CN100518892C - Method and device for removing hydrogen sulphide from mixture gas containing low-concentration hydrogen sulphide - Google Patents
Method and device for removing hydrogen sulphide from mixture gas containing low-concentration hydrogen sulphide Download PDFInfo
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- CN100518892C CN100518892C CNB2007100416962A CN200710041696A CN100518892C CN 100518892 C CN100518892 C CN 100518892C CN B2007100416962 A CNB2007100416962 A CN B2007100416962A CN 200710041696 A CN200710041696 A CN 200710041696A CN 100518892 C CN100518892 C CN 100518892C
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Abstract
The invention provides a H2s removing method from the gas mixture, comprising a provision of absorption of liquid, with the solution selected from N-methyl diethanolamine, aminoethanol and their mixture, under 0. 05-0. 30MPa absolute pressure, keeping the 18-42deg.C absorption liquid contact with the 20-52deg.C low density H2S gas, absorbing mixture gas through countercurrent and vortex, lowering the mixture gas H2S into 10ppm or even lower, separating the mixture gas for swirl gas and liquid separation. It also provides a low density H2S gas mixture to remove it.
Description
Technical field
The present invention relates to absorb the method for low concentration hydrogen sulphide gas, specifically, relate to the method for from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide.The invention still further relates to the device of from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide.
Background technology
Hydrogen sulfide is a kind of high irritating gas, has strong rotten egg smell, and is very big to the toxicity of human body, and inflammable and explosive, and very easily corroding metal causes catalyst poisoning, blocking pipe.Also can cause very big pollution even contain a spot of hydrogen sulfide in factory's discharge tail gas and the natural gas to environment.All can produce many low concentration hydrogen sulphide foul gas in the industrial process such as Coal Chemical Industry, rubber regeneration, sewage sludge and treatment of urban garbage, not only have a strong impact on daily life, be detrimental to health, the while is pollution of ecological environment also.Because the concentration of hydrogen sulfide is low in this class waste gas, do not had the value of recycling, but the purified treatment difficulty is big and expense is high, thereby is a difficult problem of industrial waste gas purifying.So the eliminating of hydrogen sulfide, especially low concentration hydrogen sulphide is current urgent problem.
China has strict regulation to the concentration of hydrogen sulfide in ambient air, workshop air and the industrial waste gas: the concentration of hydrogen sulfide is the highest in the ambient air of residential block must not surpass 0.01mg/m
3The concentration of shopwork place Air Hydrogen Sulfide is the highest must not to surpass 10mg/m
3The concentration of hydrogen sulfide must not surpass 20mg/m in the town gas
3The concentration requirement of hydrogen sulfide purifies to 10-20mg/m in the oil product refinery waste gas
3Because hydrogen sulfide has strong reducing property, itself is very easily oxidized, there are human transition metal oxide and hopcalite to come the oxidation removal low concentration hydrogen sulphide, also there is the human active carbon to come oxidation of sulfureted hydrogen to remove the hydrogen sulfide in the gaseous mixture, the low concentration hydrogen sulphide foul gas in the human aerobic microbiological purified industrial waste gas is also arranged as catalyst.But at the big and low commercial plant of concentration of hydrogen sulfide in the gaseous mixture of some mist discharge capacities, mainly there are one or more of following problem in above processing method and device:
1. the gas treatment amount is little, the hydrogen sulfide stripping rate is low;
2. regeneration of absorption solution difficulty;
3. floor space is big;
4. the absorption liquid waste is serious;
5. cost is higher.
Therefore, at the existing problem that exists be necessary to adopt novel, effectively, be fit to the absorption process and the device of long-term operation and economic low concentration hydrogen sulphide.
Summary of the invention
The invention provides a kind of method and device of removing the low concentration hydrogen sulphide in the mist, thereby solve the absorption problem of low concentration hydrogen sulphide gas effectively, eliminate the stench in the gaseous mixture, advanced the process of industrialization of petrochemical industry cleaning and safety in production.
On the one hand, the invention provides a kind of method of from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide, it comprises: absorption liquid is provided, and described absorption liquid is selected from N-Propylene Glycol amine aqueous solution, monoethanolamine solution, diethanolamine solution and their mixture; Under the absolute pressure of 0.05-0.30MPa, the mist that comprise low concentration hydrogen sulphide gas of 12-42 ℃ absorption liquid with 12-52 ℃ contacted, described mist is carried out counter-current absorption and eddy flow successively absorb, make the concentration of hydrogen sulfide in the described mist reduce to 10ppm or lower; And the mist of carrying described absorption liquid secretly is carried out cyclone gas-liquid separate.
One preferred embodiment in, described absorption liquid also comprises additive, described additive comprises that the N-methyl gives a tongue-lashing pyrrolidone, triethanolamine, sulfolane or diglycol.
Another preferred embodiment in, described absorption liquid is that mass fraction is the N-Propylene Glycol amine aqueous solution of 10-50%.
On the other hand, the invention provides a kind of device of from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide, it comprises: be positioned at the liquid storage cylinder that is used to store absorption liquid of bottom of device, described absorption liquid is selected from N-Propylene Glycol amine aqueous solution, monoethanolamine solution, diethanolamine solution and their mixture; Be positioned at the counter-current absorber and the eddy flow absorber at device middle part, be used under the absolute pressure of 0.05-0.30MPa, the mist that comprise low concentration hydrogen sulphide gas of 12-42 ℃ absorption liquid with 12-52 ℃ contacted, described mist is carried out counter-current absorption and eddy flow successively absorb, make the concentration of hydrogen sulfide in the described mist reduce to 10ppm or lower; And the cyclone gas-liquid separator that is positioned at the device top, be used for that the mist of carrying described absorption liquid secretly is carried out cyclone gas-liquid and separate.
One preferred embodiment in, described counter-current absorber is selected from plate column and packed tower.
Another preferred embodiment in, when described counter-current absorber is plate column, use cyclone-type tower tray, float valve type tower tray or sieve plate type tower tray; When described counter-current absorber is packed tower, use Raschig ring, cascade ring or Pall ring as filler.
Another preferred embodiment in, when described counter-current absorber was packed tower, the underflow of described eddy flow absorber outlet was provided with the atomizing irrigation device, described atomizing irrigation device is selected from ultrasonic atomization liquid distributor and swirling flow atomizing liquid distributor.
Another preferred embodiment in, described cyclone gas-liquid separator is three centrum gas-liquid cyclone separators.
In another preferred implementation, described device also is provided with hydrogen sulfide fast detecting instrument, in order to measure the variation of concentration of hydrogen sulfide in the mist, controls the rotating speed of frequency conversion circulating pump by the variation of concentration of hydrogen sulfide; Described frequency conversion circulating pump is controlled gas liquid ratio in the described device running by adjusting rotating speed.
Another preferred embodiment in, the operating pressure of described device is not more than 0.6Mpa, and/or absorbs temperature less than 52 ℃.
Another preferred embodiment in, the gas-liquid volume ratio of described device is 60-120.
Description of drawings
Fig. 1 is the schematic representation of apparatus of hydrogen sulfide gas that is used for absorbing the mist that the coke cooling water hot-water cylinder discharges according to one embodiment of the present invention.
The specific embodiment
The present inventor is through finding after the extensive and deep research, remove the hydrogen sulfide of low concentration in the mist that comes out for the coke drum from the coke cooling water treatment system of delayed coking, with the counter-current absorption technology, the eddy flow absorption techniques, and cyclone separation process organically combines, can solve the absorption problem of low concentration hydrogen sulphide gas effectively, treating capacity is big, infiltration rate is fast, energy consumption is low, tail gas after the absorption reaches discharging standards, and can significantly reduce the waste of absorption liquid, reduce cost, the solution that absorbs after saturated is renewable recycling, thereby has solved the problem that concentration of hydrogen sulfide exceeds standard in the existing coke-cooling waste water sealing and circulating corollary apparatus effectively.Based on above-mentioned discovery, the present invention is accomplished.
In a first aspect of the present invention, a kind of method of removing hydrogen sulfide from the mist that comprises low concentration hydrogen sulphide gas is provided, it may further comprise the steps:
Absorption liquid is provided, and described absorption liquid is an aqueous alkanolamine, comprises N-Propylene Glycol amine aqueous solution (MDEA), monoethanolamine solution (MEA), diethanolamine solution (DEA) or their mixture; By selecting different absorption liquids to improve selectivity, the desulfurization degree of hydrogen sulfide or reducing cost; Described hydramine shows alkalescence and the reaction of sour gas hydrogen sulfide by unpaired electronics on the nitrogen-atoms;
Under the absolute pressure of 0.05-0.30MPa, the mist that comprise low concentration hydrogen sulphide gas of 12-42 ℃ absorption liquid with 12-52 ℃ contacted, described mist is carried out counter-current absorption and eddy flow successively absorb, make the concentration of hydrogen sulfide in the described mist reduce to 10ppm or lower from maximum 100ppm; And
The mist of carrying described absorption liquid secretly is carried out cyclone gas-liquid to be separated.
In one embodiment, at different mist character, can be chosen in and add additive in the absorption liquid.Described additive comprises that the N-methyl gives a tongue-lashing pyrrolidone (NMP), triethanolamine (TEA), sulfolane (SF), diglycol (DEG) etc. as physical solvent.Add and to improve the selectivity of desulfurization after the N-methyl is given a tongue-lashing pyrrolidone (NMP), diglycol (DEG), sulfolane physical solvents such as (SF), and the regenerability of absorption liquid is improved; Interpolation triethanolamine (TEA) can improve the desulfuration efficiency to hydrogen sulfide, has also increased the degree of removing to carbon dioxide in the mist, causes the reproducibility quality of desulfurization lean solution to descend.
In another embodiment, described absorption liquid preferably mass fraction (ω t) be the N-Propylene Glycol amine aqueous solution of 10-50%.
In a second aspect of the present invention, a kind of device of removing hydrogen sulfide from the mist that comprises low concentration hydrogen sulphide gas is provided, it comprises: absorption tower and optional hydrogen sulfide fast detecting instrument, frequency converter and frequency conversion circulating pump.
Described absorption tower comprises:
Liquid storage cylinder: described liquid storage cylinder is positioned at the bottom on absorption tower, selects the tower diameter identical or bigger slightly than absorber portion with the absorber portion on following absorption tower, and the capacity of storage solutions is 15 minutes absorption liquid internal circulating load (m
3); Be provided with the absorption liquid outlet in the bottom of liquid storage cylinder, liquid storage cylinder is provided with liquid level gauge, so that observe the operating position of liquid storage intracavity liquid;
Absorber portion: described absorber portion is positioned at the middle part on absorption tower, comprises counter-current absorber and eddy flow absorber two parts; Wherein, counter-current absorption adopts the absorption pattern of plate column or packed tower; If the solia particle impurity content in the mist is bigger, then select for use plate column to carry out counter-current absorption, select cyclone-type tower tray, float valve type tower tray or sieve plate type tower tray for use; If the solid particle polluter content in the mist is less, then select for use packed tower to carry out counter-current absorption, select for use Raschig ring, cascade ring or Pall ring as filler; The underflow opening of described eddy flow absorber (absorption liquid outlet) is consistent with the caliber size of absorption liquid import, and overfall (mixed gas outlet) is consistent with the caliber size of combi inlet port; The frequency conversion outlet of circulating pump links to each other with the absorption liquid import; Wherein, under the absolute pressure of 0.05-0.30MPa, open the cat head mixed gas outlet, being 20-52 ℃, the gaseous mixture of sulfureted hydrogen gas concentration≤100ppm at the bottom of the tower with temperature, combi inlet port feeds the absorption tower, carry out counter current contacting with the absorption liquid that flows downward, at bubbling area generation absorption reaction, gases such as the hydrogen sulfide in the gas and a spot of carbon dioxide are dissolved in the absorption liquid; Gas enters behind absorption reaction successively and carries out secondary in the eddy flow absorber and absorb, and the concentration of hydrogen sulfide gas is reduced to 10ppm or lower in the gaseous mixture after the absorption; Simultaneously, under the absolute pressure of 0.05-0.30MPa, 18-42 ℃ absorption liquid is contacted absorption with the gaseous mixture of process counter-current absorber from cat head absorption liquid import feeding eddy flow absorber, underflow opening by the eddy flow absorber flows out to enter in the counter-current absorber and carries out counter current contacting with the gaseous mixture that rises, the concentration of contained hydrogen sulfide raises gradually in the absorption liquid, enters liquid storage cylinder by downspout at last; And
The rotational flow separation section: the absorption liquid that described rotational flow separation section adopts three centrum cyclone gas-liquid separators that gaseous mixture is carried secretly reclaims, and this cyclone gas-liquid separator adopts the double feed inlet form; Overfall is a mixed gas outlet, and the sectional area of overfall equals two import sectional area sums; Underflow opening exports for the liquid of carrying secretly that reclaims, and the underflow section is designed to long and thin pipe and inserts the counter-current absorption section; Mist has removed the mist of the absorption liquid of carrying secretly and discharged from the gaseous phase outlet on absorption tower, and the absorption liquid of carrying secretly greatly reduces the loss of absorption liquid like this by the cyclone gas-liquid separator recycling by behind the cyclone gas-liquid separator.
In one embodiment, when described counter-current absorber was packed tower, the outlet of the underflow of described eddy flow absorber was provided with the atomizing irrigation device, and described atomizing irrigation device is selected from ultrasonic atomization liquid distributor and swirling flow atomizing liquid distributor.
The operating pressure on described absorption tower is not more than 0.6Mpa.
In another embodiment, on the inlet line on absorption tower, be provided with hydrogen sulfide fast detecting instrument,, control the rotating speed of frequency conversion circulating pump by the variation of concentration of hydrogen sulfide in order to measure the variation of concentration of hydrogen sulfide in the mist.
In another embodiment, variable frequency pump is controlled gas liquid ratio in the running of absorption tower by adjusting rotating speed.
In another embodiment, the absorption temperature on described absorption tower is less than 52 ℃.
In another embodiment, the gas-liquid volume ratio on described absorption tower is 60-120.
In another embodiment, described absorption tower also is provided with manhole, gas pilot outlet, relief valve connection and absorption liquid pilot outlet.
Below referring to accompanying drawing.Fig. 1 shows the device (absorption tower) of hydrogen sulfide gas that is used for absorbing the mist that the coke cooling water hot-water cylinder discharges according to one embodiment of the present invention.The bottom on absorption tower is provided with the liquid storage cylinder 14 that is used to store absorption liquid.Be provided with the absorption liquid outlet 13 that is connected with frequency conversion circulating pump 11 at the bottom of the tower on absorption tower.Absorption liquid feeds the absorption towers from the absorption liquid import 5 on absorption tower, observes the double-colored liquid level meter 10 that absorbs at the bottom of the Tata, treats that absorption liquid reaches to stop to inject after 15 minutes the circulation fluid use amount to absorb lean solution.Open frequency conversion circulating pump 11, gas liquid ratio is chosen between the 80-120, and the absorption tower is in steady-state operation.Under the absolute pressure of 0.15MPa, open the mixed gas outlet 1 of absorption tower cat head, the combi inlet port 9 of 20-52 ℃ gaseous mixture from the absorption tower fed the absorption tower, gaseous mixture enters the 8 back gas phase imports 6 and 17 from eddy flow absorber 4 of counter-current absorption section by tower tray and enters, and the absorption liquid of coming in absorption liquid import 5 carries out eddy flow absorption back is entered the absorption tower cat head by the gaseous phase outlet 3 of eddy flow absorber 4 cyclone gas-liquid separator 18.After the gaseous mixture of carrying absorption liquid secretly feeds cyclone gas-liquid separators 18 by import 19, by rotational flow separation mist is separated with the absorption liquid of carrying secretly, remove of top overfall 21 emptyings of the gaseous mixture of absorption liquid from cyclone gas-liquid separator, the absorption liquid of carrying secretly then returns absorber portion by the underflow opening 16 of cyclone gas-liquid separator bottom, reclaims and continues to utilize.By the double colored indicator at the bottom of the observing tower 10, regularly absorption liquid is carried out supply, make circulation fluid remain 15 minutes consumption.In addition, described absorption tower also is provided with gas pilot outlet 20 and absorption liquid pilot outlet 12, and relief valve connection 2, and manhole 15 is located between the 4th and the 5th block of column plate.
In addition, can establish a hydrogen sulfide fast detecting instrument in the gas phase inlet line on absorption tower, according to the variation control frequency conversion circulating pump of concentration of hydrogen sulfide, the control gas liquid ratio is to reach the effect that cuts down the consumption of energy.
The major advantage of method and apparatus of the present invention is:
1. solved the absorption problem of low concentration hydrogen sulphide gas effectively, infiltration rate is fast, energy consumption is low, and the tail gas after the absorption reaches discharging standards, has removed the stench of H 2 S-containing gas greatly;
2. significantly reduced the waste of absorption liquid, reduced cost, the solution that absorbs after saturated is renewable recycling, has prolonged the stable operation cycle of system.
Further set forth the present invention below in conjunction with specific embodiment.But, should be understood that these embodiment only are used to the present invention is described and do not constitute limitation of the scope of the invention.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.Except as otherwise noted, all percentage and umber are by weight.
Embodiment
In the burnt watertight circulatory system of 2,500,000 tons of/year System of Cool Coking of Delayed Coking, according to method of the present invention an absorption tower is set, in order to the hydrogen sulfide gas in the mist that absorbs cold burnt hot-water cylinder discharge, and then the stench in the removal gaseous mixture, its concrete operation and effect are described below:
1. the character of gaseous mixture
The capacity V=600m of coking hot-water cylinder
3/ h, coking hot-water cylinder escape pipe is DN400mm; Mist consist of air, steam and a spot of hydrogen sulfide gas, wherein, the content of hydrogen sulfide is not more than 100ppm, temperature is 80-90 ℃.
2. the character of absorption liquid
The absorption liquid that adopts is 30% N-Propylene Glycol amine aqueous solution (MDEA), adds concentration and be 10% triethanolamine (TEA) as additive.
3. install on (absorption tower)
The absorption tower is divided into three sections, is followed successively by liquid storage section, absorber portion and segregation section from down to up.The about 6.3m of tower height, this tower are the variable cross-section tower, and the diameter of liquid storage section is 1.2m, and the tower diameter of absorber portion and segregation section is 1m.Absorber portion absorbs two parts by board-like absorption and eddy flow to be formed, and one has 9 F1 ballast valve traies; The eddy flow absorber adopts the HL/AG-300 model.Segregation section adopts the cyclone gas-liquid separator of HL/G-300 model.
4. implementation process:
Under the absolute pressure of 0.05MPa, the absorption liquid import 5 of 18-42 ℃ absorption liquid from the absorption tower fed the absorption towers, observe the double-colored liquid level meter 10 that absorbs at the bottom of the Tata, treat that absorption liquid reaches to stop to inject after 15 minutes the circulation fluid use amount and absorb lean solution.Open frequency conversion circulating pump 11, gas liquid ratio is chosen between the 80-120, and the absorption tower is in steady-state operation.Under the absolute pressure of 0.15MPa, open the mixed gas outlet 1 of absorption tower cat head, the combi inlet port 9 of 20-52 ℃ gaseous mixture from the absorption tower fed the absorption tower, gaseous mixture enters counter-current absorber 8 back and enters from the gas phase imports 6 and 17 of eddy flow absorber 4, and the absorption liquid of coming in absorption liquid import 5 carries out entering after eddy flow absorbs the cyclone gas-liquid separator 18 of absorption tower cat head.After the gaseous mixture of carrying absorption liquid secretly feeds cyclone gas-liquid separators 18 by import 19, by rotational flow separation mist is separated with the absorption liquid of carrying secretly, remove of top overfall 21 emptyings of the gaseous mixture of absorption liquid from cyclone gas-liquid separator, the absorption liquid of carrying secretly then returns absorber portion by the underflow opening 16 of cyclone gas-liquid separator bottom, reclaims and continues to utilize.By the double colored indicator at the bottom of the observing tower 10, regularly absorption liquid is carried out supply, make circulation fluid remain 15 minutes consumption.
5. interpretation of result
After mist installed by this, the content of hydrogen sulfide gas was dropped to below the 8ppm by 89ppm, and the stench of gaseous mixture also reduces greatly.Can use 30-50 days according to 15 minutes absorption liquid of different gas liquid ratios, after cyclone gas-liquid separator was set, the absorption liquid loss amount also reduced greatly.
From the foregoing description obviously as can be seen, adopt method of the present invention and device, can solve the absorption problem of low concentration hydrogen sulphide gas reliably, remove the stench of H 2 S-containing gas widely, and can solve the loss problem of absorption liquid effectively, prolonged the stable operation cycle of system.
All quote in this application as a reference at all documents that the present invention mentions, just quoted as a reference separately as each piece document.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after having read above-mentioned instruction content of the present invention, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Claims (10)
1. method of from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide, it comprises:
Absorption liquid is provided, and described absorption liquid is selected from N-Propylene Glycol amine aqueous solution, monoethanolamine solution, diethanolamine solution and their mixture;
Under the absolute pressure of 0.05-0.30MPa, the mist that comprise low concentration hydrogen sulphide gas of 18-42 ℃ absorption liquid with 20-52 ℃ contacted, described mist is carried out counter-current absorption and eddy flow successively absorb, make the concentration of hydrogen sulfide in the described mist reduce to 10ppm or lower; And
The mist of carrying described absorption liquid secretly is carried out cyclone gas-liquid to be separated.
2. the method for claim 1 is characterized in that, described absorption liquid also comprises additive, and described additive comprises that the N-methyl gives a tongue-lashing pyrrolidone, triethanolamine, sulfolane or diglycol.
3. method as claimed in claim 1 or 2 is characterized in that, described absorption liquid is that mass fraction is the N-Propylene Glycol amine aqueous solution of 23-50%.
4. device of from the mist that comprises low concentration hydrogen sulphide gas, removing hydrogen sulfide, it comprises:
Be positioned at the liquid storage cylinder that is used to store absorption liquid (14) of bottom of device, described absorption liquid is selected from N-Propylene Glycol amine aqueous solution, monoethanolamine solution, diethanolamine solution and their mixture;
Be positioned at the counter-current absorber (8) and the eddy flow absorber (4) at device middle part, be used under the absolute pressure of 0.05-0.30MPa, the mist that comprise low concentration hydrogen sulphide gas of 18-42 ℃ absorption liquid with 20-52 ℃ contacted, described mist is carried out counter-current absorption and eddy flow successively absorb, make the concentration of hydrogen sulfide in the described mist reduce to 10ppm or lower; And
Be positioned at the cyclone gas-liquid separator (18) at device top, be used for that the mist of carrying described absorption liquid secretly is carried out cyclone gas-liquid and separate.
5. device as claimed in claim 4 is characterized in that described counter-current absorber is selected from plate column and packed tower, wherein, when described counter-current absorber is plate column, uses cyclone-type tower tray, float valve type tower tray or sieve plate type tower tray; When described counter-current absorber is packed tower, use Raschig ring, cascade ring or Pall ring as filler.
6. device as claimed in claim 5 is characterized in that, when described counter-current absorber was packed tower, the outlet of the underflow of described eddy flow absorber was provided with the atomizing irrigation device, and described atomizing irrigation device is selected from ultrasonic atomization liquid distributor and swirling flow atomizing liquid distributor.
7. as claim 4 or 5 described devices, it is characterized in that described cyclone gas-liquid separator is three centrum gas-liquid cyclone separators.
8. as claim 4 or 5 described devices, described device also is provided with hydrogen sulfide fast detecting instrument, in order to measure the variation of concentration of hydrogen sulfide in the mist, controls the rotating speed of frequency conversion circulating pump by the variation of concentration of hydrogen sulfide; Described frequency conversion circulating pump is controlled gas liquid ratio in the described device running by adjusting rotating speed.
9. as claim 4 or 5 described devices, it is characterized in that the operating pressure of described device is not more than 0.6Mpa, and/or absorb temperature less than 52 ℃.
10. as claim 4 or 5 described devices, it is characterized in that the gas-liquid volume ratio of described device is 60-120.
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| CNB2007100416962A CN100518892C (en) | 2007-06-07 | 2007-06-07 | Method and device for removing hydrogen sulphide from mixture gas containing low-concentration hydrogen sulphide |
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