CN101875485A - Preparation method of high content insoluble sulfur - Google Patents
Preparation method of high content insoluble sulfur Download PDFInfo
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- CN101875485A CN101875485A CN2009102346997A CN200910234699A CN101875485A CN 101875485 A CN101875485 A CN 101875485A CN 2009102346997 A CN2009102346997 A CN 2009102346997A CN 200910234699 A CN200910234699 A CN 200910234699A CN 101875485 A CN101875485 A CN 101875485A
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Abstract
The invention discloses a preparation method of high content insoluble sulfur (IS). In the preparation technology, the procedures of extraction, washing, suction filtration and drying are continuously finished in the same drier, wherein the extraction is carried out under the protection of adding CS2 and N2; after extraction, mother solution is pumped off; CS2 is added twice for washing and then suction filtration; then, jacket hot water is used for heating and drying; the material is obtained after water cooling; the extraction and drying are carried out under rotation; suction filtration and drying are carried out under the vacuum pressure of 0.01 to 0.03MPa; a cavity of the drier is closed; and the drier only has one dynamic seal. By adopting the technological specification of the method, the materials is not transferred in the production without leakage; safety environmental requirements are satisfied; moreover, washing and suction filtration are carried out twice; vacuum drying is carried out; each technological condition and technological parameter are selected reasonably and mutually matched; remaining insoluble sulfur is reduced, thereby preventing IS from reducing into the insoluble sulfur; accordingly, the content of IS is enhanced. Indicated by a test, in IS powder prepared by the invention, the content of IS is not less than 98%.
Description
Technical field
The present invention relates to the preparation method of the method that a kind of high temperature gas phase method prepares insoluble sulfur, particularly high content insoluble sulfur.
Background technology
The chemical name of insoluble sulfur is the homopolymer of sulphur, is called for short IS.It is a kind of metastable polymkeric substance, and under the situation of being heated, can revert gradually is common sulphur (being solubility sulphur) especially.IS is a kind of vulcanizer of excellence, is mainly used in the special-purpose vulcanizing agent of radial at present, because IS is insoluble to CS
2And rubber, so have best no blooming, and can effectively prevent the incipient scorch of sizing material and promote the bonding of twine in rubber and the tire, and soluble sulfur is used as vulcanizing agent with its sulfurized rubber, can make sizing material crocking, so require the solvable sulphur content in the IS product to want≤2.5%.Each operation is independently to carry out in the domestic existing production technique, fail to accomplish serialization, security incident easily takes place in material in transfer process, difficulty reaches the processing condition of regulation, and in the existing technology, each processing parameter is selected unreasonable, not strict, can not realize in the effective cooperation, particularly drying process that the requirement of sealing and vacuum tightness does not reach, time of drying is long, causes IS content not high.
Summary of the invention
The objective of the invention is to overcome the weak point in the existing production technique, a kind of production safety, technological specification are provided, effectively improve IS content, satisfy the preparation method of the high content insoluble sulfur of radial factory demand.
Technical scheme of the present invention is: the preparation method of high content insoluble sulfur makes high-content IS powder with high-temperature evaporation polymeric IS-60 powder (IS-60 is meant the polymerised sulphur that contains 40% left and right sides soluble sulfur) behind extraction, washing, suction filtration, drying process, its improvements are that described extraction, washing, suction filtration, drying process are finished in the same equipment of multi-functional dry machine continuously, and extraction is adding CS
2And N
2Carry out under the protection, be forced into 0.4～0.6MPa pressure after the extraction and carry out suction filtration, add CS again after draining mother liquor
2Wash and suction filtration again, washing and again suction filtration repeat twice, then carry out drying, temperature of charge is 23 ℃～27 ℃ when dry, time of drying 115～125min, when temperature rises to 40 ℃～50 ℃, the dry end, described extraction and drying are carried out under drying machine rotates, and described suction filtration and drying are all carried out under vacuum tightness 0.01～0.03MPa pressure, described drying machine inner chamber is airtight, has only a dynamic seal.
Further scheme is: described drying process carries out under the heating of drying machine chuck hot water, and the hot water temperature is 80 ℃～82 ℃; Behind dry the end, discharge chuck hot water, feed water quench, drying machine rotates 25～35min again, and temperature stops operating discharging when reducing to 24 ℃～26 ℃; When drying machine rotated, velocity of rotation was 4～5r/min.
Among the present invention, each operation is finished in same equipment continuously, and material does not need to shift, and safety and environmental protection not only, and can guarantee the processing condition stipulated is accomplished technological specification, helps the raising of quality product and stablizes.In the production, the suction filtration after washing and the washing carries out at twice, soluble sulfur is fully diluted and absorbs, and after filtration unit improved in the used drying machine, filtration area increased, and makes CS
2Mother liquor suction filtration effect improves greatly, and the mother liquor suction filtration is dried more, and the soluble sulfur that remains among the IS is just few more, and then improves IS content.In addition, used dryer design becomes the eccentric rotary type of bipyramid, makes material mix better CS in drying process
2Evaporation effect is better, has shortened time of drying, and the drying machine inner chamber is airtight, has only a dynamic seal, and nothing in service is leaked, and guarantees inner chamber vacuum tightness, CS under 0.01～0.03MPa vacuum
2Boiling point is about 25 ℃, and this is quite favourable to heat-sensitive material IS, low temperature again fast drying can guarantee that IS is not reduced to soluble sulfur in the drying process, thereby effectively improve IS content.The present invention is through repetition test, each processing condition and processing parameter have been made choose reasonable, technological specification, help suitability for industrialized production, each processing condition and processing parameter cooperatively interact, and form new technical scheme, IS content 〉=98% of the IS powder of feasible preparation, reach and surpass the requirement of radial factory, this product becomes the exclusive dealing product of Michelin.
Embodiment
Further specify the present invention below by embodiment.
1, the IS-60 powder after the high-temperature evaporation polymerization (IS-60 is meant the polymerised sulphur that contains 40% left and right sides soluble sulfur) 1400kg is added by N
2In the eccentric rotary shelf drier of the 3500L bipyramid of replacing, through being sealed in N
2Protection adds CS down
22000kg, tumble dried machine 15min, rotating speed 4r/min makes IS-60 powder and CS
2The thorough mixing extraction stops operating, then with N
2Be forced into 0.5MPa, carry out the suction filtration under the vacuum tightness 0.02MPa again, in pipeline, do not have CS
2Mother liquor flows out.
2, add CS after mother liquor is drained again
21800kg under the drying machine stationary state, leaches washing 5min to material in the machine, is forced into 0.5MPa again, carries out the vacuum filtration 0.02MPa under, until draining, and then adding CS
21800kg washs suction filtration with method.
3, with the IS that drains through twice washing in the drying machine under vacuum tightness 0.02MPa pressure, feed 80 ℃ of hot water heating by chuck, and the tumble dried machine carries out drying under the 5r/min rotating speed, and temperature of charge is 23 ℃ in this opportunity, behind the dry 115min, temperature rises to 42 ℃ of dry end, discharge hot water in the chuck, feed water coolant, drying machine rotates 30min again, temperature drops to 25 ℃ and stops operating discharging.
Claims (4)
1. the preparation method of a high content insoluble sulfur, high-temperature evaporation polymeric IS-60 powder is made high-content IS powder behind extraction, washing, suction filtration, drying process, it is characterized in that described extraction, washing, suction filtration, drying process finish in the same equipment of multi-functional dry machine continuously, extraction is adding CS
2And N
2Carry out under the protection, be forced into 0.4～0.6MPa pressure after the extraction and carry out suction filtration, add CS again after draining mother liquor
2Wash and suction filtration again, washing and again suction filtration repeat twice, then carry out drying, temperature of charge is 23 ℃～27 ℃ when dry, time of drying 115～125min, when temperature rises to 40 ℃～50 ℃, the dry end, described extraction and drying are carried out under drying machine rotates, and described suction filtration and drying are all carried out under vacuum tightness 0.01～0.03MPa pressure, described drying machine inner chamber is airtight, has only a dynamic seal.
2. by the preparation method of the described high content insoluble sulfur of claim 1, it is characterized in that described drying process carries out under the heating of drying machine chuck hot water, the hot water temperature is 80 ℃～82 ℃.
3. by the preparation method of the described high content insoluble sulfur of claim 2, it is characterized in that dry the end after, discharge chuck hot water, feed water quench, drying machine rotates 25～35min again, temperature stops operating discharging when reducing to 24 ℃～26 ℃.
4. by the preparation method of claim 1 or 3 described high content insoluble sulfurs, when it is characterized in that drying machine rotates, velocity of rotation is 4～5r/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102346997A CN101875485A (en) | 2009-11-27 | 2009-11-27 | Preparation method of high content insoluble sulfur |
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| CN2009102346997A CN101875485A (en) | 2009-11-27 | 2009-11-27 | Preparation method of high content insoluble sulfur |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826515A (en) * | 2012-08-24 | 2012-12-19 | 江西恒兴源化工有限公司 | Method for preparing high-purity insoluble sulphur by using secondary purification method |
| CN104555943A (en) * | 2013-10-12 | 2015-04-29 | 江苏宏泰橡胶助剂有限公司 | Method for preparing high-quality insoluble sulphur from continuous pipelined overheated sulphur steam |
| CN106395757A (en) * | 2016-03-02 | 2017-02-15 | 赵水斌 | Fully-automatic continuous production method for insoluble sulfur |
| 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 |
-
2009
- 2009-11-27 CN CN2009102346997A patent/CN101875485A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826515A (en) * | 2012-08-24 | 2012-12-19 | 江西恒兴源化工有限公司 | Method for preparing high-purity insoluble sulphur by using secondary purification method |
| CN104555943A (en) * | 2013-10-12 | 2015-04-29 | 江苏宏泰橡胶助剂有限公司 | Method for preparing high-quality insoluble sulphur from continuous pipelined overheated sulphur steam |
| CN106395757A (en) * | 2016-03-02 | 2017-02-15 | 赵水斌 | Fully-automatic continuous production method for insoluble sulfur |
| 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 |
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Open date: 20101103 |