole pressure P1 at the bottom of the sulfur dichloride synthesis reactor still.Like this, could make the lower boiling unreacted from crude product degassing purification still, deviate from completely gas circulation enter into the sulfur oxychloride synthesis reactor and utilize once more.
Described pneumatic diaphragm pump is then brought up to the gaseous tension P3 in the crude product condenser top hole pressure P4 of crude product condenser, thus like this can so that the lower boiling gas of part that the crude product sulfur oxychloride comes out after through the cooling of crude product condenser can with from the lower boiling unreacted of deviating from the crude product degassing purification still completely gas merge and enter the sulfur oxychloride synthesis reactor.
For the consumption that reduces the energy that pump brings in course of conveying and possible leakage, the present invention also is arranged on the position of the liquid phase discharge gate of crude product condenser the place of the liquid phase feeding mouth that is higher than crude product degassing purification still, make liquid can not have pump delivery so that form pressure difference, simultaneously, between the liquid phase feeding mouth of the liquid phase discharge gate of crude product condenser and the crude product degassing purification still U-shaped pipe is set, thereby forms fluid-tight.
Method of the present invention can prevent the pressure surge between crude product degassing purification still, crude product condenser and the sulfur oxychloride synthesis reactor effectively.
The present invention compared with prior art has following advantage:
1, adopt the application method of a kind of gas unidirectional conveying apparatus of the present invention in thionyl chloride cycle production process, raw-material consumption reduces, raw-material relatively feeding intake, and the yield height, utilization rate of raw materials is up to more than 99.0%; Under processing condition of the present invention, carry out suitable control, sulphur and chlorine (seeing topmost reactant) from the angle of economy to the transformation efficiency of sulfur oxychloride near 100%;
2, adopt the totally-enclosed technology of recycle to extinction, break away from the SO in the gas
2And Cl
2Liquid product beyond the sulfur oxychloride that mixed gas and each operation produce can be recycled to corresponding charging place, makes the essentially no three waste liquid gas of complete assembly outwards discharge;
3, adopt the application method of a kind of gas unidirectional conveying apparatus of the present invention in thionyl chloride cycle production process, can be so that industrial scale enlarge, and carry out easily.
Description of drawings
Accompanying drawing 1 is the preparation technology's of a sulfur oxychloride of the present invention basic flow sheet;
Accompanying drawing 2 is that the high potential difference that utilizes of the present invention makes the synoptic diagram of gas phase crude product sulfur oxychloride from low-pressure delivery to the highly compressed method.
For the present invention clearly is described, special numbering with component names in the accompanying drawing and correspondence is listed sulfur dichloride synthesis reactor 1, sulfur oxychloride synthesis reactor 2, crude product condenser 3, crude product degassing purification still 4, crude product sulfur still 5, rectifying condenser 6, rectifying tower 7, tower still 8, sulfur monochloride transferpump 9, crude product discharge port 10, U-shaped pipe 11, unidirectional conveying apparatus 12.
Embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with accompanying drawing, described embodiment is in order to further describe the present invention, rather than restriction the present invention.
Embodiment 1
Different with prior art, the sulfur monochloride (S among the present invention
2Cl
2), can use conventional methods and produce a certain amount of at the production initial stage, also can directly purchase sulfur monochloride, perhaps the crude product that contains chlorination sulfoxide about 70% with sulfur dichloride, chlorine, sulfurous gas method synthetic gets final product, can reach the demand of sulfur monochloride and the running balance of turnout aborning later on, promptly sulfur monochloride is from the rectifying tower still.
Concrete, the gas that comes from the bottom of sulfur oxychloride synthesis reactor 2 stills is conducted through a water-cooled crude product condenser 3, at described water-cooled crude product condenser 3 condensing coil or similar condensation facility are set, cooling by water, make high boiling material obtain cooling, thereby the liquid state of changing into enters a separator(-ter) or crude product degassing purification still 4, SO herein from the liquid phase discharge port of crude product condenser 3
2And Cl
2Broken away from as gas, on described water-cooled crude product condenser 3, a gas discharge outlet is set, a gas unidirectional conveying apparatus 12 is set on discharge outlet.
Gas unidirectional conveying apparatus 12 of the present invention, it can be electric diaphragm pump, it also can be pneumatic diaphragm pump, preferred in the present invention pneumatic diaphragm pump, it is propulsion source that pneumatic diaphragm pump of the present invention adopts pressurized air, for the gas that the present invention relates to high anticorrosive barrier film is set preferably, comprises nitrile rubber, viton, chloroprene rubber and tetrafluoroethylene etc. with severe corrosive.
For control aborning easily, simultaneously, in order to increase or reduces production capacity, adopting more than one pneumatic diaphragm pump is preferably, its flow be the aggregate demand flow divided by surge pump quantity, stepless adjustable being more preferably.
The gas discharge outlet of above-mentioned pneumatic diaphragm pump outlet by pipeline and crude product degassing purification still 4 merges and leads to corresponding opening for feed at the bottom of sulfur oxychloride synthesis reactor 2 stills.The gas that comes out from the gas discharge outlet of crude product condenser 3 is transported to the pipeline by pneumatic diaphragm pump and merges with the gas of deviating from from crude product degassing purification still 4, and corresponding opening for feed enters into sulfur oxychloride synthesis reactor 2 at the bottom of sulfur oxychloride synthesis reactor 2 stills.
The sulfur oxychloride synthetic gas is after 3 condensations of crude product condenser, and the crude product phlegma enters crude product degassing purification still 4 operation that outgases by high potential difference, and the crude product after the degassing finishes is made the raw material of rectification working process.
(major ingredient is SO to not the coagulating property gas that the degassing is come out
2And Cl
2, SCl
2) behind degassing separator, circulation gas basin, be transported to circulation gas surge tank (the about 0.12Mpa of pressure), turn back to gas mixer then and use, thereby finish the gas phase circulation for building-up reactions.
Crude product degassing purification still 4 is deviate from gas, at 50-90 ℃ of temperature, pressure is under the 0.12Mpa condition, with the control of purity of sulfur oxychloride crude product between 40-70%, so that enough raw materials are arranged, comprise the gas that condensation is got rid of, the gas that crude product degassing purification still 4 is deviate from, with and subsequent the crude product sulfur oxychloride add sulphur and make unreacted reactant change into sulfur monochloride, participate in circulation once more, too low unreacted reactant content, cause the sulfur monochloride deficiency, circulation can't be carried out continuously, and unduly high unreacted reactant will cause the sulfur monochloride surplus and cause the obvious decline of output.
If pressure surge can be regulated amount of gas evolved, thereby regulate the pressure of its outlet by regulating the temperature of de-gassing vessel.
Be recycled to corresponding gas feed place at the bottom of sulfur oxychloride synthesis reactor 2 stills from the mixed gas of crude product condenser 3 and crude product degassing purification still 4.
Referring to accompanying drawing 1, at the gas discharge outlet of crude product condenser 3 pneumatic diaphragm pump 12 is set, the gas discharge outlet of the outlet of described pneumatic diaphragm pump 12 by pipeline and crude product degassing purification still 4 merges and leads to corresponding opening for feed at the bottom of sulfur oxychloride synthesis reactor 2 stills.
The position of the liquid phase discharge gate of crude product condenser 3 is arranged on the place of the liquid phase feeding mouth that is higher than crude product degassing purification still 4, simultaneously, between the liquid phase feeding mouth of the liquid phase discharge gate of crude product condenser 3 and crude product degassing purification still 4 a U-shaped pipe 11 is set, referring to accompanying drawing 2.
Among the present invention, the gas that comes from the bottom of sulfur oxychloride synthesis reactor 2 stills is conducted through a water-cooled crude product condenser 3, at described water-cooled crude product condenser 3 condensing coil or similar condensation facility are set, cooling by water, make high boiling material obtain cooling, thereby the liquid state of changing into enters a separator(-ter) or crude product degassing purification still 4, SO herein from the liquid phase discharge port of crude product condenser 3
2And Cl
2Broken away from as gas,
Above-mentioned come from gas at the bottom of sulfur oxychloride synthesis reactor 2 stills through 3 coolings of water-cooled crude product condenser after, the lower boiling gas of part is transported to the SO that deviates from above-mentioned crude product degassing purification still 4 in the pipeline by pneumatic diaphragm pump 12
2And Cl
2Merge, and corresponding opening for feed enters into sulfur oxychloride synthesis reactor 2 recycle once more at the bottom of sulfur oxychloride synthesis reactor 2 stills.
Wherein, described pneumatic diaphragm pump 12 is unidirectional delivering gas.Among the present invention, in order to keep the circulation of gas in whole process of production, gas from crude product condenser 3 has formed unidirectional delivering gas owing to gas unidirectional conveying apparatus, therefore, the top hole pressure of only regulating crude product degassing purification still 4 and corresponding inlet pressure at the bottom of sulfur oxychloride synthesis reactor 2 stills promptly can be kept the pressure dependence between the synthesizing of sulfur oxychloride, condensation and the de-gassing vessel.The variation of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still is that the Heating temperature of regulating crude product degassing purification still forms.
Further, in order to finish circulation, the top hole pressure P1 of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still 4 at the bottom of greater than sulfur dichloride synthesis reactor 2 stills injects the pressure P 2 of sulfur oxychloride synthesis reactor simultaneously greater than sulfurous gas.
Described pneumatic diaphragm pump 12 is then brought up to the gaseous tension P3 in the crude product condenser 3 the top hole pressure P4 of crude product condenser 3, thereby thereby enables to enter sulfur oxychloride synthesis reactor 2 with the gas merging of the purification still 4 that outgases from crude product.
The position of the liquid phase discharge gate of crude product condenser 3 of the present invention is arranged on the place of the liquid phase feeding mouth that is higher than crude product degassing purification still 4, make liquid can not have pump delivery so that form pressure difference, and can reduce the consumption of the energy that brings in the pump delivery process and possible leakage, simultaneously, between the liquid phase feeding mouth of the liquid phase discharge gate of crude product condenser 3 and crude product degassing purification still 4, a U-shaped pipe 11 is set, thereby forms fluid-tight.
Other is identical with embodiment 1, and different is that other end reaction gas exhaust mouth in the totally-enclosed continuous synthesis technique of sulfur oxychloride of the present invention can't all be provided with the gas diaphragm pump by the self-gas discharge outlet of adjusting pressure.
Claims (10)
1, the application method of a kind of gas unidirectional conveying apparatus in thionyl chloride cycle production process, described thionyl chloride cycle production process comprises the synthetic of sulfur oxychloride, condensation, the degassing and rectifying, the device of described thionyl chloride cycle production process comprises the sulfur dichloride synthesis reactor, the sulfur oxychloride synthesis reactor, the crude product condenser, crude product degassing purification still, the crude product sulfur still, the rectifying condenser, rectifying tower and tower still, it is characterized in that: the gas discharge outlet at described crude product condenser is provided with a gas unidirectional conveying apparatus, and the gas discharge outlet of the outlet of described gas unidirectional conveying apparatus by pipeline and crude product degassing purification still merges and lead to corresponding opening for feed at the bottom of the sulfur oxychloride synthesis reactor still.
2, application method according to claim 1 is characterized in that: described gas unidirectional conveying apparatus is a surge pump.
3, application method according to claim 2 is characterized in that: described gas unidirectional conveying apparatus is pneumatic diaphragm pump or electric diaphragm pump.
4, according to claim 1 or 2 or 3 described application methodes, it is characterized in that: described gas unidirectional conveying apparatus is a pneumatic diaphragm pump.
5, application method according to claim 4 is characterized in that: described pneumatic diaphragm pump is unidirectional delivering gas.
6, application method according to claim 1 and 2 is characterized in that: top hole pressure P1 and the sulfurous gas pressure P 2 of injecting sulfur oxychloride synthesis reactor of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still at the bottom of more than or equal to sulfur dichloride synthesis reactor still.
7, application method according to claim 1 is characterized in that: described pneumatic diaphragm pump is brought up to the gaseous tension P3 in the crude product condenser top hole pressure P4 of crude product condenser.
8, application method according to claim 2 is characterized in that: the variation of the pressure P 5 of the gas discharge outlet of described crude product degassing purification still is that the Heating temperature of regulating crude product degassing purification still forms.
9, application method according to claim 1 is characterized in that: the position of the liquid phase discharge gate of described crude product condenser is higher than the liquid phase feeding mouth of crude product degassing purification still.
10, application method according to claim 9 is characterized in that: between the liquid phase feeding mouth of the liquid phase discharge gate of described crude product condenser and the crude product degassing purification still U-shaped pipe is set.
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|---|---|---|---|
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|---|---|---|---|
| CN2008100011994A CN101412502B (en) | 2008-01-18 | 2008-01-18 | Method for using gas unidirectional conveying apparatus in thionyl chloride cycle production process |
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| CN101412502B CN101412502B (en) | 2010-12-01 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043620A (en) * | 2012-12-31 | 2013-04-17 | 山东凯盛新材料股份有限公司 | Method for recycling tail gas during thionyl chloride preparation |
| CN107930366A (en) * | 2017-11-30 | 2018-04-20 | 山东凯盛新材料股份有限公司 | The technique that thionyl chloride integrates treating tail gas |
| CN107998857A (en) * | 2017-11-30 | 2018-05-08 | 山东凯盛新材料股份有限公司 | The technique of the thionyl chloride tail gas comprehensive regulation |
| CN109399577A (en) * | 2018-11-27 | 2019-03-01 | 江西世龙实业股份有限公司 | A kind of method and apparatus refining thionyl chloride |
| CN109485019A (en) * | 2018-11-27 | 2019-03-19 | 江西世龙实业股份有限公司 | A kind of thionyl chloride production gas phase circulator and method |
| CN111453704A (en) * | 2019-01-18 | 2020-07-28 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
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2008
- 2008-01-18 CN CN2008100011994A patent/CN101412502B/en active Active
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103043620A (en) * | 2012-12-31 | 2013-04-17 | 山东凯盛新材料股份有限公司 | Method for recycling tail gas during thionyl chloride preparation |
| CN107930366A (en) * | 2017-11-30 | 2018-04-20 | 山东凯盛新材料股份有限公司 | The technique that thionyl chloride integrates treating tail gas |
| CN107998857A (en) * | 2017-11-30 | 2018-05-08 | 山东凯盛新材料股份有限公司 | The technique of the thionyl chloride tail gas comprehensive regulation |
| CN109399577A (en) * | 2018-11-27 | 2019-03-01 | 江西世龙实业股份有限公司 | A kind of method and apparatus refining thionyl chloride |
| CN109485019A (en) * | 2018-11-27 | 2019-03-19 | 江西世龙实业股份有限公司 | A kind of thionyl chloride production gas phase circulator and method |
| CN109399577B (en) * | 2018-11-27 | 2020-10-09 | 江西世龙实业股份有限公司 | Method for refining thionyl chloride |
| CN111453704A (en) * | 2019-01-18 | 2020-07-28 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
| CN111453704B (en) * | 2019-01-18 | 2021-11-23 | 江西世龙实业股份有限公司 | Device and method for recycling tail gas generated in thionyl chloride production |
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|---|---|
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