CN103043620A - Method for recycling tail gas during thionyl chloride preparation - Google Patents
Method for recycling tail gas during thionyl chloride preparation Download PDFInfo
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- CN103043620A CN103043620A CN2012105946203A CN201210594620A CN103043620A CN 103043620 A CN103043620 A CN 103043620A CN 2012105946203 A CN2012105946203 A CN 2012105946203A CN 201210594620 A CN201210594620 A CN 201210594620A CN 103043620 A CN103043620 A CN 103043620A
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Abstract
The invention relates to a method for recycling tail gas during thionyl chloride preparation, which belongs to the field of chemical engineering process. The method is that delivering the gas released during the transportation process of thionyl chloride crude product from a crude product vulcanizing tank to a crude product intermediate tank and the gas remained after the rectification and the condensation of the thionyl chloride to a thionyl chloride synthesis kettle for cyclic utilization by using a gas compression conveying machinery. The sulfur dioxide method thionyl chloride manufacturing technology forms a perfect gas phase closed cycle, which enables the yield of thionyl chloride to be above 99 percent, and saves a great amount of tail gas absorption alkali and eliminates environment pollution. The liquid ring type compressor has the advantages that the operation is simple and convenient, the construction cost is low, the maintenance quantity is small and no additional agent is used in the system.
Description
Technical field
The present invention relates to the method that tail gas recycle is utilized in a kind of sulfur oxychloride preparation, belong to the chemical technique field.
Background technology
Sulfur oxychloride is a kind of important organic synthesis chlorizating agent, such as the chlorine displacement of chlorination, organic sulfonic acid or the nitro-compound of the chlorination of the chlorination of alcohols hydroxyl, carboxylic acid, acid anhydrides.Make acyl chloride, can also be used for ring-closure reaction and beckmann rearrangement.(select from " inorganic chemicals industry handbook second edition, P601 compiles in Tianjin chemical research institute)
The synthetic method of the sulfur oxychloride of suitable suitability for industrialized production commonly used has three kinds:
⑴ sulphur trioxide method: the reaction of phosphorus pentachloride and sulphur trioxide, generate sulfur oxychloride and phosphorus oxychloride, this route technique is simple, but because sulfur oxychloride and phosphorus oxychloride separating difficulty are large, product is not easy to purify.
⑵ chlorosulfonic acid method: take antimony chloride etc. as catalyzer, make sulfur monochloride and chlorine, chlorsulfonic acid reaction, this method complex process, backward in technique, material consumption is large, and is seriously polluted.
⑶ sulfurous gas method: advanced operational path, chlorine, sulfur dichloride and sulfurous gas under the condition of activated carbon catalyst, the generation sulfur oxychloride that reacts, this technique is simple, less investment, product purity are high, at present this technique of domestic most employing.
There are three aspects in tail gas source in the standby sulfur oxychloride technique of sulfurous gas legal system:
⑴ from the gas of sulfur oxychloride synthesis reactor synthetic gas out after the crude product condenser condenses, and main component is completely sulfurous gas and chlorine of unreacted, also has simultaneously a small amount of sulfur dichloride and sulfur oxychloride.The recycling of this part tail gas is described in another patent of contriver.
⑵ the gas that the crude product after the sulfuration discharges from the crude product vulcanizing boiler toward crude product tundish feeding process, this part tail gas is mainly sulfurous gas, and a small amount of sulfur dichloride and sulfur oxychloride are arranged in addition.
⑶ sulfur oxychloride remaining tail gas after the rectifying condensation in the rectification and purification process, this part tail gas main component also is sulfurous gas, contains in addition a small amount of sulfur oxychloride.
Wang state waits clearly in the gas phase circulation method and application method two patents of CN101412502A gas unidirectional conveying apparatus in the sulfur oxychloride production technique of people in CN101284653A sulfur oxychloride is synthetic, has provided the temperature by the degassed purification still of adjusting crude product of dissolved gases in the sulfur oxychloride crude product so that its pressure that raises is sent the method for sulfur oxychloride synthesis reactor back to.Remove the method that is dissolved in the gas in the liquid two kinds of temperature-raising method and decompression methods are arranged, and thereby the degas method that this dependence raising temperature of charge makes gas deviate to return the sulfur oxychloride synthesis reactor can cause portioned product to lose, the non-condensable gasess such as sulfurous gas that are dissolved in wherein under higher pressure are also more, and the tail gas amount of a production operation increases after causing.For tai gas of rectifying, only mention simply in the patent that sending the sulfur oxychloride synthesis reactor back to surge pump recycles, this technique may cause sulfur oxychloride synthesis reactor pressure to raise gradually, and the reaction mass ratio is unbalance.
Summary of the invention
According to the deficiencies in the prior art, the technical problem to be solved in the present invention is: the method that tail gas recycle is utilized in a kind of sulfur oxychloride preparation is provided, the gas that adopts a kind of liquid-ring compressor that the sulfur oxychloride crude product is discharged from the crude product vulcanizing boiler toward crude product tundish course of conveying, and the condensation tail gas of sulfur oxychloride rectifying, send the sulfur oxychloride synthesis reactor back to and carry out recycle, improve the yield of product sulfur oxychloride, avoided exhaust emissions and environmental pollution.
The technical solution adopted for the present invention to solve the technical problems is: the method that tail gas recycle is utilized in a kind of sulfur oxychloride preparation is provided, the method that described thionyl chloride tail gas is recycled is the gas that the sulfur oxychloride crude product is discharged from the crude product vulcanizing boiler toward crude product tundish course of conveying, and the condensed residual exhaust of sulfur oxychloride rectifying is sent the method for sulfur oxychloride synthesis reactor recycle back to a kind of gas compression conveying machinery.
The present invention is different from CN101284653A, CN101412502A, and for the non-condensable gases that is dissolved in the crude product, what the contriver adopted is the degassed principle of constant temperature decompression, has reduced the gas content in the material that removes next process.For the condensed tail gas of rectifying, liquid-ring compressor, a little repair, simple to operate low than the surge pump cost that the inventor herein adopts.
Used gas compression conveying machinery is liquid-ring compressor.
In the present invention, its transfer pressure of described liquid-ring compressor can reach 0.65MPa, satisfies the requirement of sulfur oxychloride synthesis reactor pressure.
Used liquid-ring compressor with one or both the existing materials in the sulfur oxychloride production process as working medium.
The used working medium of liquid-ring compressor is sulfur monochloride, sulfur oxychloride or both mixtures.
Thionyl chloride tail gas is pressurized to 0.10MPa-0.30MPa returns the recycle of sulfur oxychloride synthesis reactor.
Liquid-ring compressor adopts gas to be back to the mode of entrance or to adopt the mode of compressor variable frequency to control pressure in sulfur oxychloride crude product basin and the distillation tower from compressor outlet.
Liquid-ring compressor adopts the mode of compressor variable frequency to control sulfur oxychloride crude product tundish and the interior pressure of rectifying tower.
Sulfur oxychloride crude product tundish pressure-controlling is at-300Pa-0Pa, and the pressure-controlling in the rectifying tower is in-500Pa--50Pa scope.
Within the time period of adding sulphur in the vulcanizing boiler of rectifying tower, the remaining tail gas aspiration that directly truncates is received after the rectifying condensation.
In the front and back 30min that adds sulphur in the vulcanizing boiler of distillation tower, the remaining tail gas aspiration that directly truncates is received after the rectifying condensation.
In the present invention, for fear of in system, introducing new material, the used working medium of described gas compression e Foerderanlage rotary pump with liquid ring is a kind of material among the sulfur oxychloride preparation technology, can be sulfur oxychloride itself, also can be the mixture of sulfur monochloride or sulfur monochloride and sulfur oxychloride.Preferably, be the higher sulfur monochloride of boiling point.
In the present invention, the gas transmission ability of described liquid-ring compressor is greater than the amount of the tail gas of the required conveying of reality, in order steadily to control the pressure in sulfur oxychloride crude product storage tank and the rectifying tower, liquid-ring compressor can adopt the mode of liquid-ring compressor frequency conversion, also can adopt gas to realize from the mode that compressor outlet is back to entrance, preferably, adopt the mode of compressor variable frequency.
In the present invention, described rectifying condensation tail gas is carried out the mode that automaticallyes switch when recycling, and prevents that the air of will sneak into when adding sulphur in the post cure tank is evacuated to catalyticreactor and causes reaction pressure to raise.
In conjunction with sulfur oxychloride preparation technology, further the present invention is described below:
Chlorine after the vaporization enters the sulfur dichloride synthesis reactor after metering, the sulfur monochloride that comes from rectifying weight-removing column tower reactor also flows into the sulfur dichloride synthesis reactor after measuring, chlorine and sulfur monochloride react under 70 ℃-92 ℃ in the ratio of 150:0.25 (liquid), generate sulfur dichloride.Sulfurous gas after the chlorine that does not react and the sulfur dichloride of generation and the metering is Cl in proportion
2: SO
2: S
2Cl
2Be 150:100:0.25 sulfur oxychloride synthesis reactor, it is 180 ℃-300 ℃ in temperature of reaction, pressure is to generate the sulfur oxychloride mixed gas under the 0.10MPa-0.25MPa, sulfur oxychloride accounts for 45%-55% in the described mixed gas, sulfur dichloride 15%-25%, chlorine 10%-20%, sulfurous gas 20%-25%, sulfuryl chloride 1%-3%.
Mixed gas condensation in the crude product condenser, described condensing temperature are 30-50 ℃, and the sulfur oxychloride crude product that condensation is got off flows in the crude product vulcanizing boiler automatically by potential difference.Sulfur dichloride, the sulfur oxychloride of the uncooled relative non-condensable gases sulfurous gas that gets off, chlorine and a small amount of not total condensation return synthesis reaction vessel with the pressure method in another patent and circulate.
In vulcanizing boiler, with the Molten sulphur that is less than the Theoretical Calculation amount crude product sulfur oxychloride is vulcanized, make sulfur dichloride wherein be converted into sulfur monochloride.The sulphur add-on of liquefaction attitude is the 80%-99% of Theoretical Calculation amount, and is preferred, and the control add-on is the 95%-98% of Theoretical Calculation amount.The amount of owing too much makes sulfur dichloride transform not exclusively, the excessive drawback that exists equally, and excessive sulphur can cause the sulphoxide chloride product color defective, also can blocking pipe, valve and pump, production can not normally be carried out.Vulcanizing boiler top communicates with the sulfur oxychloride synthesis reactor, that is to say that pressure and the sulfur oxychloride synthesis reaction system in the vulcanizing boiler balances each other.
The crude product that vulcanizates flows into the crude product tundish by pressure difference or pump, the crude product tundish keep normal pressure or little negative pressure, the crude product sulfur oxychloride is during shifting from the crude product vulcanizing boiler to the crude product tundish, because of pressure decreased, can discharge the sulfurous gas that is dissolved in wherein and a small amount of sulfur oxychloride, sulfur dichloride.This portion gas compresses with liquid-ring compressor, is pressurized to a little more than the pressure in the catalytic reaction system, makes it to return the sulfur oxychloride synthesis reactor and further reacts, and has realized recycle.
Described liquid-ring compressor is than other the gas compression conveying machinery that is applicable to the sulfur oxychloride production technique, and such as surge pump, cost is low, a little repair and simple to operate, is convenient to automatic control.Described liquid-ring compressor, need a kind of liquid to play fluid-tight and cooling effect, concrete can adopt existing material such as sulfur monochloride, sulfur oxychloride etc. in the sulfur oxychloride production technique, also can adopt the mixture of sulfur monochloride and sulfur oxychloride, preferably, adopt the higher sulfur monochloride of boiling point.
The crude product tundish keep normal pressure or micro-vacuum state, preferably, control its pressure for-100Pa～-50Pa, the large 10%-50% of displacement of actual needs in the gas transmission energy force rate technique of requirement liquid-ring compressor, the mode that the control of crude product tundish internal pressure can be adopted compressor variable frequency perhaps adopts the mode that is back to entrance from pump discharge, realizes the steady of basin internal pressure, preferably, adopt the mode of compressor variable frequency to control.
Sulfur oxychloride crude product after the sulfuration carries out rectification and purification.The mode of continuous rectification is adopted in distillation, is followed successively by weight-removing column, lightness-removing column and product tower.Weight-removing column tower reactor temperature is 100 ℃-130 ℃, tower top temperature is 68 ℃-75 ℃, and reflux ratio is 1:1, and cat head arranges the post cure tank, the sulfur dichloride that does not obtain vulcanizing because of the sulphur amount of owing in the primary vulcanization process carries out capacity but inexcessive sulfuration in the post cure tank, S+SCl
2→ S
2Cl
2, the sulfur monochloride of generation is back to tower reactor, and the high boiling material sulfur monochloride of tower reactor is discharged continuously, returns the sulfur dichloride synthesis reactor.
At the continuous operation of weight-removing column, need irregular toward the interior solid sulfur that adds of post cure tank, to guarantee the capacity sulfuration.When adding sulphur, be drawn into wherein because negative-pressure operation has a small amount of air unavoidably, if condensation tail gas is during this period of time still pushed back the sulfur oxychloride synthesis reactor by liquid-ring compressor, can cause system pressure to raise, affect normally carrying out of building-up reactions.The inventor herein adds the sulphur valve from opening through test, until fill up sulphur valve-off and timing 20-60 minute again, preferred 30 minutes, the distillation condensation tail gas in during this period of time directly removed tail gas absorber, NaOH+SO through automaticallying switch
2=NaHSO
3, after timing was complete, tail gas was through pendular ring blowback sulfur oxychloride synthesis reactor.
Lightness-removing column is identical with weight-removing column with product Ta Yintanei control pressure, and three towers can share a liquid-ring compressor and will distill the pressurization of condensation tail gas and send sulfur oxychloride synthesis reactor (so in the patent figures not shown lightness-removing column and product tower) back to.
Solid sulfur in the post cure tank contains Trace water and divides, and moisture is higher, can generate a kind of non-condensable gases, can cause equally sulfur oxychloride synthesis reactor pressure to raise, and reaction can not normally be carried out, and proves that after tested sulphur water content≤0.5% is acceptable.
The invention has the beneficial effects as follows:
⑴ make sulfurous gas method sulfur oxychloride production technique form a perfect gas phase closed cycle, and the sulfur oxychloride yield is reached more than 99%, can save a large amount of tail gas absorptions and use alkali, eliminated simultaneously environmental pollution.
⑵ liquid-ring compressor is easy and simple to handle, cost is low, a little repair, energy consumption are low, and system does not introduce new medium.
Description of drawings
Fig. 1 is schematic flow sheet of the present invention;
1 is the sulfur oxychloride synthesis reactor among the figure; 2 is the crude product condenser; 3 is the crude product vulcanizing boiler; 4 is the crude product tundish; 5 is liquid-ring compressor; 6 is rectifying tower; 7 are the post cure tank; 8 is condenser.
Embodiment
Below in conjunction with accompanying drawing embodiments of the invention are described further:
Embodiment 1
Present embodiment is described is the gas that discharges from crude product vulcanizing boiler 3 toward crude product tundish 4 feeding process is transmitted back to 1 recycling of sulfur oxychloride synthesis reactor with liquid-ring compressor 5 method, the product that makes is again through entering crude product vulcanizing boiler 3 after 2 condensations of crude product condenser, recycle, specific implementation method is as follows:
Chlorine after the vaporization enters the sulfur dichloride synthesis reactor after metering, formed by weight-removing column, dehydrogenation tower and product tower from rectifying tower 6(rectifying tower) the sulfur monochloride that comes of weight-removing column tower reactor also flow into the sulfur dichloride synthesis reactor after by metering, chlorine and sulfur monochloride are in the ratio of 150:0.25 (liquid), under 83 ℃, react, generate sulfur dichloride.Sulfurous gas after the chlorine that does not react and the sulfur dichloride of generation and the metering is Cl in proportion
2: SO
2: S
2Cl
2Being 150:100:0.25 sulfur oxychloride synthesis reactor 1, is 230 ℃ in temperature of reaction, and pressure is to generate the sulfur oxychloride mixed gas under the 0.25MPa, and sulfur oxychloride accounts for 45% in the described mixed gas, sulfur dichloride 17%, chlorine 18%, sulfurous gas 18%, sulfuryl chloride 2%.
Mixed gas condensation in crude product condenser 2, described condensing temperature are 45 ℃, and the sulfur oxychloride crude product that condensation is got off flows in the crude product vulcanizing boiler 3 automatically by potential difference.Sulfur dichloride, the sulfur oxychloride of the uncooled relative non-condensable gases sulfurous gas that gets off, chlorine and a small amount of not total condensation return synthesis reaction vessel with the pressure method in another patent and circulate.
In crude product vulcanizing boiler 3, with the Molten sulphur that is less than the Theoretical Calculation amount crude product sulfur oxychloride is vulcanized, make sulfur dichloride wherein be converted into sulfur monochloride.The sulfur content add-on of liquefaction attitude is 95% of Theoretical Calculation amount, vulcanizes.
The crude product that vulcanizates is sent into crude product tundish 4 by pressure pump, and crude product tundish 4 keep pressure-80Pa, compress with liquid-ring compressor 5 by the variable frequency adjustment compressor rotary speed, and be 600m with the gas displacement that discharges in the feeding process
3The liquid-ring compressor 5 of ∕ h is pressurized to a little more than the pressure in the catalytic reaction system, makes it to return the sulfur oxychloride synthesis reactor and reacts, and has realized recycle.
What present embodiment was described is in the sulfur oxychloride still-process, and condensation tail gas is transmitted back to the method that sulfur oxychloride synthesis reactor 1 is recycled with liquid-ring compressor 5, and concrete grammar is as follows:
Weight-removing column tower reactor temperature in the rectifying tower 6 is 130 ℃, and tower top temperature is 68 ℃, and reflux ratio is 1:1, and cat head arranges the post cure tank.To deliver to sulfur oxychloride synthesis reactor 1 by condenser 8 condensed rectifying liquefaction tail gas pressurization recovery with liquid-ring compressor 5.Liquid-ring compressor 5 is made circulatory mediator with sulfur monochloride, variable frequency control tower internal pressure, and the weight-removing column pressure tower in the rectifying tower 6 is stabilized in-when 200Pa. adds sulphur toward post cure tank 7, tail gas switched directly remove tail gas absorber, with in the alkali lye and absorb.Timing is 30 minutes after filling up the sulphur valve-off, afterwards tail gas is switched back liquid-ring compressor 5 entrances, and sulfur oxychloride synthesis reactor 1 operating pressure is normal.
Present embodiment is described is after being 0.48% solid sulfur post cure with moisture content, to distill the condensation tail gas recycle to the method for sulfur oxychloride synthesis reactor 1 circulating reaction, and concrete grammar is as follows:
Weight-removing column tower reactor temperature in the rectifying tower 6 is 125 ℃, and tower top temperature is 71 ℃, and reflux ratio is 1:1, and cat head arranges post cure tank 7.With liquid-ring compressor 5 liquefy tail gas pressurization of rectifying is reclaimed and delivered to sulfur oxychloride synthesis reactor 1.Liquid-ring compressor 5 is made circulatory mediator with the mixture of sulfur monochloride and sulfur oxychloride, adopt variable frequency control, weight-removing column tower internal pressure in the rectifying tower 6 is stabilized in-and to record the solid sulfur moisture content of adding toward the post cure tank be 0.48% to 250Pa., when adding sulphur toward the post cure tank, tail gas absorber is directly removed in the tail gas switching, use in the alkali lye and absorption.Timing is 30 minutes after filling up the sulphur valve-off, afterwards tail gas is switched back liquid-ring compressor 5 entrances, moves continuously 72 hours, and sulfur oxychloride synthesis reactor 1 operating pressure is without considerable change.
Claims (10)
1. the method that tail gas recycle was utilized during a sulfur oxychloride prepared, it is characterized in that, the method that described thionyl chloride tail gas is recycled is the gas that the sulfur oxychloride crude product is discharged from the crude product vulcanizing boiler toward crude product tundish course of conveying, and the condensed residual exhaust of sulfur oxychloride rectifying is sent the method for sulfur oxychloride synthesis reactor recycle back to a kind of gas compression conveying machinery.
2. the method that tail gas recycle is utilized in the sulfur oxychloride preparation according to claim 1 is characterized in that used gas compression conveying machinery is liquid-ring compressor.
3. the method that tail gas recycle is utilized in the sulfur oxychloride according to claim 1 preparation, it is characterized in that used liquid-ring compressor with one or both the existing materials in the sulfur oxychloride production process as working medium.
4. the method that tail gas recycle is utilized in the sulfur oxychloride preparation according to claim 3 is characterized in that the used working medium of liquid-ring compressor is sulfur monochloride, sulfur oxychloride or both mixtures.
5. the method that tail gas recycle is utilized in the sulfur oxychloride preparation according to claim 1 is characterized in that thionyl chloride tail gas is pressurized to 0.10MPa-0.30MPa returns the recycle of sulfur oxychloride synthesis reactor.
6. the method that tail gas recycle is utilized in the sulfur oxychloride according to claim 2 preparation is characterized in that liquid-ring compressor adopts gas to be back to the mode of entrance or to adopt the mode of compressor variable frequency to control pressure in sulfur oxychloride crude product basin and the distillation tower from compressor outlet.
7. the method that tail gas recycle is utilized in the sulfur oxychloride preparation according to claim 6 is characterized in that, liquid-ring compressor adopts the mode of compressor variable frequency to control sulfur oxychloride crude product tundish and the interior pressure of rectifying tower.
8. the method that tail gas recycle is utilized in the sulfur oxychloride according to claim 7 preparation is characterized in that, sulfur oxychloride crude product tundish pressure-controlling is at-300Pa-0Pa, and the pressure-controlling in the rectifying tower is in-500Pa--50Pa scope.
9. the method that tail gas recycle is utilized in the sulfur oxychloride according to claim 1 preparation is characterized in that, is adding in the time period of sulphur the remaining tail gas aspiration receipts that directly truncate after the rectifying condensation toward the vulcanizing boiler of rectifying tower in.
10. the method that tail gas recycle is utilized in the sulfur oxychloride according to claim 9 preparation is characterized in that, is adding in the front and back 30min of sulphur the remaining tail gas aspiration receipts that directly truncate after the rectifying condensation toward the vulcanizing boiler of distillation tower in.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104108686A (en) * | 2014-07-31 | 2014-10-22 | 江西世龙实业股份有限公司 | Pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride |
| CN105819405A (en) * | 2016-05-06 | 2016-08-03 | 新乡瑞诚科技股份有限公司 | Sulfur putting method in thionyl chloride refining process |
| CN106315519A (en) * | 2016-08-29 | 2017-01-11 | 山东凯盛新材料股份有限公司 | Method for preparing thionyl chloride |
| CN106335881A (en) * | 2016-08-29 | 2017-01-18 | 山东凯盛新材料股份有限公司 | Technology for preparing thionyl chloride |
| CN106348254A (en) * | 2016-08-29 | 2017-01-25 | 山东凯盛新材料股份有限公司 | Preparing method of thionyl chloride |
| CN106395761A (en) * | 2016-08-29 | 2017-02-15 | 山东凯盛新材料股份有限公司 | Preparation technology of thionyl chloride |
| CN106629626A (en) * | 2017-01-23 | 2017-05-10 | 山东凯盛新材料股份有限公司 | Production technology of thionyl chloride |
| CN106672916A (en) * | 2017-01-23 | 2017-05-17 | 山东凯盛新材料股份有限公司 | Production process of sulfoxide chloride |
| CN106698364A (en) * | 2017-01-23 | 2017-05-24 | 山东凯盛新材料股份有限公司 | Production method for thionyl chloride |
| CN106744712A (en) * | 2017-01-23 | 2017-05-31 | 山东凯盛新材料股份有限公司 | The method for producing thionyl chloride |
| CN106853958A (en) * | 2017-01-23 | 2017-06-16 | 山东凯盛新材料股份有限公司 | The production method of thionyl chloride |
| 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 |
| CN108036667A (en) * | 2017-11-30 | 2018-05-15 | 山东凯盛新材料股份有限公司 | Produce the raw material cryogenic energy utilization technique of 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 |
| CN110980629A (en) * | 2019-12-31 | 2020-04-10 | 宁夏丰华生物科技有限公司 | Liquid chlorine unloading crane pipe tail gas recycling process |
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| CN104108686A (en) * | 2014-07-31 | 2014-10-22 | 江西世龙实业股份有限公司 | Pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride |
| CN104108686B (en) * | 2014-07-31 | 2015-07-08 | 江西世龙实业股份有限公司 | Pressure-relief discharge, absorption, treatment and recycling method in production process of thionyl chloride |
| CN105819405A (en) * | 2016-05-06 | 2016-08-03 | 新乡瑞诚科技股份有限公司 | Sulfur putting method in thionyl chloride refining process |
| CN106315519A (en) * | 2016-08-29 | 2017-01-11 | 山东凯盛新材料股份有限公司 | Method for preparing thionyl chloride |
| CN106335881A (en) * | 2016-08-29 | 2017-01-18 | 山东凯盛新材料股份有限公司 | Technology for preparing thionyl chloride |
| CN106348254A (en) * | 2016-08-29 | 2017-01-25 | 山东凯盛新材料股份有限公司 | Preparing method of thionyl chloride |
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| CN106744712A (en) * | 2017-01-23 | 2017-05-31 | 山东凯盛新材料股份有限公司 | The method for producing thionyl chloride |
| CN106698364B (en) * | 2017-01-23 | 2019-03-15 | 山东凯盛新材料股份有限公司 | The production method of thionyl chloride |
| CN106698364A (en) * | 2017-01-23 | 2017-05-24 | 山东凯盛新材料股份有限公司 | Production method for thionyl chloride |
| CN106629626A (en) * | 2017-01-23 | 2017-05-10 | 山东凯盛新材料股份有限公司 | Production technology of thionyl chloride |
| CN106853958A (en) * | 2017-01-23 | 2017-06-16 | 山东凯盛新材料股份有限公司 | The production method of thionyl chloride |
| CN106744712B (en) * | 2017-01-23 | 2019-05-21 | 山东凯盛新材料股份有限公司 | The method for producing thionyl chloride |
| CN106853958B (en) * | 2017-01-23 | 2019-05-21 | 山东凯盛新材料股份有限公司 | The production method of thionyl chloride |
| CN106672916A (en) * | 2017-01-23 | 2017-05-17 | 山东凯盛新材料股份有限公司 | Production process of sulfoxide chloride |
| CN106672916B (en) * | 2017-01-23 | 2019-03-12 | 山东凯盛新材料股份有限公司 | The production technology of thionyl chloride |
| CN108036667A (en) * | 2017-11-30 | 2018-05-15 | 山东凯盛新材料股份有限公司 | Produce the raw material cryogenic energy utilization technique of thionyl chloride |
| 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 |
| 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 |
| 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 |
| CN110980629A (en) * | 2019-12-31 | 2020-04-10 | 宁夏丰华生物科技有限公司 | Liquid chlorine unloading crane pipe tail gas recycling process |
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