CN102133500B - Method for removing sulfur dioxide in smoke - Google Patents
Method for removing sulfur dioxide in smoke Download PDFInfo
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- CN102133500B CN102133500B CN2011100545349A CN201110054534A CN102133500B CN 102133500 B CN102133500 B CN 102133500B CN 2011100545349 A CN2011100545349 A CN 2011100545349A CN 201110054534 A CN201110054534 A CN 201110054534A CN 102133500 B CN102133500 B CN 102133500B
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- desulfurization lean
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Abstract
The invention discloses a method for removing sulfur dioxide in smoke, comprising the following steps: firstly, washing and spraying smoke for reducing temperature of the smoke; and secondly, contacting the smoke with reduced temperature with desulfuration barren liquor reversely so as to absorb SO2 in the smoke and generate rich liquor containing sulfur, and discharging purified smoke into air, wherein the desulfuration barren liquor, as the effective ingredient, contains macromolecule organic amine expressed by the following general formula, in the formula, R1, R2 and R3 respectively indicate H or alkyl independently, X indicates secondary amino group, tertiary amino group, cyclic annular amido, or hydramine group, and n is any one of integers between 7 and 40. According to the method for removing sulfur dioxide in smoke, the macromolecule organic amine can be regenerated under low energy consumption, and the energy consumption in the regeneration process of sulfur dioxide can be reduced.
Description
Technical field
The present invention relates to a kind of fume desulphurization method, more specifically, relate to a kind of method that removes sulfur dioxide in flue gas.
Background technology
The processing of the raw materials such as crude oil and distillate thereof, natural gas, refinery gas and use all need desulfurization.Along with crude quality becomes bad and environmental regulation increasingly stringent, industrial requirement to desulfur technology is more and more higher.The wet desulphurization treating capacity is large, and operation is continuous, and investment and operating cost are low, and therefore industrial main employing wet desulphurization is processed and contained SO
2Gas.General using liquid desulfurizing agent physics or chemical absorbing SO
2And form rich sulphur solution, the desorb and emit SO again of rich sulphur solution
2Thereby, make desulfurizer regeneration.
Wherein, using organic amine liquid desulfurizing agent to carry out desulfurization is one of method of industrial successful Application.The general employing of a large amount of amine process desulfur technologies that use contained the amine liquid of organic amine as SO at present
2Absorbent is by selective absorption SO
2And and SO
2Thereby reaction and form unstable salt and realize desulfurization.Take off SO
2After flue gas directly discharged after reaching discharge standard, and absorbed SO
2Amine liquid send into again desorber and be heated, vaporize desorb and reclaim.
This desulfurizing agent is to SO
2Absorption selectivity is good, and desulfurizing agent is renewable recycling.Yet also there is following shortcoming in this desulfurizing agent.At first, the regeneration process energy consumption of desulfurizing agent is higher.In addition, repeatedly absorb and the sulfur dioxide of regenerating after, the impurity in desulfurizing agent solution and heavy metal ion content increase, surface tension increases, easily bubbling, liquid flooding.Further this desulfurizing agent has certain corrosiveness to equipment, thereby has affected the stability of sulfur removal technology operation.
Summary of the invention
Purpose of the present invention is intended to solve at least one of above-mentioned technological deficiency, particularly solves the problem that the regeneration steam consumption is large, energy consumption is higher.
In order to achieve the above object, one aspect of the present invention has proposed to remove the method for sulfur dioxide in flue gas, comprises the following steps: (1) washes spray with cooling to flue gas; (2) make flue gas and desulfurization lean solution counter current contacting after cooling, to absorb the SO in described flue gas
2And generate the sulfur-bearing rich solution, and the flue gas after purifying is entered atmosphere, described desulfurization lean solution contains by the represented macromolecule organic amine of following general formula as active ingredient:
In formula, R
1, R
2, R
3Represent independently of one another H or alkyl, X represents secondary amine, tertiary amine groups, cyclic aminocarbonyl or pure amido, and n is 7～40 arbitrary integer.
In addition, the method that removes sulfur dioxide in flue gas according to the above embodiment of the present invention can also have following additional technical characterictic.
According to one embodiment of present invention, the described method that removes sulfur dioxide in flue gas is further comprising the steps: (3) carry out ultrafiltration after with described sulfur-bearing rich solution pressurization, thereby form filtrate and sulfur-bearing concentrate to leach 20～60% water, described filtrate is reclaimed as the desulfurization lean solution.
According to one embodiment of present invention, the described method that removes sulfur dioxide in flue gas is further comprising the steps: (4) are heated to 90 ℃ to 100 ℃ with described sulfur-bearing concentrate, make described sulfur-bearing concentrate be regenerated as the desulfurization lean solution, and generate SO
2Mist with water vapour.
According to one embodiment of present invention, the described method that removes sulfur dioxide in flue gas is further comprising the steps: (5) are carried out demist to the desulfurization lean solution of above-mentioned regeneration and are reclaimed.
According to one embodiment of present invention, the described method that removes sulfur dioxide in flue gas is further comprising the steps: (6) are cooling to carry out gas-liquid separation with described mist, obtain SO
2Gas and water, and reclaim described SO
2Gas is used for making sulfuric acid or sulfur dioxide liquid.
According to some embodiments of the present invention, the aqueous solution that described desulfurization lean solution is is 5wt%～25wt% with the water-soluble concentration that obtains of described macromolecule organic amine, described macromolecule organic amine is obtained by acyl chlorides and the rear polymerization of organic amine reaction.
Described acyl chlorides can be methacrylic chloride.
Described organic amine can be one or more in ethylenediamine, diethylenetriamine, TEPA, piperazine, monoethanolamine, diethanol amine, AEEA.
According to some embodiments of the present invention, described desulfurization lean solution further contains the defoamer of 0.05wt%～4wt%, and described defoamer is silicone based defoamer.
According to some embodiments of the present invention, described desulfurization lean solution further contains the antioxidant of 0.05wt%～3wt%, the activator of 0.05wt%～3wt% and the corrosion inhibiter of 0.01wt%～0.2wt%, described antioxidant is selected from the group that comprises tannic acid, sodium thiosulfate, aldehydes matter, described activator is selected from the group that comprises sodium cetanesulfonate, softex kw, and described corrosion inhibiter is selected from the group that comprises basic copper carbonate, single oily imidazoline.
According to the method that removes sulfur dioxide in flue gas of the present invention, described desulfurization lean solution with sulfur dioxide reaction after form unstable salt, this unstable salt can be with moisture from, the unstable salt after separation desorption major part SO fast when being heated for 90 ℃ to 100 ℃
2, thereby described desulfurization lean solution can regenerate under low energy consumption, and can reduce the energy consumption in the sulfur dioxide regenerative process.
In addition, described desulfurization lean solution can effectively reduce carrying secretly of macromolecule organic amine after demist is reclaimed.
Therefore in addition, because described desulfurization lean solution contains described defoamer, can avoid described desulfurization lean solution bubbling, liquid flooding, and can reduce corrosivity to desulphurization plant by containing described corrosion inhibiter, thereby effectively keep the stability that sulfur removal technology operates.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the flow chart according to the method that removes sulfur dioxide in flue gas of first embodiment of the invention;
Fig. 2 is the flow chart according to the method that removes sulfur dioxide in flue gas of second embodiment of the invention;
Fig. 3 is the flow chart according to the method that removes sulfur dioxide in flue gas of third embodiment of the invention.
The specific embodiment
The below describes embodiments of the invention in detail, and the following examples are exemplary, only is used for explaining the present invention, and can not be interpreted as limitation of the present invention.
The preparation of desulfurization lean solution
take the solvent of carrene as reaction, first add a certain amount of Piperazine anhydrous that it is dissolved in carrene, then add triethylamine (its addition is 1.2～1.5 times of piperazine amount), drip the methacrylic chloride of Isoequivalent weight under ice bath with constant pressure funnel, after reaction, solution revolves the carrene that steams in desolvation and the reactant of not participating in reaction in 20 ℃, products therefrom is polymerization single polymerization monomer, carry out polymerization take potassium peroxydisulfate (addition is as 0.7%～1.5% of monomer mass) as initator, 80 ℃ were reacted 4 hours under nitrogen protection, add at last hydroquinone of polymerization retarder (addition be monomer mass 0.3%～0.8%) to carry out cessation reaction, gained solution is dialysed and is removed molecular weight less than 1000 material, last rotary evaporation dehydration, make the macromolecule organic amine that is shown below.
In formula, n can be 7～40 integer.After this, macromolecule organic amine and the following auxiliary agent of gained are dissolved in the desulfurization lean solution that deionized water obtains 15wt%, wherein, contain the tannic acid of 0.1wt%, the softex kw of 0.1wt%, the silicone based defoamer of 0.2wt%, the basic copper carbonate of 0.05wt%.Need to prove, in the desulfurization lean solution, can also contain as required other auxiliary agents commonly used in the situation that do not affect desulfurized effect.
Need to prove, in order to stop polymerisation, except as the hydroquinone of polymerization retarder that provides in this example, can also realize by adding the chain-transferring agent isopropyl alcohol, its addition is 0.3%～0.8% of monomer mass.Need to prove, as the macromolecule organic amine of the active ingredient in described desulfurization lean solution, except above-mentioned substance, can also use obtained by polymerization after the reaction of acyl chlorides and organic amine, by other represented macromolecule organic amines of following general formula:
In formula, R
1, R
2, R
3Represent independently of one another H or alkyl, X represents secondary amine, tertiary amine groups, cyclic aminocarbonyl or pure amido, and n is 7～40 arbitrary integer.
Particularly, as acyl chlorides, can use methacrylic chloride.As organic amine, can use one or more in ethylenediamine, diethylenetriamine, TEPA, piperazine, monoethanolamine, diethanol amine, AEEA.
The aqueous solution that described desulfurization lean solution can be is 5wt%～25wt% with the water-soluble concentration that obtains of above-mentioned macromolecule organic amine.
In this example, as defoamer, contain the silicone based defoamer of 0.2wt% in the desulfurization lean solution.The content of described defoamer can be in 0.05wt%～4wt% scope.Contain above-mentioned defoamer in described desulfurization lean solution, can reduce the surface tension of described desulfurization lean solution, thereby can avoid described desulfurization lean solution bubbling, liquid flooding, and then effectively keep the stability of sulfur removal technology operation.
In this example, as corrosion inhibiter, also contain the basic copper carbonate of 0.05wt% in the desulfurization lean solution.Except the basic copper carbonate that uses in this example, can also select single oily imidazoline and other materials with similar effect as corrosion inhibiter.The content of corrosion inhibiter is preferably in 0.01wt%～0.2wt% scope.Contain above-mentioned corrosion inhibiter in described desulfurization lean solution, can reduce solution in the absorption tower to the corrosivity of desulphurization plant, further effectively keep the stability of sulfur removal technology operation.
In this example, further contain the tannic acid as antioxidant of 0.1wt% in described desulfurization lean solution, and the softex kw as activator of 0.1wt%.
As antioxidant, except the tannic acid that uses in this example, can also be selected from the group that comprises sodium thiosulfate, aldehydes matter.The content of described antioxidant is preferably in 0.05wt%～3wt% scope.Contain above-mentioned antioxidant in described desulfurization lean solution, can make described macromolecule organic amine have excellent non-oxidizability.
As activator, except the softex kw that uses in this example, can also use sodium cetanesulfonate and similar compound.The content of described activator is preferably in 0.05wt%～3wt% scope.Above-mentioned activator can make described macromolecule organic amine keep high activity, long-life.
Below with reference to accompanying drawing and specific embodiment and experimental example, the method for utilizing above-mentioned desulfurization lean solution to remove sulfur dioxide in flue gas is described.
Embodiment 1
Fig. 1 shows the flow chart according to the method that removes sulfur dioxide in flue gas of first embodiment of the invention.As shown in Figure 1, at first flue gas is washed spray with cooling.Then, make flue gas after cooling and the desulfurization lean solution counter current contacting of above-mentioned preparation gained, the SO in described macromolecule organic amine and described flue gas
2Reaction generates unsettled macromolecule organic amine salt, and the mixture of described macromolecule organic amine salt and water is called the sulfur-bearing rich solution, and the flue gas after purifying enters atmosphere.
Embodiment 2
Fig. 2 shows the flow chart according to the method that removes sulfur dioxide in flue gas of second embodiment of the invention.The difference of the present embodiment and embodiment 1 is: the sulfur-bearing rich solution is processed, to reclaim the desulfurization lean solution.
As shown in Figure 2, due to macromolecule organic amine salt can with moisture from, will be described carry out ultrafiltration after the pressurization of sulfur-bearing rich solution, thereby form filtrate and sulfur-bearing concentrate to leach 20～60% water, described filtrate is reclaimed as the desulfurization lean solution, can be reused for absorption SO
2Thus, can improve on the one hand the organic efficiency of desulfurization lean solution, simultaneously, can reduce the amount of liquid (being the sulfur-bearing concentrate) that regeneration is processed, thereby can further reduce the regeneration energy consumption.
Then, described sulfur-bearing concentrate is heated to 90 ℃ to 100 ℃, can the most of SO of quick desorption when macromolecule organic amine salt is heated in this temperature range
2And the regeneration macromolecule organic amine, thereby make described sulfur-bearing concentrate be regenerated as the desulfurization lean solution, and obtain SO
2Mist with water vapour.
Then, the desulfurization lean solution of above-mentioned regeneration is carried out demist reclaim, the desulfurization lean solution after recovery can be reused for and absorb SO
2
Thus, according to the method that removes sulfur dioxide in flue gas of the embodiment of the present invention, described macromolecule organic amine can be regenerated under low energy consumption, and can reduce the energy consumption in the sulfur dioxide regenerative process.It is estimated that, the heat exhaustion that is used for the regeneration processing in the present embodiment is only 50%～80% left and right of the existing organic amine desulfurizer under similarity condition, has reduced significantly energy consumption.And owing to the desulfurization lean solution of regenerating under high temperature having been carried out the demist recovery, can effectively reduce thus carrying secretly of organic amine, carry thereby can reduce the loss that causes secretly.
Embodiment 3
Fig. 3 shows the flow chart according to the method that removes sulfur dioxide in flue gas of third embodiment of the invention.The difference of the present embodiment and embodiment 2 is: resulting SO in the regeneration process to desulfurizing agent
2Process with the mist of water vapour, to reclaim SO
2Gas.
As shown in Figure 3, described mist is cooled to 40 ℃ to carry out gas-liquid separation, obtains SO
2Gas and water.Described SO
2Gas purity can reach 99%, can be used for making sulfuric acid or sulfur dioxide liquid.Water after recovery can be reused for flue gas is washed spray.Thus, one side has solved and has contained SO
2The problem of environmental pollution of flue gas, flue gas has also obtained sufficient recycling simultaneously.
Experimental example
Method based on embodiment 1 is processed the sulfur-containing smoke gas of three kinds of variable concentrations, and its result is as shown in table 1.
Table 1
As shown in Table 1, utilize according to the method that removes sulfur dioxide in flue gas of the present invention, desulfuration efficiency all can reach more than 99%.
In the description of this specification, the description of reference term " embodiment ", " some embodiment " or " example " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the characteristics of this embodiment or example description.In this manual, the schematic statement of above-mentioned term not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or characteristics can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that in the situation that do not break away from principle of the present invention and aim can be carried out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claim and equivalent thereof.
Claims (10)
1. method that removes sulfur dioxide in flue gas comprises the following steps:
(1) flue gas is washed spray with cooling;
(2) make flue gas and desulfurization lean solution counter current contacting after cooling, to absorb the SO in described flue gas
2And generate the sulfur-bearing rich solution, the flue gas after purifying is entered atmosphere,
Wherein, as active ingredient, described desulfurization lean solution contains by the represented macromolecule organic amine of following general formula:
In formula, R
1, R
2, R
3Represent independently of one another H or alkyl, X represents secondary amine, tertiary amine groups, cyclic aminocarbonyl or pure amido, and n is 7 ~ 40 arbitrary integer.
2. method according to claim 1, is characterized in that, and is further comprising the steps:
(3) will be described carry out ultrafiltration after the pressurization of sulfur-bearing rich solution, thereby form filtrate and sulfur-bearing concentrate to leach 20 ~ 60% water, described filtrate will be reclaimed as the desulfurization lean solution.
3. method according to claim 2, is characterized in that, and is further comprising the steps:
(4) described sulfur-bearing concentrate is heated to 90 ℃ to 100 ℃, makes described sulfur-bearing concentrate be regenerated as the desulfurization lean solution, and generate SO
2Mist with water vapour.
4. method according to claim 3, is characterized in that, further comprises the steps:
(5) the desulfurization lean solution of regeneration being carried out demist reclaims.
5. method according to claim 3, is characterized in that, further comprises the steps:
(6) described mist is cooling to carry out gas-liquid separation, obtain SO
2Gas and water, and reclaim described SO
2Gas is used for making sulfuric acid or sulfur dioxide liquid.
6. method according to claim 1, is characterized in that, the aqueous solution that described desulfurization lean solution is is 5wt% ~ 25wt% with the water-soluble concentration that obtains of described macromolecule organic amine, and described macromolecule organic amine is obtained by acyl chlorides and the rear polymerization of organic amine reaction.
7. method according to claim 6, is characterized in that, described acyl chlorides is methacrylic chloride.
8. method according to claim 6, is characterized in that, described organic amine is a kind of in ethylenediamine, diethylenetriamine, TEPA, piperazine, monoethanolamine, diethanol amine, AEEA.
9. method according to claim 1, is characterized in that, described desulfurization lean solution further contains the defoamer of 0.05wt% ~ 4wt%, and described defoamer is silicone based defoamer.
10. method according to claim 1, it is characterized in that, described desulfurization lean solution further contains the antioxidant of 0.05wt% ~ 3wt%, the activator of 0.05wt% ~ 3wt% and the corrosion inhibiter of 0.01wt% ~ 0.2wt%, described antioxidant is selected from the group of tannic acid, sodium thiosulfate, aldehydes matter composition, described activator is selected from the group of sodium cetanesulfonate, softex kw composition, and described corrosion inhibiter is selected from the group of basic copper carbonate, single oily imidazoline composition.
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| CN2011100545349A CN102133500B (en) | 2011-03-07 | 2011-03-07 | Method for removing sulfur dioxide in smoke |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102657999A (en) * | 2012-05-31 | 2012-09-12 | 北京化工大学 | Poly (tetramethylguandium acrylate) aqueous solution desulfurization agent and preparation method thereof |
| CN109663484A (en) * | 2017-10-17 | 2019-04-23 | 中国石油化工股份有限公司 | High performance vulcanization hydrogen inhales disappear liquid and purposes |
| CN110787601B (en) * | 2018-08-01 | 2021-11-30 | 中国石油天然气股份有限公司 | Heat-stable salt inhibitor for desulfurization system and solvent for removing sulfur dioxide |
| CN114432841A (en) * | 2020-10-20 | 2022-05-06 | 中国石油化工股份有限公司 | Absorption of low concentration SO2Bifunctional absorbent for catalyzing Claus reaction and preparation thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3764665A (en) * | 1971-02-19 | 1973-10-09 | Shell Oil Co | Combined sulfur oxides acceptance-sulfur recovery process |
| US4871521A (en) * | 1987-09-18 | 1989-10-03 | Amoco Corporation | Sulfur recovery process using metal oxide absorbent with improved purge |
| CN101507891A (en) * | 2009-02-24 | 2009-08-19 | 江苏大海水处理设备有限公司 | Liquid composition capable of removing sulfide in gas |
| CN101537304A (en) * | 2009-04-17 | 2009-09-23 | 合肥工业大学 | Cyclic amine sulfur dioxide gas absorbent and preparation method thereof |
-
2011
- 2011-03-07 CN CN2011100545349A patent/CN102133500B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3764665A (en) * | 1971-02-19 | 1973-10-09 | Shell Oil Co | Combined sulfur oxides acceptance-sulfur recovery process |
| US4871521A (en) * | 1987-09-18 | 1989-10-03 | Amoco Corporation | Sulfur recovery process using metal oxide absorbent with improved purge |
| CN101507891A (en) * | 2009-02-24 | 2009-08-19 | 江苏大海水处理设备有限公司 | Liquid composition capable of removing sulfide in gas |
| CN101537304A (en) * | 2009-04-17 | 2009-09-23 | 合肥工业大学 | Cyclic amine sulfur dioxide gas absorbent and preparation method thereof |
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