CN108079782A - PSA resolution gas optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas - Google Patents
PSA resolution gas optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas Download PDFInfo
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- CN108079782A CN108079782A CN201711415768.5A CN201711415768A CN108079782A CN 108079782 A CN108079782 A CN 108079782A CN 201711415768 A CN201711415768 A CN 201711415768A CN 108079782 A CN108079782 A CN 108079782A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8621—Removing nitrogen compounds
- B01D53/8625—Nitrogen oxides
- B01D53/8628—Processes characterised by a specific catalyst
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2255/00—Catalysts
- B01D2255/20—Metals or compounds thereof
- B01D2255/207—Transition metals
- B01D2255/20707—Titanium
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Abstract
Lazy technology is arranged in low pressure sulfur resistant conversion and proprietary adsorbent the present invention relates to a kind of raw coke oven gas hydrogen manufacturing, raw coke oven gas is first carried out to tar removing, desulfurization, dehydration, hydrogenation deoxidation detoxification treatment successively, two sections of CO sulphur-resistant conversions are carried out again, the CO conversion in raw coke oven gas is generated hydrogen, the conversion gas of hydrogen and other impurities gas is obtained, conversion gas is first carried out to first segment PSA separation afterwards to remove the hydro carbons in conversion gas, CO, CO2、CH4、H2S, then carry out that second segment PSA separation is lazy to remove the nitrogen directly row of emptying, the final hydrogen for obtaining high purity 99.9%.In addition, the technology of the present invention also makes full use of the heat that raw coke oven gas is compressed, temperature voluntarily raises after raw coke oven gas compression, then dehydration is realized after cooling；And after using the heat of two sections of CO sulphur-resistant conversions release carrying out heat exchange heating to raw coke oven gas after the dehydration, then the deoxidation detoxification treatment is carried out, without in addition setting heating unit, reduce cost.
Description
Technical field
The invention belongs to technical field of coal chemical industry, and in particular to a kind of PSA resolution gas and coal tar hydrogenating unit sour gas
Optimize combined desulfurization technology.
Background technology
Coal tar and raw coke oven gas be all semi-coke production byproduct, they all contain sulfide in various degree, by hydrogen manufacturing,
It is generated after hydrogenation containing H2S tail gas.H2S is a kind of objectionable impurities in industrial gasses, and not only serious threat ginseng is pacified for its presence
Entirely, and corrosion and the catalyst poisoning of equipment and pipeline can be caused.Therefore, it is required in oil refining, chemical system using difference
Method carry out desulfurization process, can just meet national requirements for environmental protection.The de- H of tradition2The investment of S methods is big, and processing is containing H2S gases exist
Certain selection and limitation.
The content of the invention
In order to solve the above problem existing in the prior art, the present invention provides a kind of PSA resolution gas and coal tar hydrogenatings
Device sour gas optimizes combined desulfurization technology.The technology of the present invention is mainly to H2S works, can retain other in unstrpped gas into
Point, it is particularly suitable for possessing the desulfurization process of certain calorific value, the sulfurous gas that can directly utilize.
The technical solution adopted in the present invention is：
A kind of PSA resolution gas optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, includes the following steps：
(1) the high sulfuric acid gas after coal tar hydrogenating is passed through the first desulfurization reactor, using sodium carbonate as doctor solution,
Using phthalocyanine cobalt sulfonate as catalyst, first time desulfurization process is carried out to high sulfuric acid gas, there will be the H of 50-60%2S quilts
Removing, reaction equation are as follows：
RSH+Na2CO3=====RSNa+NaHCO3
COS+2NaOH=====Na2CO2S+H2O
CS2+ 2NaOH=====Na2COS2+H2O
(2) tail gas by the first desulfurization reactor outlet discharge carries out first time gas-liquid separation, obtains separation gas and is passed through
Second desulfurization reactor using sodium carbonate as doctor solution, using phthalocyanine cobalt sulfonate as catalyst, carries out the separation gas
Second of desulfurization process；
(3) tail gas by the second desulfurization reactor outlet discharge carries out second of gas-liquid separation, obtains low sulfur-containing tail gas；
(4) the PSA resolution gas after the low sulfur-containing tail gas that step (3) obtains being extracted hydrogen with raw coke oven gas mixes, and leads to
Enter desulfuration absorbing tower and carry out desulphurization reaction, obtain desulfurizing and purifying gas.
Wherein, the main component of the PSA resolution gas after raw coke oven gas extraction hydrogen includes hydro carbons, CO, CO2、 H2S and N2。
In step (1), the phthalocyanine cobalt sulfonate catalyst is DKT-6.
In step (1), the temperature of the first time desulfurization process is 40-45 DEG C, the time of the first time desulfurization process
For 2-8s；
H in the high sulfuric acid gas2S contents are 96-98%.
In step (2), H in the separation gas2S mass percentages are 35-45%；
The temperature of second of desulfurization process is 40-45 DEG C, and the time of second of desulfurization process is 2-8s.
In step (3), H in the low sulfur-containing tail gas2S content ＜ 200mg/Nm3。
In step (4), H in the PSA resolution gas2S contents are 200-250mg/Nm3。
In step (4), the absorbing liquid in the desulfuration absorbing tower is sodium carbonate liquor.
In step (4), the temperature of the desulphurization reaction is 40-45 DEG C, and the time of the desulphurization reaction is 2-8s.
In step (4), oxidation regeneration also is carried out to the doctor solution after desulphurization reaction.
Oxidation regeneration also is carried out to the doctor solution after first time desulfurization process and second of desulfurization process, enables doctor solution
Recover to absorb H2The ability of S, the reaction equation that doctor solution carries out oxidation regeneration are as follows：
NaOH+NaHCO3=====Na2CO3+H2O
Na2CO2S+1/2O2=====Na2CO3+S↓
Na2COS2+O2=====Na2CO3+2S↓
The elemental sulfur of generation is separated in the form of sulphur foam from solution, elemental sulfur heating tank be heated to 120 DEG C into
For sulphur cream, become solid sulfur after cooling.
PSA resolution gas refers to the low sulfuric acid gas after raw coke oven gas extraction hydrogen, and coal tar hydrogenating unit sour gas refers to
High sulfuric acid gas after coal tar hydrogenating.
Beneficial effects of the present invention are：
PSA resolution gas of the present invention optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, by coal
High sulfuric acid gas after hydrogenation of tar carries out first time desulfurization process (using sodium carbonate as doctor solution, with Cobalt Phthalocyanine sulphur successively
Hydrochlorate is as catalyst) and second of desulfurization process (using sodium carbonate as doctor solution, using phthalocyanine cobalt sulfonate as catalyst),
Low sulfur-containing tail gas is obtained after gas-liquid separation, low sulfur-containing tail gas and raw coke oven gas are extracted to the PSA resolution gas after hydrogen and mixs, using taking off
After sulphur absorption tower (using sodium carbonate as doctor solution, using DKT-6 as catalyst) carries out Absorption Desulfurization, obtain sulfur-bearing and be less than
50mg/Nm3Desulfurizing and purifying gas, which uses as clean fuel gas；The technology of the present invention realization adds coal tar
High sulfuric acid gas after hydrogen carries out Multistage desulfuration, obtains low sulfur-containing tail gas and is mixed with low sulfuric acid gas, then is passed through desulfurization suction
It receives tower and carries out desulfurization so that desulfurization effect degree of controllability is high, reaches purification requirement；In addition, inventive technique is also to absorbing H2It is de- after S
Sulphur liquid carries out oxidation regeneration, and sulfide forms elemental sulfur, realizes Recovered sulphur.
Description of the drawings
It in order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is attached drawing needed in technology description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention, for those of ordinary skill in the art, without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is PSA resolution gas of the present invention and the technique of coal tar hydrogenating unit sour gas optimization combined desulfurization technology
Flow chart.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical scheme will be carried out below
Detailed description.Obviously, described embodiment is only part of the embodiment of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all on the premise of creative work is not made
Other embodiment belongs to the scope that the present invention is protected.
Embodiment 1
As shown in Figure 1, the present embodiment provides a kind of PSA resolution gas and coal tar hydrogenating unit sour gas to optimize combined desulfurization
Technology includes the following steps：
(1) by high sulfuric acid gas (H after coal tar hydrogenating297%) S is at concentrations up to the first desulfurization reactor is passed through, with carbon
Sour sodium (analysis is pure) is as doctor solution, using phthalocyanine cobalt sulfonate DKT-6 as catalyst, to high sulfuric acid gas in 40 DEG C of conditions
Lower progress first time desulfurization process 8s；Absorb H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs,
Doctor solution recovers to absorb H simultaneously2The ability of S, the elemental sulfur of generation are melted by heating, and discharge cooling and solidifying realizes recycling sulphur
Sulphur；
(2) tail gas by the first desulfurization reactor outlet discharge carries out first time gas-liquid separation, obtains H2S mass percentages
Content is 42% separation gas, and the separation gas is passed through the second desulfurization reactor, using sodium carbonate (analysis pure) as taking off
Sulphur liquid using phthalocyanine cobalt sulfonate DKT-6 as catalyst, carries out second to the separation gas under the conditions of 40 DEG C and takes off
Sulphuring treatment 8s；Absorb H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs, while doctor solution recovers
Absorb H2The ability of S, the elemental sulfur of generation are melted by heating, and discharge cooling and solidifying realizes Recovered sulphur；
(3) tail gas by the second desulfurization reactor outlet discharge carries out second of gas-liquid separation, obtains H2S contents ＜
200mg/Nm3Low sulfur-containing tail gas；
(4) the low sulfur-containing tail gas for obtaining step (3) and the PSA resolution gas (H after raw coke oven gas extraction hydrogen2S contents
For 206.58mg/Nm3) mixing, it is passed through in desulfuration absorbing tower, using sodium carbonate (analysis is pure) as doctor solution, with Cobalt Phthalocyanine sulfonic acid
Salt DKT-6 carries out desulphurization reaction 8s as catalyst under the conditions of 40 DEG C, obtain sulfur content be down to below 50ppm desulfurization it is net
Change gas.
Embodiment 2
The present embodiment provides a kind of PSA resolution gas and coal tar hydrogenating unit sour gas to optimize combined desulfurization technology, including
Following steps：
(1) by high sulfuric acid gas (H after coal tar hydrogenating296%) S is at concentrations up to the first desulfurization reactor is passed through, with carbon
Sour sodium, using phthalocyanine cobalt sulfonate as catalyst, carries out for the first time high sulfuric acid gas as doctor solution under the conditions of 45 DEG C
Desulfurization process 2s；Absorb H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs, while doctor solution is extensive
It relapses and receives H2The ability of S, the elemental sulfur of generation are melted by heating, and discharge cooling and solidifying realizes Recovered sulphur；
(2) tail gas by the first desulfurization reactor outlet discharge carries out first time gas-liquid separation, obtains H2S mass percentages
Content is 35% separation gas, the separation gas is passed through the second desulfurization reactor, using sodium carbonate as doctor solution, with phthalein
Cobalt phthalocyanine monosulfonate carries out second of desulfurization process 2s to the separation gas as catalyst under the conditions of 45 DEG C；It absorbs
H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs, while doctor solution recovers to absorb H2The ability of S,
The elemental sulfur of generation is melted by heating, and discharge cooling and solidifying realizes Recovered sulphur；
(3) tail gas by the second desulfurization reactor outlet discharge carries out second of gas-liquid separation, obtains H2S contents ＜
200mg/Nm3Low sulfur-containing tail gas；
(4) the low sulfur-containing tail gas for obtaining step (3) and the PSA resolution gas (H after raw coke oven gas extraction hydrogen2S contents
200mg/Nm3) mixing, it is passed through in desulfuration absorbing tower, using sodium carbonate as doctor solution, using DKT-6 as catalyst in 45 DEG C of conditions
Lower progress desulphurization reaction 2s, obtains the desulfurizing and purifying gas that sulfur content is down to below 50ppm.
Embodiment 3
The present embodiment provides a kind of PSA resolution gas and coal tar hydrogenating unit sour gas to optimize combined desulfurization technology, including
Following steps：
(1) by high sulfuric acid gas (H after coal tar hydrogenating298%) S is at concentrations up to the first desulfurization reactor is passed through, with carbon
Sour sodium, using phthalocyanine cobalt sulfonate as catalyst, carries out for the first time high sulfuric acid gas as doctor solution under the conditions of 42 DEG C
Desulfurization process 5s；Absorb H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs, while doctor solution is extensive
It relapses and receives H2The ability of S, the elemental sulfur of generation are melted by heating, and discharge cooling and solidifying realizes Recovered sulphur；
(2) tail gas by the first desulfurization reactor outlet discharge carries out first time gas-liquid separation, obtains H2S mass percentages
Content is 45% separation gas, the separation gas is passed through the second desulfurization reactor, using sodium carbonate as doctor solution, with phthalein
Cobalt phthalocyanine monosulfonate carries out second of desulfurization process 5s to the separation gas as catalyst under the conditions of 42 DEG C；It absorbs
H2Doctor solution after S is passed through oxidation regeneration device and desorption reaction production elemental sulfur occurs, while doctor solution recovers to absorb H2The ability of S,
The elemental sulfur of generation is melted by heating, and discharge cooling and solidifying realizes Recovered sulphur；
(3) tail gas by the second desulfurization reactor outlet discharge carries out second of gas-liquid separation, obtains H2S contents ＜
200mg/Nm3Low sulfur-containing tail gas；
(4) the low sulfur-containing tail gas for obtaining step (3) and the PSA resolution gas (H after raw coke oven gas extraction hydrogen2S contents
For 250mg/Nm3) mixing, it is passed through in desulfuration absorbing tower, using sodium carbonate as doctor solution, using DKT-6 as catalyst in 42 DEG C of items
Desulphurization reaction 5s is carried out under part, obtains the desulfurizing and purifying gas that sulfur content is down to below 50ppm.
The above description is merely a specific embodiment, but protection scope of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can readily occur in change or replacement, should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of PSA resolution gas optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, which is characterized in that including as follows
Step：
(1) the high sulfuric acid gas after coal tar hydrogenating is passed through the first desulfurization reactor, using sodium carbonate as doctor solution, with phthalein
Cobalt phthalocyanine monosulfonate carries out first time desulfurization process as catalyst to high sulfuric acid gas；
(2) tail gas by the first desulfurization reactor outlet discharge carries out first time gas-liquid separation, obtains separation gas and is passed through second
Using sodium carbonate as doctor solution, using phthalocyanine cobalt sulfonate as catalyst, second is carried out to the separation gas for desulfurization reactor
Secondary desulfurization process；
(3) tail gas by the second desulfurization reactor outlet discharge carries out second of gas-liquid separation, obtains low sulfur-containing tail gas；
(4) the PSA resolution gas after the low sulfur-containing tail gas that step (3) obtains being extracted hydrogen with raw coke oven gas mixes, and is passed through de-
Sulphur absorption tower carries out desulphurization reaction, obtains desulfurizing and purifying gas.
2. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (1), the phthalocyanine cobalt sulfonate catalyst is DKT-6.
3. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (1), the temperature of the first time desulfurization process is 40-45 DEG C, and the time of the first time desulfurization process is
2-8s；
H in the high sulfuric acid gas2S mass percentages are 96-98%.
4. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (2), H in the separation gas2S mass percentages are 35-45%；
The temperature of second of desulfurization process is 40-45 DEG C, and the time of second of desulfurization process is 2-8s.
5. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (3), H in the low sulfur-containing tail gas2S content ＜ 200mg/Nm3。
6. PSA resolution gas according to claim 5 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (4), H in the PSA resolution gas2S contents are 200-250mg/Nm3。
7. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (4), the absorbing liquid in the desulfuration absorbing tower is sodium carbonate liquor.
8. PSA resolution gas according to claim 7 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (4), the temperature of the desulphurization reaction is 40-45 DEG C, and the time of the desulphurization reaction is 2-8s.
9. PSA resolution gas according to claim 7 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas, special
Sign is, in step (4), also carries out oxidation regeneration to the doctor solution after desulphurization reaction.
10. PSA resolution gas according to claim 1 optimizes combined desulfurization technology with coal tar hydrogenating unit sour gas,
It is characterized in that, oxidation regeneration also is carried out to the doctor solution after first time desulfurization process and second of desulfurization process.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112844492A (en) * | 2021-01-04 | 2021-05-28 | 新疆宣力环保能源有限公司 | Vulcanization method and system of shift reaction catalyst for hydrogen production from raw gas and shift hydrogen production process |
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| CN112844492A (en) * | 2021-01-04 | 2021-05-28 | 新疆宣力环保能源有限公司 | Vulcanization method and system of shift reaction catalyst for hydrogen production from raw gas and shift hydrogen production process |
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Application publication date: 20180529 |