CN103318848A - Production method of high-dispersion high-thermal-stability insoluble sulfur - Google Patents
Production method of high-dispersion high-thermal-stability insoluble sulfur Download PDFInfo
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- CN103318848A CN103318848A CN2013101946919A CN201310194691A CN103318848A CN 103318848 A CN103318848 A CN 103318848A CN 2013101946919 A CN2013101946919 A CN 2013101946919A CN 201310194691 A CN201310194691 A CN 201310194691A CN 103318848 A CN103318848 A CN 103318848A
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- insoluble sulfur
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- dithiocarbonic anhydride
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Abstract
The invention discloses a production method of high-dispersion high-thermal-stability insoluble sulfur. The method comprises the following steps: sulfur melting and heating: melting common sulfur at 145-155DEG C for sulfur melting, pumping the obtained melt to a heating tank, heating to 250-280DEG C, adding diethylhydroxylamine having a weight being 0.5-1% of the weight of sulfur, uniformly stirring, and heating to 490-550DEG C; and atomizing, quenching, curing, and cladding. The production method greatly improves the high-thermal-stability and the dispersibility of insoluble sulfur, and the insoluble sulfur obtained in the invention can completely satisfy the requirements of three-high insoluble sulfur by radial tires.
Description
Technical field
The present invention relates to a kind of production method of insoluble sulfur, relate in particular to a kind of production method of high dispersive high heat stability type insoluble sulfur.
Background technology
Insoluble sulfur has the character that is insoluble to dithiocarbonic anhydride, and formal name used at school is high molecular polymerization sulphur, is called for short lS.The oil-filled composition that wherein contains different amounts forms the IS-oil-filled type of series and non-oil-filled type product.
The technical process of producing insoluble sulfur is divided into substantially: sulfur melting intensification, chilling, curing, extraction, filtration, drying, screening, wherein the most key process procedure is chilling and curing, and both affect the high thermal stability of the finished product to a great extent.There is the dispersed not good problem not high with thermostability in the insoluble sulfur that prior art is produced.
Summary of the invention
The present invention provides a kind of production method of high dispersive high heat stability type insoluble sulfur in order to remedy the deficiencies in the prior art, and by present method, product high thermal stability and dispersiveness all have significantly raising.
The present invention is achieved by the following technical solutions.
The production method of high dispersive high heat stability type insoluble sulfur is characterized in that comprising the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 145-155 ℃; Melt is squeezed in the intensification tank, be warming up to 250-280 ℃, add the diethyl hydroxylamine that is equivalent to sulphur weight 0.5-1%, stir, then be warming up to 490-550 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur uniform liquid atomizing of atomizing nozzle with melting, then in the quenching synthesizer, fully contact with 0-5 ℃ dithiocarbonic anhydride from all directions, cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride rapidly;
(3) solidify, separate: dithiocarbonic anhydride liquid is heated to 40-50 ℃, stirred 40-60 minute, stop to stir, left standstill 1-2 hour, fish for filter residue, with dithiocarbonic anhydride washing 1-2 time, obtain insolubility sulphur again;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-0.8%, under 6000-7000 rev/min, stirred 30-45 minute, coat, described stablizer is mixed by the raw material of following weight part: benzoquinones 1-2, dimethyl silicone oil 3-4, ferrocene 1-2, glycerol glycerinate 1-2, nano silicon 1-2, sodium laurylsulfate 0.3-0.5;
(5) dry, oil-filled: negative pressure drying, obtain the insoluble sulfur powder, be distributed into finished product through screening, after oil-filled.
Advantage of the present invention:
1, sizing material no blooming within processing and staging life keeps sizing material component performance homogeneous, overcomes the shortcoming that causes the sizing material poor adhesion because of bloom, and prevents the pollution to rubber item and mould.
2, non-migratory phenomenon in adjacent glue-line keeps the sizing material surface viscosity.
3, mixing and deposit and reduce incipient scorch in the process.
4, shorten curing time, reduce sulfur consumption, be conducive to the improvement of rubber item aging resistance.
5, increase the bonding of rubber and other material.
6, the characteristic that has the high dispersive high heat stability, insoluble sulfur content remains on more than 55% under 120 ℃ * 15min condition.
Embodiment
The production method of high dispersive high heat stability type insoluble sulfur comprises the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 145-150 ℃; Melt is squeezed in the intensification tank, be warming up to 270-280 ℃, add the diethyl hydroxylamine that is equivalent to sulphur weight 0.5%, then the dispersion that stirs is warming up to 490-510 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur uniform liquid atomizing of atomizing nozzle with melting, then in the quenching synthesizer, fully contact with 0-5 ℃ dithiocarbonic anhydride liquid from all directions, cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride liquid rapidly;
(3) solidify, separate: dithiocarbonic anhydride liquid is heated to 40-50 ℃, stirred 40-60 minute, stop to stir, left standstill 2 hours, fish for filter residue, with dithiocarbonic anhydride washing 2 times, obtain insolubility sulphur again;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.8%, under 6000-7000 rev/min, stirred 30 minutes, coat, described stablizer is mixed by the raw material of following weight part: benzoquinones 1, dimethyl silicone oil 4, ferrocene 1, glycerol glycerinate 2, nano silicon 1, sodium laurylsulfate 0.3;
(5) dry, oil-filled: negative pressure drying, obtain the insoluble sulfur powder, be distributed into finished product through screening, after oil-filled.
After testing, finished product insoluble sulfur content is that the high thermal stability of 90.6%, 105 ℃/15min is that the high thermal stability of 81%, 120 ℃/15min is 55%.
Claims (1)
1. the production method of high dispersive high heat stability type insoluble sulfur is characterized in that comprising the steps:
(1) molten sulphur, intensification: sulphur is melted in common sulphur heating, and the control temperature is 145-155 ℃; Melt is squeezed in the intensification tank, be warming up to 250-280 ℃, add the diethyl hydroxylamine that is equivalent to sulphur weight 0.5-1%, stir, then be warming up to 490-550 ℃;
(2) atomizing, chilling: high pressure N2 is by the high temperature sulphur uniform liquid atomizing of atomizing nozzle with melting, then in the quenching synthesizer, fully contact with 0-5 ℃ dithiocarbonic anhydride from all directions, cooling forms uniform insoluble sulfur particle and is suspended in the dithiocarbonic anhydride rapidly;
(3) solidify, separate: dithiocarbonic anhydride liquid is heated to 40-50 ℃, stirred 40-60 minute, stop to stir, left standstill 1-2 hour, fish for filter residue, with dithiocarbonic anhydride washing 1-2 time, obtain insolubility sulphur again;
(4) coat: in the insoluble sulfur powder, add the stablizer that is equivalent to its weight 0.5%-0.8%, under 6000-7000 rev/min, stirred 30-45 minute, coat, described stablizer is mixed by the raw material of following weight part: benzoquinones 1-2, dimethyl silicone oil 3-4, ferrocene 1-2, glycerol glycerinate 1-2, nano silicon 1-2, sodium laurylsulfate 0.3-0.5;
(5) dry, oil-filled: negative pressure drying, obtain the insoluble sulfur powder, be distributed into finished product through screening, after oil-filled.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013101946919A CN103318848A (en) | 2013-05-23 | 2013-05-23 | Production method of high-dispersion high-thermal-stability insoluble sulfur |
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| CN2013101946919A CN103318848A (en) | 2013-05-23 | 2013-05-23 | Production method of high-dispersion high-thermal-stability insoluble sulfur |
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| CN103318848A true CN103318848A (en) | 2013-09-25 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724681A (en) * | 2015-03-18 | 2015-06-24 | 无锡华盛橡胶新材料科技股份有限公司 | Highly dispersed high-stability insoluble sulfur and preparation method thereof |
| CN105540552A (en) * | 2016-01-22 | 2016-05-04 | 上海京海（安徽）化工有限公司 | Preparation method of pressure-resisting sulphur with high bonding strength |
| 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 |
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 |
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2013
- 2013-05-23 CN CN2013101946919A patent/CN103318848A/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》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104724681A (en) * | 2015-03-18 | 2015-06-24 | 无锡华盛橡胶新材料科技股份有限公司 | Highly dispersed high-stability insoluble sulfur and preparation method thereof |
| CN105540552A (en) * | 2016-01-22 | 2016-05-04 | 上海京海（安徽）化工有限公司 | Preparation method of pressure-resisting sulphur with high bonding strength |
| 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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Application publication date: 20130925 |