CN105502301B - A kind of extracting method of sulfur waste sulphur cycling and reutilization - Google Patents
A kind of extracting method of sulfur waste sulphur cycling and reutilization Download PDFInfo
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- CN105502301B CN105502301B CN201511022813.1A CN201511022813A CN105502301B CN 105502301 B CN105502301 B CN 105502301B CN 201511022813 A CN201511022813 A CN 201511022813A CN 105502301 B CN105502301 B CN 105502301B
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- sulphur
- sulfur waste
- cycling
- extracting method
- reutilization
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000005864 Sulphur Substances 0.000 title claims abstract description 77
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 48
- 239000011593 sulfur Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000002699 waste material Substances 0.000 title claims abstract description 44
- 230000001351 cycling effect Effects 0.000 title claims abstract description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012043 crude product Substances 0.000 claims abstract description 11
- 239000012452 mother liquor Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000007725 thermal activation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 11
- 230000006872 improvement Effects 0.000 description 8
- 239000007787 solid Substances 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 239000004570 mortar (masonry) Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000005586 Nicosulfuron Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- RTCOGUMHFFWOJV-UHFFFAOYSA-N nicosulfuron Chemical compound COC1=CC(OC)=NC(NC(=O)NS(=O)(=O)C=2C(=CC=CN=2)C(=O)N(C)C)=N1 RTCOGUMHFFWOJV-UHFFFAOYSA-N 0.000 description 3
- 238000000605 extraction Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002910 solid waste Substances 0.000 description 2
- 206010054949 Metaplasia Diseases 0.000 description 1
- 229940100389 Sulfonylurea Drugs 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- PXQLVRUNWNTZOS-UHFFFAOYSA-N sulfanyl Chemical class [SH] PXQLVRUNWNTZOS-UHFFFAOYSA-N 0.000 description 1
- YROXIXLRRCOBKF-UHFFFAOYSA-N sulfonylurea Chemical class OC(=N)N=S(=O)=O YROXIXLRRCOBKF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01B17/027—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur
- C01B17/033—Recovery of sulfur from material containing elemental sulfur, e.g. luxmasses or sulfur containing ores; Purification of the recovered sulfur using a liquid extractant
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprises the following steps：(1) sulfur waste sulphur crude product is added into organic solvent, filtering and impurity removing by fully crushing；(2) it will filter out the sulphur come and add sig water dissolving, add activated carbon to be decolourized, filter to obtain mother liquor；(3) it is mother liquid obtained to use acid for adjusting pH value, filtering；(4) by sulphur heat-activated obtained by upper step, the sulphur that can be recycled is produced；The beneficial effects of the invention are as follows：The extracting method technological reaction is simple, and operational control is easy, and production cost is low, and yield is high, effectively solves the bad processing of sulfur waste sulphur and environmental issue, belongs to efficient emission-reducing Green Manufacturing Technology, gained sulphur can cycling and reutilization, suitable for industrialized production.
Description
Technical field
The present invention relates to a kind of sulfur waste sulphur extracting method, is specifically related to a kind of extraction side of sulfur waste sulphur cycling and reutilization
Method.
Background technology
Caused sulfur waste sulphur in sulfhydrylation process, khaki solid, the hazardous chemical solid waste of bad processing, production
The chemical equation of raw sulfur waste sulphur is as follows：
In existing sulfonylurea nicosulfuron active compound synthetic technology, the sulfur waste sulphur in sulfhydrylation technique is always as danger
Fixed-end forces, with the continuous increase of Environmental Protection in China pressure in recent years, it is impossible to meet environmental protection for the conventional treatment of the solid waste
It is required that.
China Patent Publication No. CN91111804.7, publication date on June 30th, 1993, a kind of entitled sulphur of innovation and creation
The method of purification of sulphur, this application specifically disclose a kind of method of purification of sulphur, by material containing sulphur be placed in 115-445 DEG C plus
In hot device, the mixed gas that vapor is instantly available sulphur and water is passed through, then cools down the mixed gas, the sulphur of precipitation is washed with water
Wash, dry, obtain high-quality sulphur.It is disadvantageous in that：This method is high using heater heating-up temperature, complex process and danger
Dangerous height, equipment investment and maintenance cost are higher；The processing that big chemical industry produces sulfur waste sulphur is only applicable to, is not suitable for the chemical industry that becomes more meticulous
The processing of sulfur waste sulphur.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of extracting method of sulfur waste sulphur cycling and reutilization, the preparation
Method effectively solves that sulphur extraction process is complicated, dangerous high, and equipment investment and maintenance cost are higher etc. above-mentioned existing asks
Topic.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprise the following steps：
(1) sulfur waste sulphur crude product is added into organic solvent, filtering and impurity removing by fully crushing；
(2) it will filter out the sulphur come and add sig water dissolving, add activated carbon to be decolourized, filter to obtain mother liquor；
(3) it is mother liquid obtained to use acid for adjusting pH value, filtering；
(4) by sulphur heat-activated obtained by upper step, the sulphur that can be recycled is produced.
The present invention further improvement is that：Sulfur waste sulphur fineness in step (1) after crushed is 100~300 mesh.
The present invention further improvement is that：The organic solvent includes：Ethyl acetate, dichloromethane, chloroform, methanol.
The present invention further improvement is that：The sig water includes：Dilute sodium hydroxide aqueous solution, the dilute sodium carbonate aqueous solution,
Dilute wet chemical.
The present invention further improvement is that：Weight ratio：The ︰ (0.010~0.1) of sulfur waste sulphur Cu Pin ︰ activated carbons=1.
The present invention further improvement is that：Acid includes described in step (3)：Concentrated hydrochloric acid, the concentrated sulfuric acid, glacial acetic acid.
The present invention further improvement is that：The temperature range of the sulphur heat-activated is 50 DEG C~100 DEG C；Time range
For 60~120 minutes.
The present invention further improvement is that：The sulfur waste sulphur crude product selects caused sulfur waste sulphur crude product in sulfhydrylation process.
The beneficial effects of the invention are as follows：The extracting method of this kind of sulfur waste sulphur cycling and reutilization, nicosulfuron active compound can be closed
Caused sulfur waste sulphur in sulfhydrylation process in carries out cycling and reutilization, belongs to green production process.At this method
Sulphur is extracted after reason to carry out mercaptolation without influenceing the process recovery ratio as raw material again.
Present invention process reaction is simple, and operational control is easy, and production cost is low, and yield is high, and it is bad effectively to solve sulfur waste sulphur
Processing and environmental issue, belong to efficient emission-reducing Green Manufacturing Technology, gained sulphur can cycling and reutilization, suitable for industrial metaplasia
Production.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, further
Illustrate the present invention.
Embodiment one：
A kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprise the following steps：
(1) caused sulfur waste sulphur crude product 30g in the sulfhydrylation process that outward appearance is khaki, content is 86%, will with mortar
It pulverizes into powder (100 mesh), adds 80mL ethyl acetate at ambient temperature, stirs 2 hours, filtering and impurity removing.
(2) it will filter out the solid sulfur come to be dissolved in 80mL 10% dilute sodium hydroxide aqueous solution, add activity
Charcoal 3.0g, after being stirred at room temperature 60 minutes, activated carbon is filtered to remove, the mother liquor color after decolouring is shallower, is faint yellow.
(3) mother liquor is adjusted into pH value to 5.8 with 35% concentrated hydrochloric acid, filtered.
(4) after the sulphur filtered out being heated into 50 DEG C of activation 120 minutes, flaxen sulphur 25g is obtained, content 95%,
Yield 92.0%.
Embodiment two：
A kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprise the following steps：
(1) caused sulfur waste sulphur crude product 30g in the sulfhydrylation process that outward appearance is khaki, content is 85%, will with mortar
It pulverizes into powder (170 mesh), adds 80mL dichloromethane at ambient temperature, stirs 2 hours, filtering and impurity removing.
(2) it will filter out the solid sulfur come to be dissolved in the 80mL 10% dilute sodium carbonate aqueous solution, add activated carbon
1.0g, after being stirred at room temperature 60 minutes, activated carbon is filtered to remove, the mother liquor color after decolouring is shallower, is faint yellow.
(3) mother liquor is adjusted into pH value to 5.9 with 35% concentrated hydrochloric acid, filtered.
(4) after the sulphur filtered out being heated into 65 DEG C of activation 100 minutes, flaxen sulphur 24g is obtained, content 95%,
Yield 89.4%.
Embodiment three：
A kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprise the following steps：
(1) caused sulfur waste sulphur crude product 30g in the sulfhydrylation process that outward appearance is khaki, content is 86%, will with mortar
It pulverizes into powder (240 mesh), adds 80mL chloroforms at ambient temperature, stirs 2 hours, filtering and impurity removing.
(2) it will filter out the solid sulfur come to be dissolved in 80mL 10% dilute wet chemical, add activated carbon
0.5g, after being stirred at room temperature 60 minutes, activated carbon is filtered to remove, the mother liquor color after decolouring is shallower, is faint yellow.
(3) mother liquor is adjusted into pH value to 6 with 35% concentrated sulfuric acid, filtered.
(4) by the sulphur filtered out be heated to 85 DEG C activation 80 minutes after, obtain flaxen sulphur 26g, content 96%, obtain
Rate 96.7%.
Embodiment four：
A kind of extracting method of sulfur waste sulphur cycling and reutilization, the method for purification comprise the following steps：
(1) caused sulfur waste sulphur crude product 30g in the sulfhydrylation process that outward appearance is khaki, content is 86%, will with mortar
It pulverizes into powder (300 mesh), adds 80mL methanol at ambient temperature, stirs 2 hours, filtering and impurity removing.
(2) it will filter out the solid sulfur come to be dissolved in 80mL 10% dilute sodium hydroxide, add activated carbon 0.3g,
After being stirred at room temperature 60 minutes, activated carbon is filtered to remove, the mother liquor color after decolouring is shallower, is faint yellow.
(3) mother liquor is adjusted into pH value to 6.1 with 20% glacial acetic acid, filtered.
(4) after the sulphur filtered out being heated into 100 DEG C of activation 60 minutes, flaxen sulphur 26g is obtained, content 95%,
Yield 95.7%.
The invention provides a kind of extracting method of sulfur waste sulphur cycling and reutilization, sulphur is extracted after this method is handled
Mercaptolation can be carried out without influenceing the process recovery ratio as raw material again.And technological reaction is simple, operational control is easy,
Production cost is low, and yield is high, effectively solves the bad processing of sulfur waste sulphur and environmental issue, the mercapto during can nicosulfuron active compound be synthesized
Caused sulfur waste sulphur in base chemical industry sequence carries out cycling and reutilization, belongs to efficient emission-reducing Green Manufacturing Technology, gained sulphur can
Cycling and reutilization, suitable for industrialized production.
The basic principles, principal features and advantages of the present invention have been shown and described above.The technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes and improvements
It all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its equivalent circle
It is fixed.
Claims (7)
- A kind of 1. extracting method of sulfur waste sulphur cycling and reutilization, it is characterised in that：The method of purification comprises the following steps：(1) sulfur waste sulphur crude product is added into organic solvent, filtering and impurity removing, the sulfur waste sulphur crude product selects sulfydryl by fully crushing Caused sulfur waste sulphur crude product in chemical industry sequence；(2) it will filter out the sulphur come and add sig water dissolving, add activated carbon to be decolourized, filter to obtain mother liquor；(3) it is mother liquid obtained to use acid for adjusting pH value, filtering；(4) by sulphur heat-activated obtained by upper step, the sulphur that can be recycled is produced.
- A kind of 2. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：In step (1) Sulfur waste sulphur fineness after crushed is 100~300 mesh.
- A kind of 3. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：It is described organic molten Agent includes：Ethyl acetate, dichloromethane, chloroform, methanol.
- A kind of 4. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：The sig water Including：Dilute sodium hydroxide aqueous solution, the dilute sodium carbonate aqueous solution, dilute wet chemical.
- A kind of 5. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：Weight ratio：It is useless The ︰ (0.010~0.1) of sulphur Cu Pin ︰ activated carbons=1.
- A kind of 6. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：In step (3) The acid includes：Concentrated hydrochloric acid, the concentrated sulfuric acid, glacial acetic acid.
- A kind of 7. extracting method of sulfur waste sulphur cycling and reutilization according to claim 1, it is characterised in that：The sulphur adds The temperature range of thermal activation is 50 DEG C~100 DEG C；Time range is 60~120 minutes.
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| CN201511022813.1A CN105502301B (en) | 2015-12-30 | 2015-12-30 | A kind of extracting method of sulfur waste sulphur cycling and reutilization |
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|---|---|---|---|
| CN201511022813.1A CN105502301B (en) | 2015-12-30 | 2015-12-30 | A kind of extracting method of sulfur waste sulphur cycling and reutilization |
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| CN105502301A CN105502301A (en) | 2016-04-20 |
| CN105502301B true CN105502301B (en) | 2017-12-12 |
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| CN114477098A (en) * | 2021-12-17 | 2022-05-13 | 湖南道安环保科技有限公司 | Purification process of byproduct sulfur in HPF (high pressure fluidized bed) desulfurization |
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| CN101618860A (en) * | 2009-08-06 | 2010-01-06 | 湖南科技大学 | Method for extracting sulfur in sulfur-contained slag by chlorohydrocarbon organic solvent |
| CN104229745A (en) * | 2014-09-01 | 2014-12-24 | 株洲起源科技有限责任公司 | Ultrasonic extraction method and process for processing slag containing elemental sulfur |
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