CN106892410A - A kind of production method of insoluble sulfur - Google Patents
A kind of production method of insoluble sulfur Download PDFInfo
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- CN106892410A CN106892410A CN201710274173.6A CN201710274173A CN106892410A CN 106892410 A CN106892410 A CN 106892410A CN 201710274173 A CN201710274173 A CN 201710274173A CN 106892410 A CN106892410 A CN 106892410A
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- sulphur
- carbon disulfide
- settler
- insoluble sulfur
- chilling
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
- C01B17/12—Insoluble sulfur (mu-sulfur)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
A kind of production method of insoluble sulfur,It is characterized in that the use of sulphur being raw material,Sulphur is heated to 450 600 DEG C,Under 0.01 0.5MPa,It is passed through chilling tower,The top of chilling tower has carbon disulfide to spray,Chilling bottom of towe is stretched into a container settler equipped with carbon disulfide,There are umbellate form sedimentation plate and sedimentation ring in settler,Settler bottom is equipped with spiral crystallizer and agitator,Spiral crystallizer is connected with liquid phase pulverizer,Liquid phase pulverizer is connected with pump,Pump is connected with closed filtering machine,The solid that filter is filtered out enters a collection filtering together with part carbon disulfide,Washing and dry integrated machine,Filter liquid out enters curing canister,Insoluble sulfur is in filtering,Washing,Filtering is completed in dry integrated machine,Leaching,Drying process,Carried out subsequently into oil-filled machinery oil-filled.
Description
Technical field
The invention belongs to nonmetalloid and its compound field, it is related to a kind of production method of insoluble sulfur.State
Border patent classification belongs to C01B 17/12.
Background technology
Insoluble sulfur (Insoluble sulfur, abbreviation IS) is also known as μ type sulphur, is through ring-opening polymerisation shape by common sulphur
Into long chain polymeric sulphur, gained the name because it does not dissolve in carbon disulfide.Insoluble sulfur is mainly used as the vulcanizing agent of rubber, extensive
For the production of radial, with polymolecularity, high-temperature stability, being used for compounding rubber can be prevented effectively from sizing material spray
Frost, vulcanization effect is good.As the country constantly increases the demand of meridian tire, the demand to insoluble sulfur is also growing day by day.
There is economic benefit and social benefit very high with common sulfur cream insoluble sulfur.
At present, insoluble sulfur preparation method mainly has contact method, evaporating method, fusion method etc..Wherein, contact method is mainly
With hydrogen sulfide as raw material, catalytic oxidation is carried out in acid medium reactor, the method for preparing insoluble sulfur product.And
Evaporating method, fusion method are, with common sulphur as raw material, using sulphur through thermal excitation ring-opening polymerization mechanism, to prepare insoluble sulfur
Sulphur.
(1) contact method
Contact method is with H2S is raw material, by NOx+Fe3+Catalysed oxidn, the method for producing insoluble sulfur[30].Tool
Body step is as follows：By the H of high content2S gases (concentration is more than 70%) and O2It is passed through and contains strong oxidizer HNO3And FeCl3It is water-soluble
Liquid, insoluble sulfur is generated under redox.Contact method prepares insoluble sulfur reaction mechanism：H2S is in Strong oxdiative
Agent HNO3And Fe3+In the presence of, it is partially oxidized into SO3 2-, and reduzate NO；SO3 2-With H2S reaction generation insoluble sulfurs
Sulphur, and the O that reduzate NO is passed into2Oxidation generation NO2, NO2Then with H2S reaction generation insoluble sulfurs；Fe3+Also with H2S
Reaction generation insoluble sulfur and Fe2+, wherein Fe2+Again by NO2It has been oxidized to Fe3+, so as to realize FeCl3The circulation of the aqueous solution makes
With.
Contact method is compared with the method for traditional mode of production insoluble sulfur, it is to avoid the advantage of high temperature corrosion production equipment, is
Petrochemical industry and coal chemical industry enterprises provide a kind of new treatment H2The method of S waste gas.But H2S has severe toxicity, to production equipment
Sealing requirements are high, and due to source of the gas limitation, are difficult to realize large-scale production, technically also there is certain defect in addition,
Need further to be explored and research.
(2) evaporating method
Evaporating method and fusion method are to produce the most traditional method of insoluble sulfur.Wherein evaporating method be by common sulphur with it is suitable
Amount stabilizer is well mixed, and is added in reactor, is placed in and is melted in closed tubular heater and bring up to temperature
500-700 DEG C, the sulfur vapor of overheat sprays into the cooling medium containing stabilizer using the pressure of reactor itself with speed very high
In carry out chilling, a kind of plasticity sulphur can be obtained.After being reversible reaction, chilling due to the polymerisation, there is partially polymerized sulphur
Can change to solvable sulphur, so the plasticity sulphur product for obtaining is a kind of mixture.Then plasticity sulphur is placed under uniform temperature and is consolidated
Change, then crush.In order to obtain the insoluble sulfur product of high content, CS is typically also used2Solution is extracted to it, by
Suction filtration or centrifugation, remove extractant carbon disulfide, and remaining particulate matter is by being exactly products obtained therefrom after dried process.
With respect to comparative maturity for other techniques, its a most prominent advantage is exactly products obtained therefrom to evaporating method technique
In contained insoluble sulfur it is higher, therefore this kind of technique at home and abroad manufacturer first-selection.Have the disadvantage reaction in high temperature
State, equipment requirement is high, high energy consumption and seriously corroded, and production process has certain safety problem.What this technique was used
Extractant carbon disulfide can cause certain infringement to the nerve and blood vessel of people, and can cause poisoning, while being also explosive danger
Product.
(3) fusion method
The difference of state when fusion method is exactly sulphur chilling with the most significant difference of evaporating method.Evaporating method is steam sulphur chilling
And fusion method is liquid sulfur chilling, therefore chilling temperature is also high without the temperature needed for evaporating method.Fusion method prepares insoluble sulfur
The specific operation process of sulphur is：Appropriate stabilizer is added when sulphur starts melting at 130~180 DEG C, and by this state
Under fused mass be warming up to 180~210 DEG C.In order that common sulphur is converted into insoluble sulfur, sulfur melting to greatest extent
Thing is carried out being cooled to room temperature with water rapidly after keeping the stirring of a period of time, is separated water into, and the material of gained is placed in into air
In solidified, the series of process operation such as the solid mass of gained is by crushing, grinding and filtering just can obtain insoluble
The semifinished product of property sulphur.
Fusion method process operation temperatures are relatively low, lighter to equipment corrosion, small with energy consumption, the advantages of safe.But its
The conversion ratio of insoluble sulphur is low, for the stabilizer for ensureing the quenching effect that molten sulfur has had in low temperature polymerization is difficult to find again.This
Process produces insoluble sulfur still in laboratory stage and Industrial Simulation stage, due to key equipment in terms of industrialization
A series of problems, such as and be in research state.
The insoluble sulfur of preparation is divided into two kinds, and one kind is low-grade insoluble sulfur, i.e., without leaching purification
The content of insoluble sulfur, wherein insoluble sulfur only has 50-60%, and also one kind is high-grade insoluble sulfur, wherein not
The content of dissolubility sulphur reaches more than 90%.The industrial general Methods For Purification insoluble sulfur using extraction (also crying leaching),
I.e. using the soluble sulfur in carbon disulfide leaching insoluble sulfur, high-grade insoluble sulfur is obtained.
Insoluble sulfur in use, due to stirring, high temperature, can cause that Cosan flies upward, not only influence production ring
Border, also results in the danger of blast, therefore to prevent flying upward for insoluble sulfur powder, industrially using oil-filled type insoluble sulfur,
Will flash-point mineral oil high be filled into insoluble sulfur powder, reduce dust and fly upward.
Most widely used with evaporating method in the production method of above insoluble sulfur, evaporating method has two kinds of techniques, Yi Zhongshi again
It is chilling liquid with the aqueous solution, metal ion is contained in the aqueous solution, the insoluble sulfur content of ashes of this method production is high, to rubber
The vulcanization of glue and other performance are adversely affected, therefore price is low, but yield is higher；Also one kind is with carbon disulfide as chilling
Liquid, the insoluble sulfur quality of this method production is good, and content of ashes is low, and high-temperature stability is good, and price is high, but yield is relatively low.
Because the sulphur obtained after chilling is elasdco viscous solid, it is necessary to solidify for a long time, could again crush, leach, purify, therefore at present
The production of industrial insoluble sulfur is mostly using batch production method, i.e. chilling, solidification, crushing, leaching purification, oil-filled etc.
Step is carried out in the equipment of different batch (-type)s respectively.This production technology causes very big problem, due to the behaviour of each process
All there is artificial factor, thus product quality be difficult to it is homogeneous, and for using carbon disulfide for chilling liquid production
, there is carbon disulfide leakage, spontaneous combustion (self-ignition point of carbon disulfide only has 90 DEG C, and boiling point is 46 DEG C, and flash-point is -45 DEG C), poison in journey
A kind of danger such as evil, it is therefore desirable to production technology of serialization, carbon disulfide is circulated in closed system, and reduction was produced
The exposure of material, volatilization and leakage, do not keep the safety in production and provide safeguard, while improve product quality and product yield between journey.
The content of the invention
It is an object of the invention to provide a kind of method and technique for continuous production insoluble sulfur, reduce solvent and wave
Hair and consumption, reduce environmental pollution, reduce labour intensity, improve production process safe coefficient.
The present invention is raw material using industrial sulphur, specifically includes following steps：
(1) industrial sulphur is heated to 350-600 DEG C, under 0.05-1MPa, is passed through chilling tower, the top of chilling tower has
Carbon disulfide is sprayed, and has chevron shaped tower tray in chilling tower, and chilling bottom of towe stretches into a container equipped with carbon disulfide and settles
There are umbellate form sedimentation plate and sedimentation ring in device, in settler, settler bottom is equipped with spiral crystallizer and agitator, spiral crystallizer
It is connected with liquid phase pulverizer, liquid phase pulverizer is connected with pump, pump is connected with closed filtering machine, settler and saturation carbon disulfide
Tank is connected；
(2) after sulphur enters chilling tower, the carbon disulfide entered by chilling tower top spray carries out chilling, the sulphur after chilling
Sulphur becomes the semi-solid of viscoelasticity and enters in settler, and the umbellate form sedimentation plate and sedimentation ring in settler are by these viscoelasticities
Sulphur is slowly settled down to settler bottom in an orderly manner, and the agitator in settler bottom smashes these viscoelasticity sulphur, passes through
The spiral crystallizer of settler bottom is delivered to liquid phase pulverizer at leisure, and is solidified in spiral crystallizer, and sulphur exists
It is ground in liquid phase pulverizer, is crushed, the drusen as granularity 50-200 mesh；
(3) material by pulverizer out squeezes into a collection and is filtered, washed and dried three kinds of work(together with carbon disulfide pump
The machinery (abbreviation all-in-one) that can be integrated, the similar jacketed reactor of the all-in-one, bottom is equipped with stainless steel filter, can be with
Drusen is prevented to spill, inside is equipped with agitator, outside has the chuck can be heated with hot water or steam, and side is near filter
There is solid outlet position；
(4) it is then new to being squeezed into all-in-one by the carbon disulfide of one motor spindle pumping to saturation curing canister
Not sulfureted carbon disulfide that is fresh or reclaiming, the consumption of carbon disulfide is 1-2 times of sulphur weight, then stirs 30-60 points
Clock, filtering, filtrate is extracted into carbon disulfide storage tank, then adds the carbon disulfide for accounting for 0.5-1 times of volume of sulphur, stirs 30-60
Minute, then to filter, filtrate enters carbon disulfide storage tank；
(5) to hot water is passed through in all-in-one outer layer chuck, the temperature of hot water is 60-100 DEG C, it is also possible to be passed through vapor generation
For hot water, all-in-one agitator is started, and open the vavuum pump of the machine that is integrally connected, carbon disulfide remaining in all-in-one is steamed
Beam back receipts；
(6) when the liquid level of carbon disulfide in the water pot of vacuum pump outlet connection does not increase, vavuum pump is closed, to all-in-one
Cooling water is passed through in chuck, until when the insoluble sulfur temperature in all-in-one is down to less than 40 DEG C, to being passed through nitrogen in all-in-one
Then gas open the solid outlet of all-in-one side to normal pressure, and insoluble sulfur is discharged into oil charging machine；
(8) oil charging machine is the machinery with agitating device, after insoluble sulfur enters oil charging machine, squeezes into filling oil, stirring
Uniformly, that is, oil-filled type insoluble sulfur is obtained；
(9) the carbon disulfide pump in curing canister squeezes into heater and is heated to 120-200 DEG C into carbon disulfide steaming
Hair recovery tower, tower top carbon disulfide steam out enters condensate cooler and reclaims carbon disulfide, and bottom of towe is mainly sulphur and two
Nitric sulfid enters stripper, and stripper bottom has vapor to enter, and overhead vapours enters condensate cooler and reclaims carbon disulfide, tower
The sulphur that bottom obtains enters after sulfur forming machine is molded as commodity sulphur.
Chilling tower in step one is located at settler top, and settler is equipped with built with umbellate form sedimentation plate on sedimentation wall
Sedimentation ring, settler bottom is equipped with agitator；Sedimentation plate and the inclination angle that sedimentation wall is in 8-20 °；Settler bottom crystallizes with spiral
Device is connected；Spiral crystallizer is connected with liquid phase pulverizer entrance.The invention is carried out slightly not using filtering, washing, dry integrated machine
The leaching of dissolubility sulphur, purification.Sulphur all condensation, coolings that the amount of the carbon disulfide of chilling tower needs to enter are squeezed into, so
Washes clean, therefore its flow afterwards will typically reach 10-100 times of sulphur inlet amount, otherwise have the evaporation of a large amount of carbon disulfide,
Gasification.Because chilling top of tower has outflow pipeline, condensate cooler, therefore the carbon disulfide that will can not condense out are connected
Steam condensation, cooling.
The method is illustrated below in conjunction with the accompanying drawings.
Brief description of the drawings
1. sulphur tank；2. nitrogen pot；3. pump；4. heater；5. heating furnace；6. settler；7. chilling tower；8. sleeve pipe crystallization
Device；9. agitator；10. pump；11. coolers；12. liquid phase pulverizers；13. pumps；14. pans；15. saturation curing canisters；
16. filterings, washing, dry integrated machine；17. oil charging machines；18. insoluble sulfur packaging bags；19. vavuum pumps；20. water sealed tanks；21.
Filling oil tank；22. carbon disulfide storage tanks；23. filtrate tanks；24. pumps；25. pumps；26. heaters；27. evaporating columns；28. condensations are cold
But device；29. coolers；30. condensers；31. strippers；32. flowmeters；33. sulfur forming comminutors；34. containers；35. streams
Gauge；36. pumps；37. pumps；38. condensate coolers；39. pumps.
As shown in drawings, the air in all of Sealing Arrangement is replaced as nitrogen with the nitrogen in nitrogen pot (2) first,
Industrial liquid sulphur is got into steam heater (4) from sulphur tank (1) by pump (3) and is heated to 200 DEG C or so, subsequently into heating
Stove (5) is heated to 350-600 DEG C, under 0.05-1.0MPa, is passed through chilling tower (7), and the top of chilling tower has carbon disulfide to spray
Drench, and have tower tray in chilling tower, chilling bottom of towe is stretched into a container settler (6) equipped with carbon disulfide, settler (6)
Inside have umbellate form sedimentation plate and sedimentation ring, settler bottom be equipped with spiral crystallizer (8) and agitator (9), spiral crystallizer (8) and
Liquid phase pulverizer (12) is connected, and liquid phase pulverizer (12) is connected with pump (13), and pump (13) is connected with pans (14), settler
(6) it is connected with saturation curing canister (15).
After sulphur enters chilling tower (7), the carbon disulfide entered by chilling tower (7) top spray carries out chilling, after chilling
Sulphur become the semi-solid of viscoelasticity and enter in settler (6), the umbellate form sedimentation plate and sedimentation ring in settler (6) by this
The sulphur of a little viscoelasticities is slowly settled down to settler (6) bottom in an orderly manner, sedimentation plate and sedimentation wall in 8-20 ° inclination angle so that
Viscoelasticity sulphur can slowly fall, and sedimentation ring is the doughnut-shaped steel plate being close on sedimentation wall, and middle opening is less than sedimentation plate
Diameter, sedimentation ring also has downward inclination angle, about 93-110 ° of the inclination angle, and sedimentation plate and sedimentation ring are staggered up and down；In settler
(6) agitator (9) of bottom smashes these viscoelasticity sulphur, and the spiral crystallizer (8) by settler bottom is defeated at leisure
Liquid phase pulverizer (12) is delivered to, and is solidified in spiral crystallizer (8), sulphur is ground in liquid phase pulverizer (12),
Crush, the drusen as granularity 50-200 mesh squeezes into pans (14) by pump (13).Spiral crystallizer is that interior have scraper plate
Cylinder, there is screw rod centre, can provide insoluble sulfur hardening time, while can play the purpose of helical feed again.
The solid sulfur in pans (14) is filtered, washed and dried together with part carbon disulfide into a collection with pump
The machinery (abbreviation all-in-one 16) that three kinds of functions are integrated, the all-in-one (16) is jacketed reactor, and bottom is equipped with stainless steel
Filter, can prevent drusen from spilling, and inside is equipped with agitator, and outside has the chuck can be heated with hot water or steam, side
There is solid outlet on side near filtering Board position, and all-in-one can typically set many, and such one operationally, and another can be with
Charging, it is ensured that system is constantly in continuous running status.
The carbon disulfide pump (39) of all-in-one (16) bottom is extracted into saturation curing canister (15) or filtrate tank (23),
Then to the carbon disulfide that fresh or evaporation is reclaimed is squeezed into all-in-one, the consumption of carbon disulfide is 1-2 times of sulphur weight, so
Stir 30-60 minutes afterwards, filtering, filtrate is extracted into filtrate tank (23), then add 0.5-1 times of carbon disulfide, stir 30-60
Minute, then to filter, filtrate enters filtrate tank (23).
To hot water is passed through in all-in-one (16) outer layer chuck, the temperature of hot water is 60-100 DEG C, it is also possible to be passed through vapor
Instead of hot water, all-in-one agitator is started, and open the vavuum pump (19) for being integrally connected machine (16), will be residual in all-in-one (16)
Remaining carbon disulfide evaporation is reclaimed.When the liquid level of carbon disulfide in the water pot (20) of vavuum pump (19) outlet connection does not increase,
Vavuum pump (19) is closed, to being passed through cooling water in all-in-one (16) chuck, until the insoluble sulfur temperature in all-in-one (16)
When being down to less than 40 DEG C, to nitrogen to normal pressure is passed through in all-in-one (16), the solid outlet of all-in-one side is then opened, will
Insoluble sulfur is discharged to oil charging machine (17).
Oil charging machine (17) is the machinery with agitating device, after insoluble sulfur enters oil charging machine (17), with pump (36) from
Oil pumping in filling oil tank (21), to filling oil is squeezed into oil charging machine (17), stirs, that is, obtain oil-filled type insoluble sulfur.
Carbon disulfide pump in curing canister (23) squeezes into heater (26) and is heated to 120-200 DEG C and enters curing
Carbon evaporating column (27), tower top carbon disulfide steam out enters recovery carbon disulfide in condensate cooler (28), and bottom of towe is main
It is the carbon disulfide of sulphur and remaining, stripper is squeezed into pump (37), stripper bottom has vapor to enter, overhead vapours enters
Condenser (30) and cooler (29) reclaim carbon disulfide, and the sulphur that bottom of towe is obtained enters conduct after sulfur forming machine (33) shaping
Commodity sulphur, or return sulphur tank (1) reuse.
The effect of invention
The production of insoluble sulfur is carried out according to above method, it is possible to achieve continuous operation, the insoluble sulfur matter for obtaining
Amount stabilization, high income, good stability.Production process is revealed without carbon disulfide, and the consumption of carbon disulfide is substantially reduced, eliminated
Potential safety hazard, reduces labor strength.
Specific embodiment
Technique of the invention is further illustrated with reference to embodiment.
Embodiment 1：
A Pilot Unit such as accompanying drawing 1 is prepared for according to feature of the invention in the lab, it is every using sulphur
Hour inlet amount is 6kg/h, is heated to 550 DEG C, and the internal circulating load of carbon disulfide is 100kg/h, the product of the insoluble sulfur for obtaining
Rate reaches 41%, oil-filled and add after stabilizer at 105 DEG C, 15 minutes, and the stability of insoluble sulfur reaches 92%, insoluble
Sulfur content 97%；At 120 DEG C, 15 minutes, the stability of insoluble sulfur reached 45%.Thus experimental provision can be seen that
Using the method, it is possible to achieve continuous production.
Embodiment 2：
Experimental provision same as Example 1, inlet amount is 6kg/h per hour to use sulphur, is heated to 350 DEG C, two sulphur
The internal circulating load for changing carbon is 80kg/h, and the yield of the insoluble sulfur for obtaining reaches 35%, oil-filled and add after stabilizer at 105 DEG C
Under, 15 minutes, the stability of insoluble sulfur reached 93%, insoluble sulfur content 97%；At 120 DEG C, 15 minutes, insoluble sulfur
The stability of sulphur reaches 45%.Thus experimental provision can be seen that and use the method, it is possible to achieve continuous production.
Embodiment 2：
Experimental provision same as Example 1, inlet amount is 6kg/h per hour to use sulphur, is heated to 600 DEG C, two sulphur
The internal circulating load for changing carbon is 120kg/h, and the yield of the insoluble sulfur for obtaining reaches 35%, oil-filled and add after stabilizer 105
At DEG C, 15 minutes, the stability of insoluble sulfur reached 94%, insoluble sulfur content 95%；It is 15 minutes, insoluble at 120 DEG C
The stability of sulphur reaches 46%.Thus experimental provision can be seen that and use the method, it is possible to achieve continuous production.
By equipment is limited, bigger experimental provision is not manufactured, but principle is similar.Can be seen by example above
Go out, continuous production can be realized using the equipment, reduce solvent volatilization and be lost, moreover it is possible to reduce environmental pollution and disaster hidden-trouble.
Certainly, the above is only one embodiment of the present invention, it should be pointed out that those skilled in the art come
Say, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications belong to this
Within invention scope of the claims.
Claims (6)
1. a kind of production method of insoluble sulfur, it is characterised in that the use of industrial sulphur is raw material, specifically includes following steps：
(1) industrial sulphur is heated to 350-600 DEG C, under 0.05-1MPa, is passed through chilling tower, two sulphur are arranged at the top of chilling tower
Change carbon spray, and have chevron shaped tower tray in chilling tower, chilling bottom of towe is stretched into a container settler equipped with carbon disulfide,
There are umbellate form sedimentation plate and sedimentation ring in settler, settler bottom is equipped with spiral crystallizer and agitator, spiral crystallizer and liquid
Phase pulverizer is connected, and liquid phase pulverizer is connected with pump, and pump is connected with closed filtering machine, settler and saturation curing canister phase
Even；
(2) after sulphur enters chilling tower, the carbon disulfide entered by chilling tower top spray carries out chilling, and the sulphur after chilling becomes
Semi-solid into viscoelasticity enters in settler, and the umbellate form sedimentation plate and sedimentation ring in settler are by the sulphur of these viscoelasticities
Settler bottom is slowly settled down in an orderly manner, the agitator in settler bottom smashes these viscoelasticity sulphur, by sedimentation
The spiral crystallizer of device bottom is delivered to liquid phase pulverizer at leisure, and is solidified in spiral crystallizer, and sulphur is in liquid phase
It is ground in pulverizer, is crushed, the drusen as granularity 50-200 mesh；
(3) pulverizer material out together with carbon disulfide pump is squeezed into a collection it is filtered, washed and dried three kinds of functions and is
The machinery (abbreviation all-in-one) of one, the similar jacketed reactor of the all-in-one, bottom is equipped with stainless steel filter, can prevent
Drusen spills, and inside is equipped with agitator, and outside has the chuck can be heated with hot water or steam, and side is near filtering Board position
There is solid outlet；
(4) by the carbon disulfide of one motor spindle pumping to saturation curing canister, then to squeezed into all-in-one it is fresh or
The not sulfureted carbon disulfide for reclaiming, the consumption of carbon disulfide is 1-2 times of sulphur weight, is then stirred 30-60 minutes, mistake
Filter, filtrate is extracted into carbon disulfide storage tank, then adds the carbon disulfide for accounting for 0.5-1 times of volume of sulphur, stirs 30-60 minutes,
Then filter, filtrate enters carbon disulfide storage tank；
(5) to hot water is passed through in all-in-one outer layer chuck, the temperature of hot water is 60-100 DEG C, it is also possible to is passed through vapor and replaces heat
Water, all-in-one agitator is started, and opens the vavuum pump of the machine that is integrally connected, and carbon disulfide remaining in all-in-one is evaporated back
Receive；
(6) when the liquid level of carbon disulfide in the water pot of vacuum pump outlet connection does not increase, vavuum pump is closed, to all-in-one chuck
In be passed through cooling water, until when the insoluble sulfur temperature in all-in-one is down to less than 40 DEG C, to being passed through nitrogen in all-in-one extremely
Normal pressure, then opens the solid outlet of all-in-one side, and insoluble sulfur is discharged into oil charging machine；
(8) oil charging machine is the machinery with agitating device, after insoluble sulfur enters oil charging machine, squeezes into filling oil, is stirred,
Obtain oil-filled type insoluble sulfur；
(9) the carbon disulfide pump in curing canister squeezes into heater and is heated to 120-200 DEG C and evaporates back into carbon disulfide
Tower is received, tower top carbon disulfide steam out enters condensate cooler and reclaims carbon disulfide, and bottom of towe is mainly sulphur and curing
Carbon enters stripper, and stripper bottom has vapor to enter, and overhead vapours enters condensate cooler and reclaims carbon disulfide, and bottom of towe is obtained
The sulphur for arriving enters after sulfur forming machine is molded as commodity sulphur.
2. method according to claim 1, it is characterised in that chilling tower is located at settler top, and settler is built with umbellate form
Sedimentation plate, equipped with sedimentation ring on sedimentation wall, settler bottom is equipped with agitator.
3. the method according to claim 1 and 2, it is characterised in that sedimentation plate and sedimentation wall are in 8-20 ° of inclination angle.
4. method according to claim 1, it is characterised in that settler bottom is connected with spiral crystallizer.
5. the method according to claim 1 and 4, it is characterised in that spiral crystallizer is connected with liquid phase pulverizer entrance.
6. method according to claim 1, it is characterised in that carry out insoluble sulfur using filtering, washing, dry integrated machine
The leaching of sulphur, purification.
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| CN108383088A (en) * | 2018-04-28 | 2018-08-10 | 上海京海（安徽）化工有限公司 | A kind of production system and production method of insoluble sulfur |
| CN110304610A (en) * | 2019-08-06 | 2019-10-08 | 武汉轻工大学 | A kind of quenching synthesizer preparing insoluble sulfur |
| CN110697659A (en) * | 2019-08-12 | 2020-01-17 | 中国石油大学(华东) | Method for separating and extracting sulfur powder in water in insoluble sulfur preparation process |
| CN112209349A (en) * | 2020-09-29 | 2021-01-12 | 广州市来力实业有限公司 | Method and device for full-automatic continuous preparation of polymeric sulfur |
| CN113120869A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur production method and production system |
| CN113120867A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur processing method and system |
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| CN114436220A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | Quenching system and method for producing insoluble sulfur by low-temperature melting method |
| CN116062705A (en) * | 2021-10-31 | 2023-05-05 | 中国石油化工股份有限公司 | Insoluble sulfur production system and method by low-temperature melting method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202139051U (en) * | 2011-07-26 | 2012-02-08 | 山东阳谷华泰化工股份有限公司 | Multifunctional device for producing insoluble sulfur |
| CN106082139A (en) * | 2016-06-13 | 2016-11-09 | 黄煜 | The production method of insoluble sulfur and the equipment of production |
-
2017
- 2017-04-25 CN CN201710274173.6A patent/CN106892410B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202139051U (en) * | 2011-07-26 | 2012-02-08 | 山东阳谷华泰化工股份有限公司 | Multifunctional device for producing insoluble sulfur |
| CN106082139A (en) * | 2016-06-13 | 2016-11-09 | 黄煜 | The production method of insoluble sulfur and the equipment of production |
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| CN107185691B (en) * | 2017-07-10 | 2020-04-14 | 河北锐智纳米科技有限公司 | Sulfur powder production line based on nitrogen protection |
| CN108383088A (en) * | 2018-04-28 | 2018-08-10 | 上海京海（安徽）化工有限公司 | A kind of production system and production method of insoluble sulfur |
| CN108383088B (en) * | 2018-04-28 | 2023-12-15 | 上海京海（安徽）化工有限公司 | Production system and production method of insoluble sulfur |
| CN110304610A (en) * | 2019-08-06 | 2019-10-08 | 武汉轻工大学 | A kind of quenching synthesizer preparing insoluble sulfur |
| CN110697659A (en) * | 2019-08-12 | 2020-01-17 | 中国石油大学(华东) | Method for separating and extracting sulfur powder in water in insoluble sulfur preparation process |
| CN113120869B (en) * | 2019-12-31 | 2023-01-10 | 中国石油化工股份有限公司 | Insoluble sulfur production method and production system |
| CN113120867A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur processing method and system |
| CN113120869A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur production method and production system |
| CN113120867B (en) * | 2019-12-31 | 2023-01-10 | 中国石油化工股份有限公司 | Insoluble sulfur processing method and system |
| CN112209349A (en) * | 2020-09-29 | 2021-01-12 | 广州市来力实业有限公司 | Method and device for full-automatic continuous preparation of polymeric sulfur |
| CN114436220A (en) * | 2020-10-31 | 2022-05-06 | 中国石油化工股份有限公司 | Quenching system and method for producing insoluble sulfur by low-temperature melting method |
| CN116062705A (en) * | 2021-10-31 | 2023-05-05 | 中国石油化工股份有限公司 | Insoluble sulfur production system and method by low-temperature melting method |
| CN114011558A (en) * | 2021-11-05 | 2022-02-08 | 山东阳谷华泰化工股份有限公司 | Particle size control method of insoluble sulfur |
| CN114011558B (en) * | 2021-11-05 | 2022-08-09 | 山东阳谷华泰化工股份有限公司 | Particle size control method of insoluble sulfur |
| CN113893587A (en) * | 2021-11-25 | 2022-01-07 | 常州工学院 | Continuous sedimentation collector for producing insoluble sulfur quenching material |
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