CN101693164A - Method for obtaining high-purity sulphur from Claus reactive tail-gases - Google Patents
Method for obtaining high-purity sulphur from Claus reactive tail-gases Download PDFInfo
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- CN101693164A CN101693164A CN200910210198A CN200910210198A CN101693164A CN 101693164 A CN101693164 A CN 101693164A CN 200910210198 A CN200910210198 A CN 200910210198A CN 200910210198 A CN200910210198 A CN 200910210198A CN 101693164 A CN101693164 A CN 101693164A
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- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention relates to a method for obtaining high-purity sulphur from Claus reactive tail-gases, which belongs to the technical field of environmental protection. The method comprises steps as follows: (1) Claus tail-gas is preheated to reach the temperature between 160 DEG C to 300 DEG C; (2) the preheated gas enters a reduction reaction furnace filled with selective reaction catalysts to perform reduction reaction; (3) liquid sulphur is separated out of the reacted process gas via a condenser; (4) the process gas performs direct oxidization reaction inside a direct oxidizing reactor after being compensated with oxygen and preheated again; (5) liquid sulphur is separated out of gas on an outlet of the reactor via a sulphur condenser and a separator, tail gases after burned are cooled, washed by using an alkaline liquor and then discharged. The method overcomes the shortcoming that sulphur can not be produced by a traditional tail-gas hydrogenation reactor, improves total recovery efficiency of sulphur in a single process, and has the advantages of saving energy, lowering H2 consumption amount, reducing volume of absorption towers, decreasing arranged devices, lowering manufacturing cost and reducing operating load of the overall set of devices.
Description
Technical field
The invention belongs to environmental protection technical field, be specifically related to from Claus tail gases, obtain the method for high purity sulphur.
Background technology
Sulfide in crude oil or the coal is converted into H in process
2S, and H
2S is an extremely toxic substance, and human body and environment are had great toxic action, must carry out harmless treatment, and the only technology of corresponding employing is exactly recovery technology of sulfur.The sour gas of oil plant is mainly derived from devices such as catalysis drying gas desulfurization, the desulfurization of coking dry gas, sewage gas stripping tower gas, hydro-refining unit desulfurization.
The main work flow of the sour gas of oil plant is: the sulphur → PETROLEUM PROCESSING in the crude oil (normal decompression) → gasoline kerosene diesel oil → hydrofinishing → H
2S → sulphur recovery → sulphur;
Be in the chemical plant of raw material with the coal, the work flow of sour gas mainly is: coal → Coal Chemical Industry → desulfurization → H
2S → sulphur recovery → sulphur;
Industry generally adopts the improvement claus process to handle the H that contains of generations such as oil plant, chemical plant
2The sour gas of S, Recovered sulphur is also protected environment, and its basic principle is as follows:
Because the existence of hydro carbons under the hot conditions of combustion furnace, inevitably has a spot of organic sulfur compound CS in the sour gas
2Generate with COS, therefore must be removed by the tempreture organic sulphur hydrolysis reaction at catalytic reactor:
The basic technology type of claus reaction has three kinds: direct current method, shunting and sulfur cycle method: direct current method be sour gas all by combustion furnace and waste heat boiler, in combustion furnace, generate a large amount of sulphur; Shunting is to have only 1/3rd sour gas to burn into SO by combustion furnace
2, before converter, being mixed into converter with remainder, the sulphur that generates in the stove is seldom; The sulfur cycle method be sour gas by combustion furnace, and the sulphur generation SO that in stove, burn
2And before first converter with contain H
2The sour gas mixing of S is reacted.
The world has proposed more and more higher requirement to the demand of clean fuel and from the pressure of the environmental regulation of increasingly stringent to the total sulfur recovery of sulfur recovery facility, on the one hand, because the H of the increase by-product of oil plant working ability
2S is more and more, and the device discharge capacity that government department requires is more and more lower, improves the total sulfur recovery of device when this just requires to increase the sulfur recovery facility disposal ability to satisfy double requirements.
State Bueau of Environmental Protection has formulated strict more discharge standard of air pollutants (GB16297-1996) and has stipulated since mandatory enforcement on January 1 in 1997.GB16297 is to SO
2Strict regulations have been made in discharging, new pollution sources SO
2≤ 960mg/m3 (336ppmv), existing pollution sources SO
2≤ 1200mg/m3 (420ppmv), and the sulfide emission amount also made regulation.By this standard, require oil plant and chemical plant sulphur recovery total sulfur recovery will reach 99.7～99.9%.Claus plant has only the reduction adopted to absorb the requirement that tail gas treatment process just can reach above-mentioned environmental protection standard.
Traditional claus process mainly comprises equipment compositions such as sour gas combustion furnace, waste heat boiler, two or three catalytic reactors and condenser, trap.The total sulfur conversion ratio can reach 94～97% behind general second reactor.The catalyst of corresponding employing mainly contains activated alumina catalyst, auxiliary agent type aluminium oxide catalyst and titanium deoxide catalyst etc.
In order to satisfy higher environmental requirement, must make further purified treatment to the tail gas that Cross unit is discharged, the technology that the past adopts mainly contains low-temperature Claus technology, super claus process, tail gas hydrogenation reducing process etc.In these technologies, have only the tail gas hydrogenation reducing process can satisfy the strictest environmental protection standard, total sulfur recovery can reach more than 99.8%, and its process chart is seen Fig. 1, and the cardinal principle of tail gas hydrogenation reducing process is to adopt hydrogen with the non-H in the sulfur recovery facility tail gas
2The sulfur-containing compound of S such as S0
2/ COS/CS
2/ S etc. all are hydrogenated to H
2S, then by MDEA with H
2The sour gas combustion furnace that turns back to sulfur recovery facility after S absorption and the desorb carries out further sulphur recovery.The tail gas of discharging from the top, absorption tower only contains the sulfide of trace, by entering atmosphere behind the incinerator high temperature incineration.SO in the flue gas
2Discharge capacity less than 960mg/m
3, satisfy the emission request of GB16297-1996.
That the tail gas hydrogenation reduction reactor adopts is common CoO/MoO/Al
2O
3Hydrogenation catalyst, inlet temperature are 280～300 ℃, and reactor batch temperature is generally 300～330 ℃.
From the above mentioned as can be known, traditional hydrogenating reduction refers to all sulfide in the claus reaction tail gas all is reduced into hydrogen sulfide, and then handle through various channels, and all sulfide are changed into hydrogen sulfide, more than temperature required 300 degree, middle pressure steam can't satisfy, and needs the peripheral hardware heating furnace; The hydrogen source of Xiao Haoing is also bigger in addition, and the hydrogen that the burning zone cracking produces can't satisfy, and need add hydrogen source.
Summary of the invention
To the objective of the invention is the problems referred to above of existing in traditional claus reaction in order solving, to provide under the middle pressure steam condition, need not to add hydrogen source, just the sulphur dioxide reduction in the Claus tail gases can be generated a kind of method that obtains high purity sulphur of sulphur and water.
Technical scheme of the present invention is as follows:
A kind of method that from claus reaction tail gas, obtains high purity sulphur, it may further comprise the steps:
(1), Claus tail gases is through being preheated to 160 ℃～300 ℃;
(2), the gas after the preheating enters and carries out reduction reaction in the reduction reaction furnace, be filled with in the described reduction reaction furnace only to SO in the Claus tail gases
2The selective reduction catalyst that plays a driving role of reduction, key reaction is 2H in the stove
2+ SO
2=S+2H
2O; Wherein said selective reduction catalyst has only to SO in the Claus tail gases
2Reduction play a driving role, and other sulfide in the tail gas are not had the characteristic of impetus, this selective reduction catalyst can buy from the market also can request for utilization number be 200810237813.7, name is called the catalyst in " a kind of efficient selective reducing catalyst " patent application;
(3), reacted process gas is separated out molten sulfur by condenser;
(4), the process gas that comes out from condenser is being filled with after joining oxygen, preheating again in the direct oxidation reactor of Ti-base catalyst and carrying out the direct oxidation reaction, the key reaction in reactor is 2H
2S+O
2=2S+2H
2O and 2H
2S+SO
2=3S+2H
2O, the described in this step oxygen of joining is meant hydrogen sulfide content in the testing process gas, then according to the ratio of hydrogen sulfide and oxygen in the above-mentioned chemical equation with hydrogen sulfide and oxygen mix, the oxygen here can be pure oxygen, oxygen enrichment or air, and the preheating in this step is meant and is preheated to 200 ℃～220 ℃;
(5), separate out molten sulfur through sulfur condenser, separator, from the direct oxidation reactor gas that comes out tail gas after burning with alkaline solution cooling, washing back emptying.
Method described in the technique scheme, the Claus tail gases in the wherein said step (1) are preheated to 180 ℃～200 ℃.
Method described in the technique scheme, the Claus tail gases preheating in the wherein said step (1) is by the middle pressure steam preheating, also can select modes such as online heating furnace, hot fusion to heat.
Method described in the technique scheme, hydrogen sulfide and sulfur dioxide ratio in the process gas in the wherein said step (2) are far longer than 2, and promptly the amount of sulfur dioxide is infinitely close to 0 in the process gas.
Method described in the technique scheme, the direct oxidation reactor that is adopted when carrying out the direct oxidation reaction in the wherein said step (4) is the thermal insulation-isothermal one reactor that is filled with Ti-base catalyst.
Method described in the technique scheme, wherein contained concentration of hydrogen sulfide is 1.2% when following in the process gas in the described step (4), and the direct oxidation reactor that carries out being adopted when direct oxidation is reacted is the adiabatic reactor that is filled with Ti-base catalyst.
Owing to adopted above-mentioned technical scheme, the present invention has following beneficial effect:
1, the reduction reaction among the present invention is to react under the effect of selective reduction catalyst, this catalyst only plays a driving role to the reduction of sulfur dioxide in the Claus tail gases, and other sulfide are not had impetus, the hydrogen that reducing agent produces for the burning zone cracking, need not to add hydrogen source, key reaction is that hydrogen and sulfur dioxide reaction generate sulphur and water; And traditional hydrogenating reduction refers to all sulfide in the tail gas all is reduced into hydrogen sulfide, and then handle through various channels, and it is also bigger that all sulfide are changed into the hydrogen source that hydrogen sulfide consumes, therefore need add hydrogen source and in the present invention handles the process of Claus tail gases, need not to make the equipment and the technology of establishing hydrogenation, thereby technological design and processing step have been reduced, and the optional equipment amount that has reduced equipment, thereby reduced cost;
2, reduction reaction of the present invention is that Claus tail gases is preheated under 160 ℃～300 ℃ temperature, and the reaction of carrying out under preferred 180 ℃～200 ℃ temperature can be carried out preheating with middle pressure steam, does not need to re-use heating furnace; And traditional hydrogenation reduction is if change into hydrogen sulfide with all sulfide, more than temperature required 300 degree, middle pressure steam can't satisfy, therefore necessary peripheral hardware heating furnace, and temperature range span of the present invention is big, therefore technical scheme of the present invention can adopt multiple preheating method to carry out preheating, the adverse consequences of having avoided single preheating method to produce;
3, in technical scheme of the present invention, adopted the catalytic action of selective reduction catalyst, made that the main reaction in the reacting furnace is 2H
2+ SO
2=S+2H
2O, promptly directly with selective reduction catalyst with SO
2Be reduced to S, solved the shortcoming that traditional tail gas hydrogenation reactor does not generate sulphur, improved the total sulphur recovery efficiency of one way of device;
4, adopt special selective reduction catalyst, the operating temperature of hydrogenation reduction device is lower, the practical operation temperature is 160 ℃～400 ℃, the hydrogenation reactor inlet temperature can be controlled at 160 ℃～200 ℃, therefore only need just can reach the requirement of reactor inlet temperature fully by heat exchange, do not need to re-use heating furnace, saved the energy greatly;
5, since selectivity tail gas hydrogenation reactor only to SO
2Carry out hydrogenation reaction, can reduce 30%H at least
2Consumption;
6, because the SO in the tail gas
2Be converted into S and collect in the molten sulfur storage tank in the hydrogenation reduction device, therefore, the load of tail gas absorber can reduce more than 30%;
7, because tail gas absorber load reduces, reduced the volume on absorption tower accordingly, compared with traditional tail gas hydrogenation reducing process, setting, the technical process that has reduced equipment be simple, reduced manufacturing cost;
8, because the one way total sulfur recovery improves, be equivalent to reduce the operational load of package unit.
Description of drawings:
Fig. 1 is traditional claus reaction tail gas hydrogenation reducing process flow chart;
Fig. 2 is a claus reaction tail gas reducing process flow chart of the present invention.
The specific embodiment:
For making technical scheme of the present invention be convenient to understand, the present invention is further illustrated below in conjunction with the specific embodiment.
Embodiment 1:
A kind of method that from claus reaction tail gas, obtains high purity sulphur, it may further comprise the steps:
(1), Claus tail gases is preheated to 180 ℃～200 ℃ by heat exchange;
(2), the gas after the preheating enters that to carry out key reaction in the reduction reaction furnace that is filled with selective reduction catalyst be 2H
2+ SO
2=S+2H
2The reduction reaction of O, wherein selective reduction catalyst is the catalyst for recovering sulfur of A999 for the specification from Shandong Xunda Chemical Industrial Group Co., Ltd.;
(3), reacted process gas is separated out molten sulfur by condenser;
(4), the process gas that comes out from condenser enters the thermal insulation-isothermal one reactor that is filled with Ti-base catalyst and carries out the direct oxidation reaction after joining oxygen, preheating again;
(5), separate out molten sulfur through sulfur condenser, separator, from the reactor gas that comes out tail gas after burning with alkaline solution cooling, washing back emptying.
Embodiment 2:
The operating process of present embodiment is identical with embodiment 1, and its difference is: the concentration of hydrogen sulfide in step (4) in process gas is below 1.2%, and oxidation reaction is to carry out in being filled with the adiabatic reactor of Ti-base catalyst.
Embodiment 3:
The operating process of present embodiment is identical with embodiment 1, and its difference is: the concentration of hydrogen sulfide in step (4) in process gas is below 1%, and oxidation reaction is to carry out in being filled with the adiabatic reactor of Ti-base catalyst.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any formal and substantial restriction, all those skilled in the art, in not breaking away from the technical solution of the present invention scope, when can utilizing the above technology contents that discloses, and a little change of making, modify the equivalent variations with differentiation, be equivalent embodiment of the present invention; Simultaneously, all foundations essence technology of the present invention all still belongs in the scope of technical scheme of the present invention change, modification and the differentiation of any equivalent variations that above embodiment did.
Claims (6)
1. method that from claus reaction tail gas, obtains high purity sulphur, it may further comprise the steps:
(1), Claus tail gases is through being preheated to 160 ℃～300 ℃;
(2), the gas after the preheating enters and carries out reduction reaction in the reduction reaction furnace, be filled with in the described reduction reaction furnace only to SO in the Claus tail gases
2The selective reduction catalyst that plays a driving role of reduction, key reaction is 2H in the stove
2+ SO
2=S+2H
2O;
(3), reacted process gas is separated out molten sulfur by condenser;
(4), the process gas that comes out from condenser is being filled with after joining oxygen, preheating again and is carrying out the direct oxidation reaction in the direct oxidation reactor of Ti-base catalyst;
(5), separate out molten sulfur through sulfur condenser, separator, from the direct oxidation reactor gas that comes out tail gas after burning with alkaline solution cooling, washing back emptying.
2. method according to claim 1 is characterized in that: the Claus tail gases in the described step (1) is preheated to 180 ℃～200 ℃.
3. method according to claim 1 and 2 is characterized in that: the Claus tail gases preheating in the described step (1) is by the middle pressure steam preheating.
4. method according to claim 1 is characterized in that: hydrogen sulfide and sulfur dioxide ratio in the process gas in the described step (3) are far longer than 2.
5. method according to claim 1 is characterized in that: the direct oxidation reactor that is adopted when carrying out the direct oxidation reaction in the described step (4) is thermal insulation-isothermal one reactor.
6. method according to claim 1 or 5 is characterized in that: when concentration of hydrogen sulfide contained in the process gas in the described step (4) 1.2% when following, carrying out direct oxidation, to react the direct oxidation reactor that is adopted be adiabatic reactor.
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|---|---|---|---|
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249197A (en) * | 2010-05-17 | 2011-11-23 | 淄博高汇化工有限公司 | Method for converting hydrogen sulfide gas in production of thiofide MTB |
| CN103170223A (en) * | 2013-04-11 | 2013-06-26 | 上海华畅环保设备发展有限公司 | Rotational flow strengthening method and device for purifying sulfur production tail gases by Claus method |
| CN103318846A (en) * | 2013-06-21 | 2013-09-25 | 邵志辉 | Method for obtaining sulfur from sulfur compounds in coal chemical plant and electric power plant |
| CN103495333A (en) * | 2013-10-11 | 2014-01-08 | 陕西延长石油（集团）有限责任公司炼化公司 | Treatment technology for Claus tail gas containing sulfur dioxide, hydrogen sulfide and organic sulfur |
| CN103663386A (en) * | 2012-09-19 | 2014-03-26 | 中国石油化工股份有限公司 | Method for reducing SO2 emission concentration of sulfur device |
| CN103950900A (en) * | 2014-05-04 | 2014-07-30 | 田晓良 | Sulfur recovery process by Krauss and HOV (Tail Gas Hydrogenation+Direct Oxidation+High Energy Venturi Scrubbing) tail gas treatment |
| CN104003357A (en) * | 2014-05-21 | 2014-08-27 | 杨皓 | Tail gas treatment process of Claus desulfurization process |
| CN104528659A (en) * | 2014-12-17 | 2015-04-22 | 田晓良 | Sulfur recycling process for circularly treating low-concentration acidy gas by utilizing liquid sulfur |
| CN105293442A (en) * | 2014-06-06 | 2016-02-03 | 中国石油化工股份有限公司 | Method for decreasing flue gas SO2 emission concentration in sulphur apparatus |
| CN108128921A (en) * | 2017-12-23 | 2018-06-08 | 江苏恒新能源科技有限公司 | A kind of sewage disposal containing sodium thiocarbonate and resource recovery device and its method |
| CN110124487A (en) * | 2019-05-28 | 2019-08-16 | 重庆兴发金冠化工有限公司 | A kind of device and its technique of Claus method processing sulfur-containing tail gas |
| CN110304609A (en) * | 2018-03-27 | 2019-10-08 | 中国科学院过程工程研究所 | A kind of sulphur purification schemes suitable for coal gas direct-reduction metallurgical gas production |
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2009
- 2009-10-30 CN CN200910210198A patent/CN101693164A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102249197A (en) * | 2010-05-17 | 2011-11-23 | 淄博高汇化工有限公司 | Method for converting hydrogen sulfide gas in production of thiofide MTB |
| CN103663386A (en) * | 2012-09-19 | 2014-03-26 | 中国石油化工股份有限公司 | Method for reducing SO2 emission concentration of sulfur device |
| US8871176B2 (en) | 2012-09-19 | 2014-10-28 | China Petroleum & Chemical Corporation | Process for reducing sulfur emission of sulfur plant |
| CN103170223B (en) * | 2013-04-11 | 2015-10-21 | 上海华畅环保设备发展有限公司 | The eddy flow intensifying method of Clause method sulfur production tail gas clean-up and device |
| CN103170223A (en) * | 2013-04-11 | 2013-06-26 | 上海华畅环保设备发展有限公司 | Rotational flow strengthening method and device for purifying sulfur production tail gases by Claus method |
| CN103318846A (en) * | 2013-06-21 | 2013-09-25 | 邵志辉 | Method for obtaining sulfur from sulfur compounds in coal chemical plant and electric power plant |
| CN103495333A (en) * | 2013-10-11 | 2014-01-08 | 陕西延长石油（集团）有限责任公司炼化公司 | Treatment technology for Claus tail gas containing sulfur dioxide, hydrogen sulfide and organic sulfur |
| CN103495333B (en) * | 2013-10-11 | 2016-02-17 | 陕西延长石油（集团）有限责任公司炼化公司 | A kind of for the claus tail-gas clean-up technique containing sulfur dioxide, hydrogen sulfide and organic sulfur |
| CN103950900B (en) * | 2014-05-04 | 2016-04-06 | 田晓良 | A kind of Crouse adds the recovery technology of sulfur of HOV vent gas treatment |
| CN103950900A (en) * | 2014-05-04 | 2014-07-30 | 田晓良 | Sulfur recovery process by Krauss and HOV (Tail Gas Hydrogenation+Direct Oxidation+High Energy Venturi Scrubbing) tail gas treatment |
| CN104003357A (en) * | 2014-05-21 | 2014-08-27 | 杨皓 | Tail gas treatment process of Claus desulfurization process |
| CN105293442A (en) * | 2014-06-06 | 2016-02-03 | 中国石油化工股份有限公司 | Method for decreasing flue gas SO2 emission concentration in sulphur apparatus |
| CN105293442B (en) * | 2014-06-06 | 2018-03-20 | 中国石油化工股份有限公司 | Sulphur unit reduces flue gas SO2The method of concentration of emission |
| CN104528659A (en) * | 2014-12-17 | 2015-04-22 | 田晓良 | Sulfur recycling process for circularly treating low-concentration acidy gas by utilizing liquid sulfur |
| CN108128921A (en) * | 2017-12-23 | 2018-06-08 | 江苏恒新能源科技有限公司 | A kind of sewage disposal containing sodium thiocarbonate and resource recovery device and its method |
| CN110304609A (en) * | 2018-03-27 | 2019-10-08 | 中国科学院过程工程研究所 | A kind of sulphur purification schemes suitable for coal gas direct-reduction metallurgical gas production |
| CN110124487A (en) * | 2019-05-28 | 2019-08-16 | 重庆兴发金冠化工有限公司 | A kind of device and its technique of Claus method processing sulfur-containing tail gas |
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Open date: 20100414 |