CN106829876B - The recoverying and utilizing method of oil plant sulfur removal plant sulphur steam - Google Patents
The recoverying and utilizing method of oil plant sulfur removal plant sulphur steam Download PDFInfo
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- CN106829876B CN106829876B CN201710120959.2A CN201710120959A CN106829876B CN 106829876 B CN106829876 B CN 106829876B CN 201710120959 A CN201710120959 A CN 201710120959A CN 106829876 B CN106829876 B CN 106829876B
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- sulfur
- carbon disulfide
- sulphur steam
- oil
- recoverying
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- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 167
- 239000011593 sulfur Substances 0.000 title claims abstract description 100
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 100
- 239000005864 Sulphur Substances 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 28
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims abstract description 100
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 54
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000007789 gas Substances 0.000 claims abstract description 42
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 claims abstract description 29
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims abstract description 27
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 238000011084 recovery Methods 0.000 claims abstract description 15
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 13
- QGJOPFRUJISHPQ-NJFSPNSNSA-N carbon disulfide-14c Chemical compound S=[14C]=S QGJOPFRUJISHPQ-NJFSPNSNSA-N 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000008246 gaseous mixture Substances 0.000 claims abstract description 9
- XDAHMMVFVQFOIY-UHFFFAOYSA-N methanedithione;sulfane Chemical compound S.S=C=S XDAHMMVFVQFOIY-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002918 waste heat Substances 0.000 claims abstract description 5
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 34
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 21
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 18
- 239000003381 stabilizer Substances 0.000 claims description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 12
- 239000000126 substance Substances 0.000 claims description 12
- 239000000920 calcium hydroxide Substances 0.000 claims description 10
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 7
- -1 N- cyclohexyl sulfo-amino Chemical group 0.000 claims description 7
- 239000001569 carbon dioxide Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- STRTXDFFNXSZQB-UHFFFAOYSA-N calcium;cyanamide Chemical compound [Ca+2].NC#N STRTXDFFNXSZQB-UHFFFAOYSA-N 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- IOJUPLGTWVMSFF-UHFFFAOYSA-N cyclobenzothiazole Natural products C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 6
- 238000004073 vulcanization Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- RZFBEFUNINJXRQ-UHFFFAOYSA-M sodium ethyl xanthate Chemical compound [Na+].CCOC([S-])=S RZFBEFUNINJXRQ-UHFFFAOYSA-M 0.000 claims description 5
- QMXSSEWSCICQCP-UHFFFAOYSA-N 2-ethyl-1,3-benzothiazole-4-carbothioamide Chemical compound C(N)(=S)C1=CC=CC2=C1N=C(S2)CC QMXSSEWSCICQCP-UHFFFAOYSA-N 0.000 claims description 4
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- LBVNUQQORDPZCR-UHFFFAOYSA-N calcium;sulfane Chemical compound S.[Ca] LBVNUQQORDPZCR-UHFFFAOYSA-N 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000011085 pressure filtration Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical compound [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 claims description 2
- 125000002252 acyl group Chemical group 0.000 claims 1
- SARKRSWCLHYVGQ-UHFFFAOYSA-N ethoxymethanedithioic acid;sodium Chemical compound [Na].CCOC(S)=S SARKRSWCLHYVGQ-UHFFFAOYSA-N 0.000 claims 1
- 239000000419 plant extract Substances 0.000 claims 1
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 19
- 239000002994 raw material Substances 0.000 description 9
- 238000000605 extraction Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- XAQHXGSHRMHVMU-UHFFFAOYSA-N [S].[S] Chemical compound [S].[S] XAQHXGSHRMHVMU-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000855 fungicidal effect Effects 0.000 description 2
- 239000000417 fungicide Substances 0.000 description 2
- 238000012946 outsourcing Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000004174 sulfur cycle Methods 0.000 description 2
- 238000012719 thermal polymerization Methods 0.000 description 2
- 150000003568 thioethers Chemical class 0.000 description 2
- 239000000052 vinegar Substances 0.000 description 2
- 235000021419 vinegar Nutrition 0.000 description 2
- UZASMYQTKALYAA-UHFFFAOYSA-N 1-benzothiophene 1H-pyrrole Chemical class N1C=CC=C1.S1C=CC2=C1C=CC=C2 UZASMYQTKALYAA-UHFFFAOYSA-N 0.000 description 1
- ZQDMKVFNIVOKBB-UHFFFAOYSA-N 2-ethylbenzenecarbothioamide Chemical compound CCC1=CC=CC=C1C(N)=S ZQDMKVFNIVOKBB-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- FZWLAAWBMGSTSO-UHFFFAOYSA-N Thiazole Chemical compound C1=CSC=N1 FZWLAAWBMGSTSO-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- MEKDPHXPVMKCON-UHFFFAOYSA-N ethane;methane Chemical compound C.CC MEKDPHXPVMKCON-UHFFFAOYSA-N 0.000 description 1
- 239000008396 flotation agent Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000002674 ointment Substances 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- GPNLWUFFWOYKLP-UHFFFAOYSA-N s-(1,3-benzothiazol-2-yl)thiohydroxylamine Chemical compound C1=CC=C2SC(SN)=NC2=C1 GPNLWUFFWOYKLP-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 230000019086 sulfide ion homeostasis Effects 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
- C01B17/12—Insoluble sulfur (mu-sulfur)
-
- 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
- C01B17/16—Hydrogen sulfides
- C01B17/161—Preparation from elemental sulfur
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C335/00—Thioureas, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C335/02—Thiourea
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
- Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The invention discloses a kind of recoverying and utilizing methods of oil plant sulfur removal plant sulphur steam, belong to field of fine chemical.Sour gas from distillation system is sent to the Cross unit of sulfur recovery first, 300 DEG C 500 DEG C of mixed gas is obtained after 1100-1300 DEG C of processing, waste heat boilers take heat, mixed gas is trapped to obtain 160-170 DEG C of molten sulfur through cooler cooling and trap；Then molten sulfur is sent directly into heating furnace, 500-700 DEG C of sulphur steam is heated in heating furnace and is divided into two-way：Sulfur vapor is to prepare the insoluble sulfur with highly resistance hot function all the way, and another way sulphur steam is sent to carbon disulfide reactor after being mixed with methane or methane, ethane gaseous mixture, prepares carbon disulfide and hydrogen sulfide.The present invention takes comprehensive utilization energy consumption resource, reduces by 33% -37% to make it produce the production cost of similar insoluble sulfur, carbon disulfide, hydrogen sulfide and its derivative thiocarbamide, reduces general item investment volume 31% -34%, energy-saving and environment-friendly.
Description
Technical field
The invention belongs to field of fine chemical, and in particular to a kind of recycling side of oil plant sulfur removal plant sulphur steam
Method.
Background technology
Carbon disulfide is widely used, and can be used as chemical materials intermediate, also can be used as solvent and extractant etc..Insoluble sulfur
Sulphur, also known as：Polymerised sulphur, english abbreviation：IS.It is manufactured for automobile tire, rubber roller rubber product is used for, such as carpet, sebific duct, glue
Band, rubber overshoes etc..The market share in the U.S. Flexsys monopolization whole world about 63%.About 20000 yuan of price per ton, global insoluble sulfur
Sulphur about needs 1,100,000 tons.Good market prospect.The project belongs to national high-tech industry scope.
And the production technology of sulphur, charcoal production carbon disulfide is utilized in the prior art, seriously polluted, produced hydrogen sulfide
Gas is all discharged to air, this production method is prohibited by International Environmental Protection department.And it is domestic with sulphur, natural gas life
The enterprise for producing carbon disulfide technique, is that National Environmental Protection Agency is approved, but its thermal energy, electric energy, the public utilities such as cooling water
It needs newly to add, create, raw material are entirely outsourcing, and therefore, its manufacturing cost is higher.
Being warming up to 500-700 ° by electrical heating with solid sulfur by domestic and international convention production insoluble sulfur can consume largely
Thermal energy power supply and fund for equipment investment, the sulphur steam cooling-cooling-molten sulfur-solid sulfur generated in production consume take greatly again
The energy consumption of amount accounts for about 28% -37% budget fund of its oil refining, natural gas investment.And equipment is corroded in the two production process
Seriously, certain pollution is generated to environment, and negative effect is risen to global warming, it is vertical not meet energy-efficient chemical products
Item principle.
Invention content
It is an object of the invention to be directed to carbon disulfide, technology present in insoluble sulfur production process in the prior art
Problem, provides a kind of recoverying and utilizing method of oil plant sulfur removal plant sulphur steam, and this method is raw simultaneously in oil plant sulfur removal plant
Carbon disulfide and insoluble sulfur, public set of device are produced, construction cost and production cost reduce, and possess raw material advantage, first
Alkane and sulphur do not have to outsourcing, save storage and transportation expense, can gather materials on the spot, and efficiently solve the emission problem of sulfur vapor, environmental protection, warp
Ji.
Purpose to realize the present invention, the technical solution adopted by the present invention are：A kind of oil plant sulfur removal plant sulphur steam returns
The method of utilizing is received, the sour gas from distillation system is sent to the Cross unit of sulfur recovery first, through 1100-1300
DEG C processing, waste heat boiler obtain 300 DEG C -500 DEG C of mixed gas after taking heat, by mixed gas through cooler is cooling and trap
Trapping obtains 160-170 DEG C of molten sulfur；Then molten sulfur is sent directly into heating furnace, heating furnace is heated to 500-700 DEG C
Form sulphur steam, then by from distillation system methane or methane, ethane gaseous mixture also heated stove heat to 500-700
DEG C, it is heated to 500-700 DEG C of sulphur steam in heating furnace and is divided into two-way：Sulphur steam is injected directly into insoluble sulfur all the way
Reactor, the chilling in the carbon disulfide solution containing compound stabilizer crush after chilling molding, and it is 63-68% to obtain content
Insoluble sulfur, through the benzene extraction from oil plant, obtaining content after being stablized with stabilizer is for the insoluble sulfur of 63-68%
The insoluble sulfur of 98.8-99.2%, insoluble sulfur obtain the insoluble sulfur with highly resistance hot function after oil-filled stirring；
And carbon disulfide reactor is sent to after another way sulphur steam and the gas mixing from distillation system, sulfur vapor and
Catalyst haptoreaction in methane, ethane and reactor, generates carbon disulfide and vulcanization hydrogen mixed gas, and mixed gas enters
Carbon disulfide and hydrogen sulphide separator, isolate carbon disulfide and hydrogen sulfide, and the hydrogen sulfide isolated removes sulfur recovery unit all the way
Sulfur recovery processing is carried out, goes to react with milk of lime all the way and manufactures thiocarbamide, the carbon disulfide isolated does product after rectifying
It goes to sell.
Based on the above-mentioned technical proposal, the method for the hydrogen sulfide and milk of lime reaction manufacture thiocarbamide is：First, stink damp
Hydrogen sulfide calcium solution is made through milk of lime negative pressure absorbing in body, and chemical equation is：2H2S+Ca (OH) 2 → Ca (SH) 2+2H2O,
Then it is reacted again with nitrolim, the molar ratio of calcium sulfhydrate and nitrolim is 1:5, under constant stirring, instead
It is 75-85 DEG C to answer temperature, reaction time 2.5-3.5h, through negative pressure filtration, you can generates thiocarbamide liquid, thiocarbamide liquid is again through steaming
To get crystal thiocarbamide, crystal thiocarbamide centrifugal drying is got product for hair, filtering, cooling, crystallization
Based on the above-mentioned technical proposal, the sour gas is a kind of plyability gas, including hydrogen sulfide, sulfur dioxide, chlorine
Gas, hydrogen chloride and carbon dioxide, nitric oxide gas, wherein hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride and carbon dioxide, one
The ratio of nitrogen oxide gas is：77.63:11.76:2.36:1.19:4.22:2.84.
Based on the above-mentioned technical proposal, the methane from distillation system, methane at least accounts for 93% or more in ethane gaseous mixture,
Remaining is ethane.
Based on the above-mentioned technical proposal, the compound stabilizer is by carbon disulfide, sodium ethylxanthate, curing benzo thiophene
Azoles, a- methyl styrenes, N tert butyl benzothiazole 2 sulfenamide, N- cyclohexyls thiocarbamoyl -ethyl- benzothiazole,
Potassium iodide forms, wherein carbon disulfide, sodium ethylxanthate, benzothiazole disulfide, a- methyl styrenes, N- tertiary butyls -2-
The weight ratio of benzothiazole sulfenamide, N- cyclohexyls thiocarbamoyl -ethyl- benzothiazole and potassium iodide is：74.09:
0.5-5:1-8:1-3:1-5:1-4：0.001.
Based on the above-mentioned technical proposal, the stabilizer is titanate esters.
Based on the above-mentioned technical proposal, the catalyst in the carbon disulfide reactor is potassium iodide catalyst, and potassium iodide is urged
Agent can be such that insoluble sulfur content increases.
Based on the above-mentioned technical proposal, the oil of the oil-filled stirring of insoluble sulfur is naphthenic oil.
Based on the above-mentioned technical proposal, ethylene glycol and sulfonic acid are also contained in the carbon disulfide solution containing compound stabilizer
Ester, the heat resistanceheat resistant stability of sulphur can be increased by increasing ethylene glycol and sulphonic acid ester.
The present invention has following advantageous effect：The present invention be applicant be engaged in all one's life oil-refining chemical, natural gas production with
Waste gas recovery, rubber on the basis of research, production, foreign exchange earning in 26 years, are different from both at home and abroad specially with " insoluble sulfur "
The production insoluble sulfur of the sharp similar application of document, the technique of carbon disulfide, hydrogen sulfide and thiocarbamide, take comprehensive utilization can cost
Source, to make it produce the reduction of the production cost of similar insoluble sulfur, carbon disulfide, hydrogen sulfide and its derivative thiocarbamide
33% -37%, general item investment volume 31% -34% is reduced, it is rationally comprehensive using generated pernicious gas in oil refining process to meet it
It closes and recycles, and water, gas recycle multiple utilization up to standard by each road pipeline, it is energy-saving and environment-friendly.Specifically utilize oil plant
The sulfur vapor that existing desulfurizer generates, divides two-way：Sulfur vapor is through reacting generation two with the methane ethane from system all the way
Nitric sulfid；Another way sulphur steam is through with after compound stabilizer thermal polymerization, obtaining common insoluble sulfur, using extraction with carbon disulfide
High-purity insoluble sulfur is obtained afterwards.It saves sulphur workshop and pollutes larger sulfur prilling and pelletizer.
The benzene of oil plant production of the present invention, can be used as the extractant of insoluble sulfur.Insoluble sulfur is used for automobile tire
Manufacture is used for rubber roller rubber product, such as carpet, sebific duct, rubber overshoes.Deep processing is carried out to sulphur using oil plant self-produced raw material,
Its is at low cost, high efficiency.
The present invention is to produce insoluble sulfur in oil plant and sulfur removal plant, possesses raw material advantage, and benzene and sulphur do not have to outer
Purchase, saves equipment and storage and transportation expense, can gather materials on the spot；Meanwhile the molten sulfur of oil plant sulfur recovery unit is without cooling but straight
Use is connect, cooling and the process equipment in later stage etc. are saved.Therefore, using the new production technology of the present invention, the market of product is competing
Striving power can greatly improve.
Description of the drawings
Fig. 1 is the process flow diagram of the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam of the present invention.
Embodiment
With reference to specific embodiment, the present invention will be further described, to more fully understand technical solution of the present invention.
Embodiment 1：A kind of recoverying and utilizing method of oil plant sulfur removal plant sulphur steam, first by the acid from distillation system
Property gas be sent to the Cross unit of sulfur recovery, obtain 300 DEG C -500 after 1100-1200 DEG C of processing, waste heat boiler take heat
DEG C mixed gas, sour gas by Cross unit time it is very of short duration, substantially 0.01-0.5s.Wherein sour gas
It is a kind of plyability gas, including hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride gas, carbon dioxide, nitric oxide etc., wherein
Hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride and carbon dioxide, nitric oxide gas ratio be：77.63:11.76:2.36:
1.19:4.22: 2.84。
Mixed gas is cooled down through cooler and trap traps to obtain 160-165 DEG C of molten sulfur, the cooling temperature of cooler
Degree selection is at 160-165 DEG C；Then molten sulfur is sent directly into heating furnace, heating furnace is heated to 500-600 DEG C of formation sulphur
Steam, then also heated stove heat is to 500-600 DEG C by methane, ethane gaseous mixture from distillation system, wherein in gaseous mixture
Methane at least accounts for 93% or more, remaining is ethane.
It is heated to 500-600 DEG C of sulphur steam in heating furnace and is divided into two-way：Sulphur steam is injected directly into insoluble all the way
Sulfur reaction device, the chilling in the carbon disulfide solution containing compound stabilizer are crushed to 180 mesh after chilling molding, are contained
Amount is the insoluble sulfur of 63-65%, and the insoluble sulfur of 63-65% enters back into insoluble sulfur extraction kettle and passes through the benzene from oil plant
Extraction, with stabilizer titanate esters（CH3 (CH2) 20) Ti, C12H28O4Ti）It is the insoluble of 98.8-99% that content is obtained after stabilization
Property sulphur, obtain content be 98.8-99% insoluble sulfur, go oil-filled stirring, obtain HIS-7020, HIS-6033, OT-33 high
The insoluble sulfur of heat resistanceheat resistant, spin-off are medical cream, efficient thioether vinegar fungicide, wherein the oil for oil-filled stirring is ring
Alkane oil.The additive amount of benzene extraction is preferably 3 times of manufactured insoluble sulfur.It is with the difference of the prior art herein：It is not
Production molten sulfur is removed by domestic and international convention, through its cooling, is solidified into its sulphur, and is to leave out solid sulfur and is warming up to by electrical heating
Sulphur steam cooling-the cooling-generated in 500-600 ° of a large amount of thermal energy power supplys and fund for equipment investment consumed, and production
Molten sulfur-solid sulfur consumes take a large amount of energy consumption, the present embodiment that the molten sulfur of sulfur removal plant is directly heated to 500-600 DEG C again
Temperature forms sulphur steam, and insoluble sulfur is obtained after thermal polymerization, saves sulphur workshop and pollutes larger sulfur prilling and film-making dress
It sets.It is to be noted that the heating furnace of molten sulfur and the heating furnace of methane, ethane gaseous mixture are different furnace bodies in the present embodiment.Separately
Outside, ethylene glycol and sulphonic acid ester are also added in the present embodiment carbon disulfide solution other than containing compound stabilizer, adds ethylene glycol
The heat resistanceheat resistant stability of insoluble sulfur can be improved with sulphonic acid ester.
And another way sulphur steam is sent to carbon disulfide after being mixed with methane, ethane gaseous mixture from distillation system and reacts
Potassium iodide catalyst haptoreaction in device, sulfur vapor and methane, ethane and reactor interacts, methane conversion per pass
Up to 90%, chemical equation is：CH4+4S=CS2+2H2S, under conditions of methane abundance, the common sulphur of 128kg can give birth to
76kg carbon disulfide is produced, generation goes back by-product hydrogen sulfide 68kg, uses Crouse（Claus）Method can make it be changed into sulfur cycle
It uses.Its chemical equation is：2H2S+3O2=2SO2+2H2O, SO2+2H2S=3S+2H2O, i.e., in carbon disulfide reactor
Obtain carbon disulfide and vulcanization hydrogen mixed gas.Insoluble sulfur content can be made to increase using potassium iodide catalyst in the present embodiment.
Mixed gas enters carbon disulfide and hydrogen sulphide separator, isolates carbon disulfide and hydrogen sulfide, the sulphur isolated
Change hydrogen goes sulfur recovery unit to carry out sulfur recovery processing all the way, goes to react with milk of lime all the way and manufactures thiocarbamide, two isolated
Nitric sulfid does product after rectifying and goes to sell.And carbon disulfide is widely used, and can be used as chemical materials intermediate, also can be used as molten
Agent and extractant etc..The dry gas that the present embodiment generates during producing carbon disulfide, can produce High-purity hydrogen sulfide, hydrogen sulfide
Spin-off thiocarbamide can also be produced, and hydrogen sulfide can also be sold directly as product, High-purity hydrogen sulfide be production electronic product and
The fluorescent powder of television picture tube, it is the raw material for producing many chemical products.The present embodiment production technology, raw material self-sufficiency is certainly
Foot, production cost is minimum, comprehensive benefit highest, and environmentally friendly, safe and reliable.
To produce thiocarbamide（CN2H4S, also referred to as thio urea）For, the preparation method of hydrogen sulfide production spin-off thiocarbamide is：
First, hydrogen sulfide calcium solution is made through milk of lime negative pressure absorbing in hydrogen sulfide gas, and chemical equation is：2H2S+Ca(OH)2→
Ca (SH) 2+2H2O,
Then it is reacted again with nitrolim, the molar ratio of calcium sulfhydrate and nitrolim is 1:5, under constant stirring, instead
The temperature is answered to be（80±5）DEG C, reaction time 3h, through negative pressure filtration, you can generate thiocarbamide liquid, then through evaporation, filtering, cold
But, to get crystal thiocarbamide, centrifugal drying is got product for crystallization.Thiocarbamide is widely used in manufacture drug, dyestuff, resin, pressure
The raw material of molding powder etc. also serves as the vulcanization accelerator of rubber, flotation agent of metalliferous mineral etc..
Embodiment 2：A kind of recoverying and utilizing method of oil plant sulfur removal plant sulphur steam, first by the acid from distillation system
Property gas be sent to the Cross unit of sulfur recovery, obtain 300 DEG C -500 after 1200-1300 DEG C of processing, waste heat boiler take heat
DEG C mixed gas, wherein sour gas is a kind of plyability gas, including hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride gas
Body, carbon dioxide, nitric oxide etc..Mixed gas is trapped to obtain 165-170 DEG C of liquid through cooler cooling and trap
Sulphur；Then molten sulfur is sent directly into heating furnace, heating furnace is heated to 600-700 DEG C of formation sulphur steam, then oil refining will be come from
The methane of system also heated stove heat to 600-700 DEG C.
It is heated to 600-700 DEG C of sulphur steam in heating furnace and is divided into two-way：Sulfur vapor is injected directly into insoluble all the way
Sulfur reaction device, the chilling in the carbon disulfide solution containing compound stabilizer are crushed to 180 mesh after chilling molding, are contained
Amount is the insoluble sulfur of 65.5-68%, and the insoluble sulfur of 65.5-68% enters back into insoluble sulfur extraction kettle and passes through from oil plant
Benzene extraction, obtain the insoluble sulfur that content is 99-99.2% after being stablized with stabilizer, be 99-99.2% content is obtained
Insoluble sulfur goes oil-filled stirring, obtains the insoluble sulfur of HIS-7020, HIS-6033, OT-33 high heat resistanceheat resistant, and spin-off is doctor
With ointment, efficient thioether vinegar fungicide.Compound stabilizer in the present embodiment is by carbon disulfide, sodium ethylxanthate, curing
Benzothiazole, a- methyl styrenes, N tert butyl benzothiazole 2 sulfenamide, N- cyclohexyls thiocarbamoyl -ethyl- benzene
And thiazole, potassium iodide composition, wherein carbon disulfide, sodium ethylxanthate, benzothiazole disulfide, a- methyl styrenes, uncle N-
The weight ratio of butyl -2-[4-morpholinodithio sulfenamide, N- cyclohexyls thiocarbamoyl -ethyl- benzothiazole and potassium iodide is：
75:0.5-5:1-8:1-3:1-5:1-4：0.001.With the important indicator for the insoluble sulfur that the compound stabilizer produces：It is hot steady
Qualitative is the optimal highest product of current international industry, is the vulcanizing agent of Global Auto tyre production enterprise first choice.It is heavy using this
The combination of stabilizers for measuring ratio, HG/T2525-2011 standards more existing than China are high, can reach international similar product best quality mark
It is accurate.And the product quality of domestic insoluble sulfur enterprise is molten into Molten sulphur in 120 degree of 15min, is substandard product.
And another way sulphur steam is sent to carbon disulfide reactor after being mixed with both the methane from distillation system, sulphur steams
Vapour and methane and the potassium iodide catalyst haptoreaction in reactor, interact, and methane conversion per pass is changed up to 92%
Learning reaction equation is：CH4+4S=CS2+2H2S, under conditions of methane abundance, the common sulphur of 131kg can produce 78kg curing
Carbon, generation go back by-product hydrogen sulfide 69kg, use Crouse（Claus）Method can make it be changed into sulfur cycle use.Its chemistry
Equation is：2H2S+3O2=2SO2+2H2O, SO2+2H2S=3S+2H2O obtain carbon disulfide in carbon disulfide reactor
With vulcanization hydrogen mixed gas.
Mixed gas enters carbon disulfide and hydrogen sulphide separator, isolates carbon disulfide and hydrogen sulfide, the sulphur isolated
Change hydrogen goes sulfur recovery unit to carry out sulfur recovery processing all the way, goes to react with milk of lime all the way and manufactures thiocarbamide, two isolated
Nitric sulfid does product after rectifying and goes to sell.And carbon disulfide is widely used, and can be used as chemical materials intermediate, also can be used as molten
Agent and extractant etc..The dry gas that the present embodiment generates during producing carbon disulfide, can produce High-purity hydrogen sulfide, hydrogen sulfide
Spin-off thiocarbamide can also be produced, and hydrogen sulfide can also be sold directly as product, High-purity hydrogen sulfide be production electronic product and
The fluorescent powder of television picture tube, it is the raw material for producing many chemical products.The present embodiment production technology, raw material self-sufficiency is certainly
Foot, production cost is minimum, comprehensive benefit highest, and environmentally friendly, safe and reliable.
Claims (9)
1. a kind of recoverying and utilizing method of oil plant sulfur removal plant sulphur steam, it is characterized in that：First by the acid from distillation system
Property gas be sent to the Cross unit of sulfur recovery, obtain 300 DEG C-500 after 1100-1300 DEG C of processing, waste heat boilers take heat
DEG C mixed gas, by mixed gas through cooler cooling and trap trap to obtain 160-170 DEG C of molten sulfur；Then by liquid
Sulphur is sent directly into heating furnace, heating furnace is heated to 500-700 DEG C of formation sulphur steam, then by the methane from distillation system
Or also heated stove heat is heated to 500-700 DEG C of sulphur to 500-700 DEG C in heating furnace for methane, ethane gaseous mixture
Steam is divided into two-way：Sulphur steam is injected directly into insoluble sulfur reactor all the way, in the carbon disulfide containing compound stabilizer
Chilling in solution crushes after chilling molding, obtains the insoluble sulfur that content is 63-68%, the insoluble sulfur of 63-68% is through coming from
The benzene of oil plant extracts, and the insoluble sulfur that content is 98.8-99.2% is obtained after being stablized with stabilizer, insoluble sulfur is stirred through oil-filled
The insoluble sulfur with highly resistance hot function is obtained after mixing；
And it is sent to carbon disulfide reactor, sulfur vapor and first after another way sulphur steam and the gas mixing from distillation system
Catalyst haptoreaction in alkane, ethane and reactor, generates carbon disulfide and vulcanization hydrogen mixed gas, and mixed gas enters two
Nitric sulfid and hydrogen sulphide separator, isolate carbon disulfide and hydrogen sulfide, the hydrogen sulfide isolated go all the way sulfur recovery unit into
Row sulfur recovery is handled, and is gone to react with milk of lime all the way and is manufactured thiocarbamide, the carbon disulfide isolated does product after rectifying and goes
Sale.
2. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：The vulcanization
Hydrogen and milk of lime react the method for manufacturing thiocarbamide：First, hydrogen sulfide gas is molten through the obtained hydrogen sulfide calcium of milk of lime negative pressure absorbing
Liquid, chemical equation are：2H2S+Ca (OH) 2 → Ca (SH) 2+2H2O,
Then it is reacted again with nitrolim, the molar ratio of calcium sulfhydrate and nitrolim is 1:5, under constant stirring, reaction temperature
Degree be 75-85 DEG C, reaction time 2.5-3.5h, through negative pressure filtration, you can generate thiocarbamide liquid, thiocarbamide liquid again through evaporation,
To get crystal thiocarbamide, crystal thiocarbamide centrifugal drying is got product for filtering, cooling, crystallization.
3. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：The acidity
Gas is a kind of plyability gas, including hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride and carbon dioxide, nitric oxide gas,
Wherein hydrogen sulfide, sulfur dioxide, chlorine, hydrogen chloride and carbon dioxide, nitric oxide gas ratio be：77.63:11.76:
2.36:1.19:4.22:2.84。
4. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：From oil refining
Methane at least accounts for 93% or more in the methane of system, ethane gaseous mixture, remaining is ethane.
5. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：It is described compound
Stabilizer is by carbon disulfide, sodium ethylxanthate, benzothiazole disulfide, a- methyl styrenes, N- tertiary butyls -2-[4-morpholinodithio
Sulfenamide, N- cyclohexyls thiocarbamoyl -ethyl- benzothiazole, potassium iodide composition, wherein carbon disulfide, ethoxy-dithioformic acid
Sodium, benzothiazole disulfide, a- methyl styrenes, N tert butyl benzothiazole 2 sulfenamide, N- cyclohexyl sulfo-amino first
The weight ratio of acyl -ethyl- benzothiazole and potassium iodide is：74.09:0.5-5:1-8:1-3:1-5:1-4：0.001.
6. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：The stabilization
Agent is titanate esters.
7. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：Two sulphur
It is potassium iodide catalyst to change the catalyst in carbon reactor.
8. the recoverying and utilizing method of oil plant sulfur removal plant sulphur steam according to claim 1, it is characterized in that：Insoluble sulfur
The oil of oil-filled stirring is naphthenic oil.
9. according to the recoverying and utilizing method of claim 1-8 any one of them oil plant sulfur removal plant sulphur steam, it is characterized in that：
Also contain ethylene glycol and sulphonic acid ester in the carbon disulfide solution containing compound stabilizer.
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