CN103204478A - Production method for high-stability insoluble sulfur - Google Patents
Production method for high-stability insoluble sulfur Download PDFInfo
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- CN103204478A CN103204478A CN2013100940154A CN201310094015A CN103204478A CN 103204478 A CN103204478 A CN 103204478A CN 2013100940154 A CN2013100940154 A CN 2013100940154A CN 201310094015 A CN201310094015 A CN 201310094015A CN 103204478 A CN103204478 A CN 103204478A
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Abstract
The invention discloses a production method for high-stability insoluble sulfur. The production method includes heating common sulfur to be melted, and controlling the temperature at 130-145 DEG C, pushing the melt into a temperature raising tank by a sulfur metering pump, raising the temperature automatically and controlling the temperature at 370-450 DEG C, atomizing, quenching, solidifying and coating the melt and the like. By the production method, product yield, high thermal stability and dispersibility are greatly improved, and finished products can fully meet the requirements of radial tires on insoluble sulfur with high content, high thermal stability and high dispersibility.
Description
Technical field
The present invention relates to a kind of Manufacture of insoluble sulphur method, relate in particular to a kind of high stability Manufacture of insoluble sulphur method.
Background technology
Insoluble sulfur is a kind of allotropic substance of common sulphur, it is the linear polymeric that is polymerized by a large amount of sulphur atoms, be insoluble to dithiocarbonic anhydride, also be insoluble to rubber, so be referred to as insoluble sulfur or polymerization sulphur, formal name used at school is high molecular polymerization sulphur (English name is INSOLUBIESULFUR, is called for short IS), and it is widely used in the manufacturing of rubber items such as tire mainly as a kind of vulcanizing agent of rubber industry.Existing insoluble sulfur is dispersed bad in Rubber processing, causes the rubber vulcanization heterogeneity easily, influences the processing characteristics of sizing material, thereby influences the performance of rubber item.
Summary of the invention
The present invention provides a kind of high stability Manufacture of insoluble sulphur method in order to remedy the deficiencies in the prior art, and by present method, product yield, high thermal stability and dispersiveness all have significantly raising.
The present invention is achieved by the following technical solutions.
A kind of high stability Manufacture of insoluble sulphur method is characterized in that comprising the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 130-145 ℃; Melt with the sulphur volume pump squeeze into heat up jar in, heat up automatically and control temperature at 370 ℃-450 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 30-35 ℃ dithiocarbonic anhydride liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride liquid;
(3) solidify, extract, separate: mixed dithiocarbonic anhydride suspension liquid enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-60 ℃, and be 1-2h set time; Filter filter residue and obtain insolubility sulphur;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-1.0%, under 3000-4000 rev/min, stirred 10-15 minute, coat, described stablizer is mixed by the raw material of following weight part: 2.4.6-three (dimethylamino methyl) phenol 1-2, benzene 10-12, emulsifier BP 2-3, petroleum sodium sulfonate 1-2, ferrocene 1-2, nano-attapulgite powder 0.1-0.2, linking agent TAC 1-2
,Pentanoic 1-2, oxidation inhibitor 1035 0.1-0.2;
(5) drying: negative pressure drying obtains fineness 150-200 purpose insoluble sulfur powder;
(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.
Production method of the present invention, product yield, high thermal stability and dispersiveness all have significantly raising.
Embodiment
A kind of high stability Manufacture of insoluble sulphur method is characterized in that comprising the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur 500 gram heating, and the control temperature is 140-145 ℃; Melt with the sulphur volume pump squeeze into heat up jar in, heat up automatically and control temperature at 390 ℃-430 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 30-35 ℃ dithiocarbonic anhydride liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride liquid;
(3) solidify, extract, separate: mixed dithiocarbonic anhydride suspension liquid enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-50 ℃, and be 2h set time; Filter filter residue and obtain insolubility sulphur 238 grams;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%, under 3000-3500 rev/min, stirred 15 minutes, coat, described stablizer is mixed by the raw material of following weight part: 2.4.6-three (dimethylamino methyl) phenol 2, benzene 12, emulsifier BP 3, petroleum sodium sulfonate 1, ferrocene 1, nano-attapulgite powder 0.2, linking agent TAC 1
,Pentanoic 1, oxidation inhibitor 1,035 0.2;
(5) drying: negative pressure drying obtains fineness 150-200 purpose insoluble sulfur powder;
(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.
After testing, finished product insoluble sulfur content is that the high thermal stability of 90.2%, 105 ℃/15min is that the high thermal stability of 80%, 120 ℃/15min is 51%.
Claims (1)
1. a high stability Manufacture of insoluble sulphur method is characterized in that comprising the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 130-145 ℃; Melt with the sulphur volume pump squeeze into heat up jar in, heat up automatically and control temperature at 370 ℃-450 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur liquid uniform atomizing of atomizing nozzle with fusion, in the quenching synthesizer, fully contact with 30-35 ℃ dithiocarbonic anhydride liquid from all directions then, quick cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride liquid;
(3) solidify, extract, separate: mixed dithiocarbonic anhydride suspension liquid enters in the reactor that has whipping appts, and insoluble sulfur is cured in device, and solidification value is 40-60 ℃, and be 1-2h set time; Filter filter residue and obtain insolubility sulphur;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-1.0%, under 3000-4000 rev/min, stirred 10-15 minute, coat, described stablizer is mixed by the raw material of following weight part: 2.4.6-three (dimethylamino methyl) phenol 1-2, benzene 10-12, emulsifier BP 2-3, petroleum sodium sulfonate 1-2, ferrocene 1-2, nano-attapulgite powder 0.1-0.2, linking agent TAC 1-2
,Pentanoic 1-2, oxidation inhibitor 1035 0.1-0.2;
(5) drying: negative pressure drying obtains fineness 150-200 purpose insoluble sulfur powder;
(6) screening, oil-filled: the insoluble sulfur powder is through screening, be distributed into finished product after oil-filled.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2013100940154A CN103204478A (en) | 2013-03-22 | 2013-03-22 | Production method for high-stability insoluble sulfur |
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| CN2013100940154A CN103204478A (en) | 2013-03-22 | 2013-03-22 | Production method for high-stability insoluble sulfur |
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| CN103204478A true CN103204478A (en) | 2013-07-17 |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539078A (en) * | 2013-10-25 | 2014-01-29 | 北京化工大学 | Method for preparation of insoluble sulfur |
| CN104401945A (en) * | 2014-10-20 | 2015-03-11 | 江西恒兴源化工有限公司 | High-temperature molten sulfur porous spraying type chilling quenching method |
| CN104787728A (en) * | 2015-03-10 | 2015-07-22 | 长春帝博科技有限公司 | Soluble polymerized sulphur production process and equipment |
| CN105037803A (en) * | 2015-06-06 | 2015-11-11 | 青岛科技大学 | Preparation method of composite double-layer-film coated sulfur microcapsule |
| CN105502303A (en) * | 2016-01-22 | 2016-04-20 | 上海京海（安徽）化工有限公司 | Production process for preparing insoluble sulfur high in thermal stability and content |
| CN108439348A (en) * | 2018-04-21 | 2018-08-24 | 河南省开仑化工有限责任公司 | A kind of insoluble sulfur production method |
| CN113120868A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur production method and 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730648A (en) * | 2012-07-03 | 2012-10-17 | 山东尚舜化工有限公司 | Production method of high-quality insoluble sulfur |
-
2013
- 2013-03-22 CN CN2013100940154A patent/CN103204478A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102730648A (en) * | 2012-07-03 | 2012-10-17 | 山东尚舜化工有限公司 | Production method of high-quality insoluble sulfur |
Non-Patent Citations (1)
| Title |
|---|
| 李双文: "不溶性硫磺的研究和开发进展", 《精细化工原料及中间体》, no. 3, 31 December 2010 (2010-12-31), pages 19 - 23 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539078A (en) * | 2013-10-25 | 2014-01-29 | 北京化工大学 | Method for preparation of insoluble sulfur |
| CN103539078B (en) * | 2013-10-25 | 2015-07-08 | 北京化工大学 | Method for preparation of insoluble sulfur |
| CN104401945A (en) * | 2014-10-20 | 2015-03-11 | 江西恒兴源化工有限公司 | High-temperature molten sulfur porous spraying type chilling quenching method |
| CN104787728A (en) * | 2015-03-10 | 2015-07-22 | 长春帝博科技有限公司 | Soluble polymerized sulphur production process and equipment |
| CN105037803A (en) * | 2015-06-06 | 2015-11-11 | 青岛科技大学 | Preparation method of composite double-layer-film coated sulfur microcapsule |
| CN105037803B (en) * | 2015-06-06 | 2018-04-20 | 青岛科技大学 | A kind of preparation method of compound double membrane cladding sulfur microcapsule |
| CN105502303A (en) * | 2016-01-22 | 2016-04-20 | 上海京海（安徽）化工有限公司 | Production process for preparing insoluble sulfur high in thermal stability and content |
| CN108439348A (en) * | 2018-04-21 | 2018-08-24 | 河南省开仑化工有限责任公司 | A kind of insoluble sulfur production method |
| CN113120868A (en) * | 2019-12-31 | 2021-07-16 | 中国石油化工股份有限公司 | Insoluble sulfur production method and 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 |
| 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 |
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Application publication date: 20130717 |
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