CN102502521A - Preparation method for sulfur micro-emulsion - Google Patents

Preparation method for sulfur micro-emulsion Download PDF

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Publication number
CN102502521A
CN102502521A CN2011103404681A CN201110340468A CN102502521A CN 102502521 A CN102502521 A CN 102502521A CN 2011103404681 A CN2011103404681 A CN 2011103404681A CN 201110340468 A CN201110340468 A CN 201110340468A CN 102502521 A CN102502521 A CN 102502521A
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China
Prior art keywords
sulfur
sulphur
microemulsion
solvent
preparation
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Pending
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CN2011103404681A
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Chinese (zh)
Inventor
夏新兴
张克娟
崔丽娟
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Priority to CN2011103404681A priority Critical patent/CN102502521A/en
Publication of CN102502521A publication Critical patent/CN102502521A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a preparation method for a sulfur microemulsion, which comprises the following steps: evenly mixing tetrahydronaphthalene with an anthracene solvent in the weight ratio of (20-80):1 in a reaction kettle; adding sulfur while stirring is performed; stirring for 5-60 minutes under controlling the temperature to be 20-90 DEG C; and then, removing the undissolved sulfur to obtain the sulfur microemulsion, wherein the maximum dissolvability of the sulfur reaches 19.11g in every 100g of solvent. According to the preparation method for the sulfur microemulsion, very good dissolving power can be performed on the sulfur under the required temperature after the tetrahydronaphthalene and the anthracene solvent are mixed; the dissolvability of the sulfur microemulsion on the sulfur exceeds that of all industrial sulfur solvents on the sulfur except for carbon disulfide, but the toxicity of the sulfur microemulsion is far lower than that of the carbon disulfide and all the industrial sulfur solvents.

Description

A kind of sulphur preparation of microemulsion method
Technical field
The invention belongs to rubber industry and paper industry field, be specifically related to a kind of sulphur preparation of microemulsion method.
Background technology
The rubber sheet gasketing of producing with paper process is applied in industry, various fields of recent life; Its basic procedure is to be medium with water, in water, disperses fibrous material, adds filler breast, vulcanizing agent, filler etc. then; The moulding of on the paper machine, manufacturing paper with pulp is again through high temperature vulcanized process.Sulphur plays an important role to performance of products as main vulcanizing agent.In the process of manufacturing paper with pulp, sulphur is because of water insoluble easy loss, and the particle Sulfur is difficult in paper, form uniform distribution, through the sulphur microemulsion is processed in sulphur dissolving, emulsification, can improve the cure efficiency and the quality product of product.Dithiocarbonic anhydride is acknowledged as the optimum solvent of sulphur, but shortcomings such as dithiocarbonic anhydride is volatile, inflammable, explosive, strong toxicity are brought a series of safety and environmental protection problems to industrial production.The industrial sulphur solvent that exploitation in recent years is used for alternative dithiocarbonic anhydride has zellon, tetracol phenixin, toluene and various double solventss etc.Though these solvent toxicity are lower than dithiocarbonic anhydride,, can not satisfy sealing material far away to the deliquescent requirement of sulphur to the dissolving power of the too late dithiocarbonic anhydride of the dissolving power of sulphur to sulphur.
Summary of the invention
The object of the present invention is to provide that a kind of toxicity is low, boiling point is high, not volatile, big sulphur preparation of microemulsion method to sulphur solubleness.
For achieving the above object; The technical scheme that the present invention adopts is: in reaction kettle with naphthane with fear solvent with mass ratio 20-80: 1 mixes; Add Sulfur while stirring, controlled temperature 20 ℃-90 ℃, stir the 5-60min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion.
Prepared sulphur microemulsion reaches the 19.11g/100g solvent to the sulphur maxima solubility.
The present invention has good dissolving power to sulphur with naphthane with after fearing mixing under the temperature that requires; The solubleness of sulphur is surpassed except that dithiocarbonic anhydride all industrial sulphur solvents to the solubleness of sulphur, but toxicity is far below dithiocarbonic anhydride and various sulphur industrial solvent.
Embodiment
Embodiment 1: in reaction kettle with naphthane with fear solvent and mix at 50: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 30 ℃, stir the 50min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 2: in reaction kettle with naphthane with fear solvent and mix at 30: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 80 ℃, stir the 5min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 3: in reaction kettle with naphthane with fear solvent and mix at 70: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 40 ℃, stir the 30min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 4: in reaction kettle with naphthane with fear solvent and mix at 20: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 50 ℃, stir the 20min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 5: in reaction kettle with naphthane with fear solvent and mix at 80: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 20 ℃, stir the 60min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 6: in reaction kettle with naphthane with fear solvent and mix at 60: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 60 ℃, stir the 40min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.
Embodiment 7: in reaction kettle with naphthane with fear solvent and mix at 40: 1 with mass ratio; Add Sulfur while stirring; Controlled temperature 70 ℃, stir the 10min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion, through detecting to such an extent that the solubleness of sulphur reaches the 19.11g/100g solvent.

Claims (2)

1. sulphur preparation of microemulsion method; It is characterized in that: in reaction kettle with naphthane with fear solvent with mass ratio 20-80: 1 mixes; Add Sulfur while stirring, controlled temperature 20 ℃-90 ℃, stir the 5-60min after-filtration and remove undissolved sulphur and obtain the sulphur microemulsion.
2. sulphur preparation of microemulsion method as claimed in claim 1, it is characterized in that: prepared sulphur microemulsion reaches the 19.11g/100g solvent to the sulphur maxima solubility.
CN2011103404681A 2011-11-02 2011-11-02 Preparation method for sulfur micro-emulsion Pending CN102502521A (en)

Priority Applications (1)

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CN2011103404681A CN102502521A (en) 2011-11-02 2011-11-02 Preparation method for sulfur micro-emulsion

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CN2011103404681A CN102502521A (en) 2011-11-02 2011-11-02 Preparation method for sulfur micro-emulsion

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CN102502521A true CN102502521A (en) 2012-06-20

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109835873A (en) * 2019-03-27 2019-06-04 淮北师范大学 The device and method for producing sulphur from sulfur-bearing waste residue
CN110835097A (en) * 2019-11-21 2020-02-25 太原科技大学 High-yield nano-sulfur particle microemulsion preparation method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1143652A (en) * 1995-08-21 1997-02-26 四川联合大学 Method for preparing polyarylene sulfide with high molecular and high toughness
CN1424247A (en) * 2002-12-25 2003-06-18 南化集团研究院 Insoluble sulfur preparation
EP1338557A1 (en) * 2000-10-18 2003-08-27 Jgc Corporation Method and apparatus for removing sulfur compound in gas containing hydrogen sulfide, mercaptan, carbon dioxide and aromatic hydrocarbon
CN101337659A (en) * 2007-07-04 2009-01-07 中国石油天然气股份有限公司 Process for extracting insoluble sulfur

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1143652A (en) * 1995-08-21 1997-02-26 四川联合大学 Method for preparing polyarylene sulfide with high molecular and high toughness
EP1338557A1 (en) * 2000-10-18 2003-08-27 Jgc Corporation Method and apparatus for removing sulfur compound in gas containing hydrogen sulfide, mercaptan, carbon dioxide and aromatic hydrocarbon
CN1424247A (en) * 2002-12-25 2003-06-18 南化集团研究院 Insoluble sulfur preparation
CN101337659A (en) * 2007-07-04 2009-01-07 中国石油天然气股份有限公司 Process for extracting insoluble sulfur

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《现代化工》 20110630 张克娟 等 "四氢萘/甲苯混合溶剂中硫璜的溶解特性" 第253-256页 1-2 第31卷, *
张克娟 等: ""四氢萘/甲苯混合溶剂中硫璜的溶解特性"", 《现代化工》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109835873A (en) * 2019-03-27 2019-06-04 淮北师范大学 The device and method for producing sulphur from sulfur-bearing waste residue
CN110835097A (en) * 2019-11-21 2020-02-25 太原科技大学 High-yield nano-sulfur particle microemulsion preparation method

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Application publication date: 20120620