CN101337660B - Method for producing insoluble sulfur - Google Patents
Method for producing insoluble sulfur Download PDFInfo
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- CN101337660B CN101337660B CN2008100736950A CN200810073695A CN101337660B CN 101337660 B CN101337660 B CN 101337660B CN 2008100736950 A CN2008100736950 A CN 2008100736950A CN 200810073695 A CN200810073695 A CN 200810073695A CN 101337660 B CN101337660 B CN 101337660B
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- sulfur
- sulphur
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- functional revolution
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 239000011593 sulfur Substances 0.000 title claims abstract description 56
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000010298 pulverizing process Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 239000005864 Sulphur Substances 0.000 claims description 34
- 239000000203 mixture Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 12
- 238000003860 storage Methods 0.000 claims description 12
- 238000000605 extraction Methods 0.000 claims description 8
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 238000010924 continuous production Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 235000019628 coolness Nutrition 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 2
- 230000002631 hypothermal effect Effects 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010791 quenching Methods 0.000 abstract description 5
- 230000000171 quenching effect Effects 0.000 abstract description 5
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 239000000428 dust Substances 0.000 abstract description 3
- 238000007789 sealing Methods 0.000 abstract 2
- 239000007789 gas Substances 0.000 description 8
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- TXKMVPPZCYKFAC-UHFFFAOYSA-N disulfur monoxide Inorganic materials O=S=S TXKMVPPZCYKFAC-UHFFFAOYSA-N 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Muffle Furnaces And Rotary Kilns (AREA)
Abstract
The invention discloses a method for producing insoluble sulfur, which comprises the steps of melting sulfur, extracting, drying and pulverizing. By using the method, the insoluble sulfur is continuously produced under the totally-enclosed condition of normal pressure, nitrogen of normal pressure is used for sealing a heating groove, and the extracting step and the pulverizing step are completed in the same reactor. The specific operation steps are as follows in sequence: (1) melting the sulfur and heating up; (2) extracting and pulverizing; and (3) drying to obtain products produced through the method. The method has the advantages that: (1) the insoluble sulfur is continuously produced under the totally-enclosed condition of the normal pressure, and nitrogen is used for sealing the upper space of the sulfur heating groove, thereby resulting in no oxide leakage of carbon bisulfide and sulfur, and achieving safe and environmental-friendly production; (2) the pulverizing and quenching processes are finished in the same multifunctional rotary reactor, thus saving pulverizing devices, avoiding dust pollution when pulverizing, and protecting production environment.
Description
Technical field
The invention belongs to the insoluble sulfur preparing technical field, the method for a kind of specifically normal pressure, fully-closed state, continuous production insoluble sulfur.
Background technology
Insoluble sulfur is the polymkeric substance of sulphur, is insoluble to dithiocarbonic anhydride and gains the name.Be widely used in tire industry as vulcanizing agent, along with the linearize of tire meridian, the demand growth of insoluble sulfur is rapid.Thereby the research to insoluble sulfur in recent years also causes increasing attention, has also worked out some production methods, but all has the problem of aspects such as some quality stabilities, security, environment protection.The one-step process for producing of known patent number 03117763.8 described insoluble sulphur for example, its high temperature sulphur will pressurize poor stability; Its single stage method work in-process all process steps is finished in a jar, technic index control difficulty, and level of automation is low, batch quality instability; Work in-process also will be through pulverizing, and dust pollution is big; High temperature sulphur and dithiocarbonic anhydride feed the mixing tank circulating quenching, and easily blocking pipe is cleared up difficulty contaminate environment simultaneously.
Summary of the invention
The objective of the invention is provides the method for a kind of normal pressure, fully-closed state, continuous production insoluble sulfur in order to overcome the deficiency of existing skill wood.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
1. Manufacture of insoluble sulphur method, comprising molten sulphur, extraction, drying and pulverizing, is continuous production insoluble sulfur under normal pressure fully-closed condition, the normal pressure nitrogen-sealed of intensification groove headspace, extraction, pulverizing are finished in same retort, and the concrete operations steps in sequence is:
1). melt sulphur, intensification: sulphur is placed to melt deliver to intensification groove 2 after the fusing of sulphur pond 1 and be warming up to 370～450 ℃, the normal pressure nitrogen-sealed of intensification groove 2 headspaces;
2). extraction, pulverizing:
A. extract: the dithiocarbonic anhydride that with temperature is 0 ℃ is added to the multi-functional revolution retort 5 of rotation from storage tank 9, during to 1/3rd jars, 370～450 ℃ liquid gaseous sulfur are put into multi-functional revolution retort 5 from intensification groove 2, cryogenic dithiocarbonic anhydride cools off high temperature liquid gasiform sulphur suddenly, and the molten wherein soluble sulfur of getting, obtain the refrigerative insoluble sulfur in the leading portion A of multi-functional revolution retort 5 district's sedimentation; Meanwhile, in the tank body periphery of multi-functional revolution retort 5 with-5 ℃ of hypothermic saline spraying coolings;
B. solidify: along with the rotation of multi-functional revolution retort 5, under the material delivering plate effect in multi-functional revolution retort, the mixture that has dissolved the dithiocarbonic anhydride of soluble sulfur and insoluble sulfur slowly moves forward to the B district, middle part of multi-functional revolution retort 5, and insoluble sulfur solidifies;
C. pulverize: rotate with multi-functional revolution retort 5, the mixture that has dissolved the dithiocarbonic anhydride of soluble sulfur and solidified insoluble sulfur moves forward to the afterbody C district of multi-functional revolution retort 5 again, and the solidified insoluble sulfur is ground into 120 purpose powderies under the bump of C district steel ball;
D. the carbon disulfide gas in the multi-functional revolution retort 5 drain into and are condensed into 0 ℃ in the cooler condenser 8 and send into storage tank 9;
3). drying:
A. when mixture reaches 1/2nd jars in the multi-functional revolution retort 5, suspend the rotation of multi-functional revolution retort 5, mixture is put into drying machine;
B. when mixture is reduced to 1/3rd jars in the multi-functional revolution retort 5, stop blowing, be rotated further multi-functional revolution retort 5;
C. in order to control in the multi-functional revolution retort 5 mixtures between 1/2nd to 1/3rd jars, above-mentioned steps 3) in the operation of a and b hocket incessantly;
D. after mixture enters in the rotary vacuum dryer, the dithiocarbonic anhydride that contains soluble sulfur is discharged from the liquid discharge pipe of drying machine by filter cloth, stay insoluble powdery sulphur, meanwhile, in the heating jacket of drying machine, constantly feed 90 ℃ of hot water heating, dry insoluble sulfur;
E. the dithiocarbonic anhydride that contains soluble sulfur from drying machine liquid discharge pipe row is isolated purified dithiocarbonic anhydride through distillation tower 16, is 0 ℃ through cooler condenser 8 coolings, gets back to dithiocarbonic anhydride storage tank 9, isolates sulphur and gets back to and melt sulphur pond 1 and make raw material and use.
The invention has the beneficial effects as follows compared with the prior art:
1. the present invention's continuous production insoluble sulfur under normal pressure fully-closed condition is used nitrogen-sealed sulphur intensification groove headspace, and no dithiocarbonic anhydride and sulfur oxide leak, and produce safe and environmentally friendly.
2. pulverize with quenching process and finish in same multi-functional revolution retort, both saved disintegrating apparatus, production environment has been protected in the pollution of dust when having avoided again pulverizing.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Among the figure: melt sulphur pond 1, intensification groove 2, intensification groove outlet valve 3, swivel joint 4 and 6, multi-functional revolution retort 5, carbon disulfide gas outlet valve 7, cooler condenser 8, dithiocarbonic anhydride storage tank 9, pump 10, pump discharge valve 11, mixture outlet valve 12, rapid-acting coupling 13, drying machine imported valve 14-1,14-2,14-3, drying machine 15-1,15-2,15-3, column still 16.
Embodiment
The present invention is further elaborated to engage accompanying drawing and an embodiment of the invention below:
Production Flow Chart of the present invention as shown in Figure 1
The first step:
One, melting sulphur heats up: adding with industrial sulphur has high-order uncovered the melting in the sulphur pond 1 of steam coils to dissolve, and is warmed up to 370-450 ℃, intensification groove 2 headspace nitrogen protection under normal pressure by putting into the airtight intensification groove 2 of electrically heated communicating pipe.
Two, extraction: start multi-functional revolution retort 5,0 ℃ of low temperature carbon bisulfide of storage tank 9 is pumped in the multi-functional revolution retort 5 to 1/3rd jars by pump 10, pump discharge valve 11, swivel joint 6, and 370-450 ℃ high temperature sulphur in the intensification groove 2 is put into rotation by intensification groove outlet valve 3, swivel joint 4 multi-functional revolution retort 5 is mixed with 0 ℃ of low temperature carbon bisulfide of multi-functional revolution retort and is finished extraction.Thereby tank body is taken away the heat that sulphur quenches and produces in the multi-functional revolution retort with-5 ℃ of cryogenic freezing brine sparge coolings.
Three, carry, solidify, pulverize: the insoluble solid phase sulphur in the mixed solution after the above-mentioned quenching accounts for 45%, rotation along with multi-functional revolution retort 5, pass and be settled down to the A district, rotate under the effect of material delivering plate slowly mobile by multi-functional revolution retort 5, be 8 meters through 4 hours miles of relative movement and arrive the curing of B district, be 2 meters through 1 hour miles of relative movement again and arrive the C district, C is equipped with in the district steel ball bump shredder assembly, thereby steel ball is constantly raised height with the rotation of multi-functional revolution retort 5 and is left the insoluble sulfur pulverizing of bump to the C district under the effect of material delivering plate, finish conveying, solidify, pulverizing process.ABC three districts do not have deadening, because multi-functional revolution retort 5 is installed as the C district state lower than the AB district (multi-functional revolution retort 5 axis and horizontal plane angle are 3 °), steel ball is limited in the C district.Thereby a small amount of carbon disulfide gas is expelled to through swivel joint 6, carbon disulfide gas outlet valve 7 and flows back to dithiocarbonic anhydride storage tank 9 after cooler condenser 8 is condensed into 0 ℃ of cryogenic liquid and guarantee multi-functional revolution retort 5 in to be normal pressure.
Four, by switch valve 7,11 stop carbon disulfide gas through swivel joint 6, valve 7 is expelled to two cooler condensers 8, the low temperature carbon bisulfide of storage tank 9 is passed through pump 10, valve 11, swivel joint 6 pumps in the multi-functional revolution retort 5, switch valve 7 again, 11 allow carbon disulfide gas in the multi-functional revolution retort 5 through swivel joint 6, carbon disulfide gas outlet valve 7 is expelled to and is back to dithiocarbonic anhydride storage tank 9 after cooler condenser 8 is condensed into liquid, in conjunction with second step one described later, binomial, control multi-functional revolution retort 5 interior liquid levels between 1/3rd and 1/2nd, go round and begin again, thereby realize continuous quenching.
Second step:
Conveying, washing, filtration, drying:
One, in insoluble sulfur in the multi-functional revolution retort 5 and dithiocarbonic anhydride mixed solution liquid level reach jar two/for the moment, suspend the rotation of multi-functional revolution retort 5, the dithiocarbonic anhydride by having dissolved soluble sulfur and mixture outlet valve 12, rapid-acting coupling 13, rotary vacuum dryer inlet valve 14-1,14-2 or the 14-3 of powdery insoluble sulfur are discharged to rotary vacuum dryer 15-1,15-2 or 15-3.
Two, when insoluble sulfur and dithiocarbonic anhydride mixed solution in the multi-functional revolution retort 5 remaining 1/3rd or blowing time reach 10 minutes, close the dithiocarbonic anhydride that dissolved soluble sulfur and the mixture outlet valve 12 of powdery insoluble sulfur, take rapid-acting coupling 13 apart, be rotated further multi-functional revolution retort 5, avoid being deposited in the insoluble sulfur heap height in A district.
Three, above-mentioned second step, one, two continuous alternate run.
When four, insoluble sulfur and dithiocarbonic anhydride mixed solution reach 1/2nd jars in each rotary vacuum dryer 15-1,15-2 or the 15-3, filter the insoluble sulfur that stays by the drying machine filter cloth and wash with pure dithiocarbonic anhydride respectively, the dithiocarbonic anhydride of washing back sulfur-bearing cloth after filtration drains into the dithiocarbonic anhydride distillation tower.Washing is to dithiocarbonic anhydride sulphur content≤2% of discharging o'clock, in the heating jacket of drying machine, constantly feed 90 ℃ of hot water heating, dry insoluble sulfur, obtain the product that purity is 95% the inventive method, extract the carbon disulfide gas that produces in the heat-processed with water ring vacuum pump simultaneously, to vacuum tightness reach-during 0.09Mp with the discharging of nitrogen vacuum breaker.The dissolving that guarantees to be free drying machine to receive at any time and emit by valve 12, rapid-acting coupling 13 dithiocarbonic anhydride of soluble sulfur and the mixture of powdery insoluble sulfur.
The sulfur-bearing dithiocarbonic anhydride of discharging when five, each rotary vacuum dryer is washed material is isolated pure dithiocarbonic anhydride by distillation tower and is returned dithiocarbonic anhydride storage tank 9; Isolated sulphur is then got back to and is melted the sulphur pond and recycle as raw material.
Claims (1)
1. a Manufacture of insoluble sulphur method comprises molten sulphur, extraction, drying and pulverizing, it is characterized in that, continuous production insoluble sulfur under normal pressure fully-closed condition, with normal pressure nitrogen-sealed intensification groove, extraction, pulverizing are finished in same retort, and the concrete operations steps in sequence is:
1). molten sulphur, intensification: sulphur placed to melt deliver to intensification groove (2) after melt in sulphur pond (1) and be warming up to 370～450 ℃, the normal pressure nitrogen-sealed of intensification groove (2) headspace;
2) extraction, pulverizing:
A. extract: the dithiocarbonic anhydride that with temperature is 0 ℃ is added to the multi-functional revolution retort (5) of rotation from storage tank (9), during to 1/3rd jars, 370～450 ℃ liquid gaseous sulfur are put into multi-functional revolution retort (5) from intensification groove (2), cryogenic dithiocarbonic anhydride cools off high temperature liquid gasiform sulphur suddenly, and the molten wherein soluble sulfur of getting, obtain the refrigerative insoluble sulfur in the leading portion A of multi-functional revolution retort (5) district's sedimentation; Meanwhile, in the tank body periphery of multi-functional revolution retort (5) with-5 ℃ of hypothermic saline spraying coolings;
B. solidify: along with the rotation of multi-functional revolution retort (5), under the material delivering plate effect in multi-functional revolution retort, the mixture that has dissolved the dithiocarbonic anhydride of soluble sulfur and insoluble sulfur slowly moves forward to the B district, middle part of multi-functional revolution retort (5), and insoluble sulfur solidifies;
C. pulverize, rotate with multi-functional revolution retort (5), the mixture that has dissolved the dithiocarbonic anhydride of soluble sulfur and solidified insoluble sulfur moves forward to the afterbody C district of multi-functional revolution retort (5) again, and the solidified insoluble sulfur is ground into 120 purpose powderies under the bump of C district steel ball;
D. the carbon disulfide gas in the multi-functional revolution retort (5) drains into and is condensed into 0 ℃ in the cooler condenser (8) and sends into storage tank (9);
3). drying:
A. when mixture reaches 1/2nd jars in the multi-functional revolution retort (5), suspend the rotation of multi-functional revolution retort (5), C district mixture is put into drying machine;
B. when mixture is reduced to 1/3rd jars in the multi-functional revolution retort (5), stop blowing, be rotated further multi-functional revolution retort (5);
C. for the mixture of controlling multi-functional revolution retort (5) between 1/2nd to 1/3rd jars, above-mentioned steps 3) in the operation of a and b hocket incessantly;
D. after C district mixture enters in the drying machine, the dithiocarbonic anhydride that contains soluble sulfur is discharged from the liquid discharge pipe of drying machine by filter cloth, stay insoluble powdery sulphur, meanwhile, in the heating jacket of drying machine, constantly feed 90 ℃ of hot water heating, dry insoluble sulfur;
E. the dithiocarbonic anhydride that contains soluble sulfur from drying machine liquid discharge pipe row is isolated purified dithiocarbonic anhydride through distillation tower (16), is 0 ℃ through cooler condenser (8) cooling, gets back to dithiocarbonic anhydride storage tank (9), isolates sulphur and gets back to and melt sulphur pond (1) and make raw material and use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100736950A CN101337660B (en) | 2008-07-24 | 2008-07-24 | Method for producing insoluble sulfur |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100736950A CN101337660B (en) | 2008-07-24 | 2008-07-24 | Method for producing insoluble sulfur |
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| Publication Number | Publication Date |
|---|---|
| CN101337660A CN101337660A (en) | 2009-01-07 |
| CN101337660B true CN101337660B (en) | 2011-06-01 |
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| CN2008100736950A Expired - Fee Related CN101337660B (en) | 2008-07-24 | 2008-07-24 | Method for producing insoluble sulfur |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101798066B (en) * | 2010-04-15 | 2015-04-08 | 江西恒兴源化工有限公司 | Method for preparing nano insoluble sulphur |
| CN102070127B (en) * | 2011-02-17 | 2012-07-18 | 四川晨辉化工有限公司 | Method for producing insoluble sulfur |
| CN103193205A (en) * | 2012-01-09 | 2013-07-10 | 江西恒兴源化工有限公司 | Continuous production method of insoluble sulfur |
| CN102874766A (en) * | 2012-09-26 | 2013-01-16 | 江西恒兴源化工有限公司 | Method for allowing multiple fluid working substances to enter rotating reaction container in insoluble sulphur production |
| JP2014175246A (en) * | 2013-03-12 | 2014-09-22 | Sony Corp | Secondary battery, method for manufacturing secondary battery, positive electrode for secondary battery, method for manufacturing positive electrode for secondary battery, battery pack, electronic apparatus and electric vehicle |
| CN105621370B (en) * | 2016-02-29 | 2017-12-15 | 湖北仙隆化工股份有限公司 | The recovery process and equipment of sulphur in a kind of diethylaluminum monochloride |
| CN106395757A (en) * | 2016-03-02 | 2017-02-15 | 赵水斌 | Fully-automatic continuous production method for insoluble sulfur |
| CN108584884A (en) * | 2018-07-26 | 2018-09-28 | 山西铁峰化工有限公司 | A kind of device and method detaching carbon disulfide byproducts hydrogen sulfide using plasma |
| CN111377411B (en) * | 2018-12-29 | 2021-12-07 | 中国石油化工股份有限公司 | Insoluble sulfur production method and production system |
| CN109896504A (en) * | 2019-04-11 | 2019-06-18 | 无锡华盛橡胶新材料科技股份有限公司 | For the continuous separation of wet production insoluble sulfur, dry system |
| CN113860268A (en) * | 2021-11-18 | 2021-12-31 | 常州工学院 | Insoluble sulfur continuous production screening tank and processing method thereof |
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