CN107043091A - A kind of preparation technology of high stability insoluble sulfur - Google Patents
A kind of preparation technology of high stability insoluble sulfur Download PDFInfo
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- CN107043091A CN107043091A CN201710233545.0A CN201710233545A CN107043091A CN 107043091 A CN107043091 A CN 107043091A CN 201710233545 A CN201710233545 A CN 201710233545A CN 107043091 A CN107043091 A CN 107043091A
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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
- 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
- C01B17/0221—Melting
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Abstract
The present invention proposes a kind of preparation technology of high stability insoluble sulfur, first in proportion by industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides are added in sulfur melting kettle, compound stabilizer is added after heat temperature raising thereto, stirring reaction certain time is warming up to more than transition point again, promote the generation of insoluble type sulphur, then insoluble sulfur crude product is obtained by chilling, most afterwards through extract high content insoluble sulfur, insoluble sulfur high conversion rate made from preparation technology of the present invention, with high content, high temperature tolerance and high stability, and technique is easy, it is adapted to industrialized production.
Description
Technical field
The present invention relates to insoluble sulfur preparing technical field, and in particular to a kind of preparation of high stability insoluble sulfur
Technique.
Background technology
Insoluble sulfur (IS) is also known as polymerised sulphur, also known as μ types sulphur, refers to the sulphur insoluble in carbon disulfide, is the long-chain of sulphur
Polymer, with chemically and physically inertia, distributional stability is good in sizing material, and product vulcanization crosslinking point is uniform, with its vulcanization
Rubber has an optimal no blooming, and can effectively prevent sizing material occur early stage incipient scorch in process and promote rubber with
The bonding of steel wire or chemical fibre cord fabric thread, is the dedicated vulcanization agent of radial tyre production.It is right with the raising of tire meridian rate
The demand of high quality insoluble sulphur is also increased rapidly.It is external also there was only a few countries such as U.S., Germany, Russia, Japan etc.
It can produce.China will lean on a large amount of imports to meet demand every year.Therefore, the market prospects of domestic insoluble sulfur are seen very much
It is good.
The domestic and international method for preparing IS is divided from temperature mainly high temperature gasification and watery fusion method, from quenching medium again
Immersion method and solvent method can be divided into.The advantage that high temperature gasification prepares IS is that the content of IS in product is of a relatively high, is had the disadvantage
Whole course of reaction is under high-temperature and high-pressure conditions, and the requirement to consersion unit is harsher, and potential safety hazard is big in production process.
What the difference of watery fusion method and evaporating method was quenching is sulphur melt rather than overheat sulfur vapor, so with reaction temperature
Low, equipment corrosion is small, atmospheric operation, small investment, instant effect, operate it is comparatively safe the advantages of, but in product IS content it is relatively low.
Either evaporating method or fusion method, its key problem in technology are mainly the selection of stabilizer, chilling liquid and cooling mode
Determination, therefore develop a kind of rationally efficient stabilizer and preparation method is very necessary.
The content of the invention
For above-mentioned problem, the present invention proposes a kind of preparation technology of high stability insoluble sulfur, is made
Insoluble sulfur high conversion rate, with high content, high temperature tolerance and high stability, and technique is easy, is adapted to industrialized production.
In order to realize above-mentioned purpose, the present invention uses following technical scheme：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides are added in sulfur melting kettle in proportion, are warming up to
140-145 DEG C, Cosan quality 0.8-1.5% compound stabilizer, stirring reaction 1-1.2h, Ran Housheng are then added thereto
Temperature continues stirring reaction 1.5-1.8h to 230-240h；
2) molten reaction products in sulfur melting kettle are sent into be atomized with quenching medium in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product；
3) insoluble sulfur crude product is separated into drying, is crushed to particle diameter and is less than 0.05mm, then with extractant in mass ratio
1:12-14 be blended, 75 DEG C extract 1.8-2h, suction filtration it is dry high stability insoluble sulfur.
It is preferred that, sulphur mass fraction is more than 99% in the industrial sulphur powder.
It is preferred that, step 1) in the addition mass ratio of Cosan and double (diethyl sulfide phosphoryl) trisulfides be 35-40:
1。
It is preferred that, the compound stabilizer is the composition of halogen or halogen derivatives and gas-phase silica, wherein gas phase
White carbon accounts for the 85-90% of compound stabilizer gross mass.
It is preferred that, quenching medium is water, and temperature is 10-15 DEG C.
It is preferred that, contained insoluble sulfur mass fraction is more than 54.28% in insoluble sulfur crude product.
It is preferred that, drying temperature is 45 DEG C during the separation is dried, and drying time is 5h, and drying temperature is during suction filtration is dried
55 DEG C, drying time is 4-4.5h.
It is preferred that, the extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein to account for extractant total for tetrachloro-ethylene
The 65-70% of quality.
It is preferred that, contained insoluble sulfur mass fraction is more than 98.75% in high stability insoluble sulfur.
It is preferred that, the extractant is reclaimed Posterior circle and used using vacuum evaporation, condensation.
Due to using above-mentioned technical scheme, the beneficial effects of the invention are as follows：The present invention is using double (diethyl sulfide phosphinylidynes
Base) trisulfide, compound stabilizer collective effect, effectively increase stabilizer effect and the combination property of insoluble sulfur, because
Insoluble sulfur percent reduction reduces more than 25% caused by polymeric chain fracture, significantly improves the conversion ratio of insoluble sulfur,
And (diethyl sulfide phosphoryl) trisulfide as sulfur donor, can improve the high thermal stability of insoluble sulfur.The present invention
Insoluble sulfur high conversion rate made from preparation technology, with high content, high temperature tolerance and high stability, and technique is easy, fits
Close industrialized production.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described.Based on embodiments of the invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Embodiment 1：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 35:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
145 DEG C are warming up to, the compound stabilizer of Cosan quality 1.2% is then added thereto, stirring reaction 1.2h is then heated to
235h, continues stirring reaction 1.5h；Wherein compound stabilizer is the composition of KI and gas-phase silica, and gas-phase silica is accounted for
The 85% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 10 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 55.15% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:12 blendings, 1.5h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is done
The dry time is 4h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
99.36%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
68%.
Embodiment 2：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 36:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
145 DEG C are warming up to, the compound stabilizer of Cosan quality 1.5% is then added thereto, stirring reaction 1h is then heated to
235h, continues stirring reaction 1.5h；Wherein compound stabilizer is the composition of thionyl chloride and gas-phase silica, gas-phase silica
Account for the 85% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 10 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 54.63% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:13 blendings, 1.8h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is done
The dry time is 4.5h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur
For 98.87%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
65%.
Embodiment 3：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 40:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
140 DEG C are warming up to, the compound stabilizer of Cosan quality 1.5% is then added thereto, stirring reaction 1.1h is then heated to
230h, continues stirring reaction 1.5h；Wherein compound stabilizer is the composition of silicon tetrachloride and gas-phase silica, gas-phase silica
Account for the 90% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 15 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 54.28% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:14 blendings, 2h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is dried
Time is 4.5h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
98.75%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
67%.
Embodiment 4：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 38:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
140 DEG C are warming up to, the compound stabilizer of Cosan quality 1% is then added thereto, stirring reaction 1.1h is then heated to
230h, continues stirring reaction 1.8h；Wherein compound stabilizer is the composition of titanium tetrachloride and gas-phase silica, gas-phase silica
Account for the 90% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 15 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 54.85% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:14 blendings, 2h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is dried
Time is 4.5h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
99.14%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
65%.
Embodiment 5：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 35:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
142 DEG C are warming up to, the compound stabilizer of Cosan quality 0.8% is then added thereto, stirring reaction 1.2h is then heated to
235h, continues stirring reaction 1.6h；Wherein compound stabilizer is the composition of titanium tetrachloride and gas-phase silica, gas-phase silica
Account for the 90% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 15 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 55.3% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:14 blendings, 1.8h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is done
The dry time is 4h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
99.48%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
68%.
Embodiment 6：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 38:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
145 DEG C are warming up to, the compound stabilizer of Cosan quality 0.9% is then added thereto, stirring reaction 1h is then heated to
240h, continues stirring reaction 1.8h；Wherein compound stabilizer is the composition of thionyl chloride and gas-phase silica, gas-phase silica
Account for the 85% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 10 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 54.65% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:12 blendings, 1.8h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is done
The dry time is 4h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
98.88%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
70%.
Embodiment 7：
A kind of preparation technology of high stability insoluble sulfur, step is as follows：
1) in mass ratio 40:1 adds industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides in sulfur melting kettle,
142 DEG C are warming up to, the compound stabilizer of Cosan quality 1.2% is then added thereto, stirring reaction 1.2h is then heated to
240h, continues stirring reaction 1.6h；Wherein compound stabilizer is the composition of KI and gas-phase silica, and gas-phase silica is accounted for
The 85% of compound stabilizer gross mass；
2) molten reaction products in sulfur melting kettle are sent into be atomized with 10 DEG C of cold water in atomisation tower by spray gun and contacted, obtain insoluble
Property sulphur crude product, contained insoluble sulfur mass fraction is 55.21% in insoluble sulfur crude product；
3) insoluble sulfur crude product is separated into drying, drying temperature is 45 DEG C, and drying time is 5h, is crushed to particle diameter and is less than
0.05mm, then with extractant in mass ratio 1:12 blendings, 2h is extracted at 75 DEG C, and suction filtration is dried, and drying temperature is 55 DEG C, is dried
Time is 4.5h, obtains contained insoluble sulfur mass fraction in high stability insoluble sulfur, high stability insoluble sulfur and is
99.45%, wherein, extractant is the composition of carbon disulfide and tetrachloro-ethylene, and wherein tetrachloro-ethylene accounts for extractant gross mass
68%.
Product of the embodiment of the present invention is subjected to performance test, data are as follows：
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (10)
1. a kind of preparation technology of high stability insoluble sulfur, it is characterised in that step is as follows：
1) industrial Cosan, double (diethyl sulfide phosphoryl) trisulfides are added in sulfur melting kettle in proportion, is warming up to 140-
145 DEG C, Cosan quality 0.8-1.5% compound stabilizer is then added thereto, and stirring reaction 1-1.2h is then heated to
230-240h, continues stirring reaction 1.5-1.8h；
2) molten reaction products in sulfur melting kettle are sent into be atomized with quenching medium in atomisation tower by spray gun and contacted, obtain insoluble sulfur
Sulphur crude product；
3) insoluble sulfur crude product is separated into drying, particle diameter is crushed to less than 0.05mm, then with extractant in mass ratio 1:12-
14 blending, 75 DEG C extract 1.8-2h, suction filtration it is dry high stability insoluble sulfur.
2. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：The industrial sulphur
Sulphur mass fraction is more than 99% in powder.
3. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：Step 1) in sulphur
The addition mass ratio of powder and double (diethyl sulfide phosphoryl) trisulfides is 35-40:1.
4. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：The stable composition
Agent is the composition of halogen or halogen derivatives and gas-phase silica, and wherein gas-phase silica accounts for compound stabilizer gross mass
85-90%.
5. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：Quenching medium is
Water, temperature is 10-15 DEG C.
6. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：Insoluble sulfur is thick
Contained insoluble sulfur mass fraction is more than 54.28% in product.
7. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：The separation drying
Middle drying temperature is 45 DEG C, and drying time is 5h, and drying temperature is 55 DEG C during suction filtration is dried, and drying time is 4-4.5h.
8. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：The extractant is
The composition of carbon disulfide and tetrachloro-ethylene, wherein tetrachloro-ethylene account for the 65-70% of extractant gross mass.
9. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：High stability is insoluble
Property sulphur in contained insoluble sulfur mass fraction be more than 98.75%.
10. the preparation technology of high stability insoluble sulfur according to claim 1, it is characterised in that：The extractant
Used using being evaporated in vacuo, condensing recovery Posterior circle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661120A (en) * | 2020-12-17 | 2021-04-16 | 淮北师范大学 | Method and process for preparing insoluble sulfur from coking desulfurization waste residues |
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| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| CN104724680A (en) * | 2015-03-17 | 2015-06-24 | 中国石油化工股份有限公司 | Insoluble sulfur, preparation method thereof, oil-charged insoluble sulfur, application of oil-charged insoluble sulfur and application of ionic liquid as stabilizer |
| CN105694095A (en) * | 2016-01-22 | 2016-06-22 | 上海京海（安徽）化工有限公司 | High-quality and wear-resisting insoluble sulfur for rubber and production process of high-quality and wear-resisting insoluble sulfur |
| CN105752941A (en) * | 2016-01-22 | 2016-07-13 | 上海京海（安徽）化工有限公司 | Method for preparing high-purity and high-dispersibility insoluble sulfur |
-
2017
- 2017-04-11 CN CN201710233545.0A patent/CN107043091A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424247A (en) * | 2002-12-25 | 2003-06-18 | 南化集团研究院 | Insoluble sulfur preparation |
| CN104724680A (en) * | 2015-03-17 | 2015-06-24 | 中国石油化工股份有限公司 | Insoluble sulfur, preparation method thereof, oil-charged insoluble sulfur, application of oil-charged insoluble sulfur and application of ionic liquid as stabilizer |
| CN105694095A (en) * | 2016-01-22 | 2016-06-22 | 上海京海（安徽）化工有限公司 | High-quality and wear-resisting insoluble sulfur for rubber and production process of high-quality and wear-resisting insoluble sulfur |
| CN105752941A (en) * | 2016-01-22 | 2016-07-13 | 上海京海（安徽）化工有限公司 | Method for preparing high-purity and high-dispersibility insoluble sulfur |
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| 华南理工大学等合编 张海等主编: "《橡胶及塑料加工工艺》", 30 November 1997 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661120A (en) * | 2020-12-17 | 2021-04-16 | 淮北师范大学 | Method and process for preparing insoluble sulfur from coking desulfurization waste residues |
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