CN211521596U - System for preparing analytically pure sulfuric acid from smelting flue gas - Google Patents
System for preparing analytically pure sulfuric acid from smelting flue gas Download PDFInfo
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- CN211521596U CN211521596U CN202020124151.9U CN202020124151U CN211521596U CN 211521596 U CN211521596 U CN 211521596U CN 202020124151 U CN202020124151 U CN 202020124151U CN 211521596 U CN211521596 U CN 211521596U
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Abstract
The utility model discloses a system for smelt flue gas preparation assay pure sulphuric acid, this system is including the washing cooling tower that communicates in proper order, the electric demister, the sulfur dioxide absorption tower, the sulfur dioxide desorber, join in marriage the gas pitcher, the drying tower, conversion system, system acid absorption tower and degasser, be equipped with between sulfur dioxide absorption tower and the sulfur dioxide desorber and be used for sending the rich liquid of absorption liquid that the sulfur dioxide absorption tower produced to the sulfur dioxide desorber, send the absorption liquid barren liquor that the sulfur dioxide desorber produced to the sulfur dioxide absorption tower and carry out the barren liquor heat exchanger of barren liquor heat exchange, system acid tail gas export, the system acid tail gas export,The stripping waste gas outlet is respectively communicated with the air inlet arranged on the electric demister. The system of the utility model can lead the SO of almost 100 percent2The gas is recycled to prepare sulfuric acid, the yield of analytically pure sulfuric acid reaches 100%, the finished acid completely reaches the standard of analytically pure sulfuric acid, and the method is suitable for various flue gas conditions.
Description
Technical Field
The utility model relates to a preparation technique of analytically pure sulfuric acid, in particular to a system for preparing analytically pure sulfuric acid by smelting flue gas.
Background
Analytically pure sulfuric acid is widely applied to industries such as industrial analysis, chemical experiments, medicines, storage batteries, electronics and the like. The traditional rectification process adopts a method of firstly oxidizing industrial sulfuric acid, then carrying out reduced pressure rectification and finally carrying out microfiltration on the distillate to prepare analytically pure sulfuric acid. The process has high requirements on equipment, high energy consumption and high cost, is only suitable for small-scale production, cannot meet the requirements of large-scale use, energy conservation and consumption reduction of the current analytically pure sulfuric acid, and is imperative in development of a new analytically pure sulfuric acid preparation process.
In the prior art, some technologies firstly adopt converted flue gas to prepare nicotinic acid and then utilize heat sources such as steam and the like to partially dissociate SO of fuming sulfuric acid3Evaporated and absorbed by ultrapure water to prepare analytically pure sulfuric acid. The technology can only distill part of SO in the nicotinic acid3Therefore, the yield of the analytically pure sulfuric acid is low, and meanwhile, an acid evaporator has the defect of small single processing capacity, a plurality of acid evaporators need to be arranged to run simultaneously during mass production, so that the investment cost, the operation difficulty and the occupied area are increased, in addition, impurities in the nicotinic acid can be separated out in the acid evaporation process, equipment and pipelines are scaled, the regular cleaning is needed, otherwise, the acid evaporation efficiency is influenced, and the energy consumption of the acid evaporation is increased. There are also some technologies to clean the flue gas by washing, filtering and other means, and then to remove SO from the flue gas2Conversion to SO3Then directly absorbing SO by adopting ultrapure water3Analytically pure sulfuric acid was prepared. There are several drawbacks to this type of technique: (1) the nitrogen oxides in the smelting flue gas can not be removed by the cleaning means such as washing, filtering and the like, and the content of nitrate radical impurities in the prepared sulfuric acid directly absorbed after the flue gas is cleaned and converted can not reach the analytic purity of the sulfuric acidIndexes; (2) before the flue gas is converted, concentrated sulfuric acid is used for drying to remove water, but impurities in the flue gas cannot be completely removed by flue gas washing, filtering and other purification, the impurities are introduced in the concentrated sulfuric acid drying, and the dried acid can only be used for preparing industrial sulfuric acid and cannot produce analytically pure sulfuric acid meeting the standard; (3) SO in flue gas2Catalytic conversion to SO3Requires SO2The concentration is kept in a certain range and is continuously stable, SO2The smelting flue gas with too low concentration, too high concentration or large fluctuation can not be used by the method.
In the preparation method and the system of the analytically pure sulfuric acid, both indirect method and direct method have a common problem that the analytically pure sulfuric acid can not be prepared 100 percent, and the by-product industrial sulfuric acid is accompanied, so that the economic benefit of sulfur resource recovery can not be maximized.
SUMMERY OF THE UTILITY MODEL
The to-be-solved technical problem of the utility model is to overcome the not enough of prior art, provide one kind be applicable to various flue gas conditions, can be to the maximize, make SO of sulfur-containing flue gas utilization of resources2The gas recovery utilization rate almost reaches 100%, and the finished acid completely reaches the standard of analytically pure sulfuric acid.
In order to solve the technical problem, the utility model adopts the following technical scheme.
The utility model provides a system for smelt flue gas preparation assay pure sulphuric acid, including the washing cooling tower, electric demister, sulfur dioxide absorption tower, sulfur dioxide desorber, the gas preparation jar, drying tower, conversion system, system acid absorption tower and the degasser that communicate in proper order, be equipped with between sulfur dioxide absorption tower and the sulfur dioxide desorber and be used for sending the absorption liquid pregnant solution that the sulfur dioxide absorption tower produced to the sulfur dioxide desorber, send the absorption liquid barren solution that the sulfur dioxide desorber produced to the sulfur dioxide absorption tower and carry out the barren solution heat exchanger of barren solution heat exchange, system acid absorption tower is equipped with system acid tail gas export, the degasser is equipped with and blows off the exhaust gas export, system acid tail gas export blow off the exhaust gas export respectively with the air inlet intercommunication that electric demister was equipped with.
In the above system for preparing analytically pure sulfuric acid from smelting flue gas, preferably, the drying tower is provided with a dry acid outlet, a dry acid inlet and an absorption acid reflux port, the acid making absorption tower is provided with an absorption acid outlet, an absorption acid inlet and a dry acid reflux port, the degassing tower is provided with a degassing tower inlet, the dry acid outlet is communicated with a third pipeline, the third pipeline is provided with a dry acid cooler, the third pipeline is provided with a first branch and a second branch, the first branch is communicated with the dry acid inlet, the second branch is communicated with the dry acid reflux port, the absorption acid outlet is communicated with a fourth pipeline, the fourth pipeline is provided with an acid making cooler, the fourth pipeline is provided with a third branch, a fourth branch and a fifth branch, the third branch is communicated with the absorption acid inlet, and the fourth branch is communicated with the degassing tower inlet, the fifth branch is communicated with the absorption acid return opening.
Preferably, the washing cooling tower is provided with a liquid outlet and a liquid inlet, the liquid outlet and the liquid inlet of the washing cooling tower are communicated through a first pipeline, and the first pipeline is provided with a washing acid cooler.
Preferably, the sulfur dioxide desorption tower is provided with a rich liquid heat exchange outlet and a rich liquid heat exchange inlet, the rich liquid heat exchange outlet is communicated with the rich liquid heat exchange inlet through a second pipeline, and the second pipeline is provided with a reboiler.
In the system for preparing analytically pure sulfuric acid from smelting flue gas, preferably, the gas distribution tank is provided with a gas distribution inlet, and the gas distribution inlet is communicated with a gas distribution filter.
In the system for preparing analytically pure sulfuric acid from smelting flue gas, preferably, the degassing tower is provided with an air inlet, and the air inlet is communicated with an air filter.
Preferably, the system for preparing analytically pure sulfuric acid from smelting flue gas further comprises a dynamic wave scrubber, and the dynamic wave scrubber is communicated with an air inlet formed in the scrubbing cooling tower.
Preferably, the system for preparing analytically pure sulfuric acid from smelting flue gas further comprises SO3A precision filter, wherein SO is passed between the conversion system and the acid making absorption tower3The precision filter is communicated.
Preferably, the conversion system comprises a converter and a heat exchange assembly which are communicated with each other, and the converter is a three-stage converter.
Compared with the prior art, the utility model has the advantages of:
1. the system of the utility model can be used for flue gas SO2Preparation of ultrapure SO by absorption and desorption2Gas, then to ultra pure SO2Gas distribution, drying, conversion, filtration, absorption, and finally blowing off, oxidizing and removing impurities to obtain SO2Conversion of the gas to analytically pure sulfuric acid, and SO2The utilization of (c) is almost 100%.
The utility model discloses a system mainly involves two aspects to the maximize of sulfur-containing flue gas resource utilization: (1) by blowing off SO in acid making tail gas and stripping waste gas2The sulfur resource in the flue gas is almost 100 percent prepared into sulfuric acid by secondary absorption, and the defects that the sulfur resource in the acid making tail gas cannot be recovered by other technologies and a tail gas treatment device needs to be additionally arranged do not exist; (2) the utility model discloses a system is 100% to the yield of analytically pure sulphuric acid, and other technical yields are only about 50% lower even, and analytically pure sulphuric acid unit price is far above the industrial sulphuric acid, and equal quality's sulphur resource adopts the utility model discloses a device can produce higher economic value.
The utility model is suitable for various flue gas conditions, including SO2Too low, too high or unstable concentration. Adjustment of SO by design2The scale of the absorption-desorption system can realize the preparation of the ultrapure SO from the flue gas under various conditions2The gas can always meet the acid preparation condition of a contact method after being distributed, so that various sulfur-containing flue gases which cannot prepare acid originally can also prepare refined acid, the operation cost is reduced, and benefits are created for enterprises.
The utility model discloses a systemThe finished product acid chromaticity, ignition residues, chlorides, nitrates, amine salts, metal ions, reducing substances and other impurity contents of the analytically pure sulfuric acid prepared by the system completely reach GB/T625-2007 analytically pure sulfuric acid indexes. Preparation of ultrapure SO by absorption-desorption2Preparation of ultrapure SO by gas, gas distribution and conversion3And blowing off and oxidizing after absorption to ensure that the product completely reaches the standard of analytically pure sulfuric acid.
The utility model discloses a drying tower, acid production absorption tower produce acid impurity content and all reach the analytical purification rank, all can adjust acid concentration and realize preparing the analytical purification sulphuric acid, do not need output industrial sulphuric acid.
2. The utility model discloses a system can prepare ultrapure sulfur trioxide (convert gas promptly) is one of the key that gas absorption method acid production can reach the analytically pure sulphuric acid, in addition, links up each other between each part, synergy:
when the washing cooling tower is used for removing impurities and cooling the flue gas, the temperature of the flue gas is reduced to be below 40 ℃ SO as to meet the requirement of SO2Absorbing the required substances while removing SO2Impurities such as external smoke dust (including metal ions), fluorine, chlorine and the like are removed to reach the emission standard;
when the sulfur dioxide absorption tower and the sulfur dioxide desorption tower carry out adsorption-desorption, the organic amine liquid absorbs SO2After that, SO in the tail gas2The concentration of (A) is up to 50mg/m3Hereinafter, SO2The absorption-desorption system can be adjusted by design to realize the preparation of the ultrapure SO from the flue gas under various conditions2A gas;
in the gas distribution tank, ultrapure SO2Mixing with air to distribute gas, and can treat SO in acid-making gas2The concentration is effectively controlled and kept stable, and the preparation of analytically pure sulfuric acid from various kinds of low-sulfur, high-sulfur and unsteady-state flue gases is realized; the obtained acid making gas does not contain nitrogen oxide, and the mass content of nitrate in the prepared analytically pure sulfuric acid is less than 0.00005%; SO in the acid making gas can be obtained by adjusting the gas distribution ratio2The mass content is stably controlled to be 4-6 percent, and the SO can be absorbed by one rotation2The conversion and absorption can be achieved, the conversion rate can reach more than 95 percent through one-time conversion, and the absorption can be completed by adopting one acid making absorption tower, compared with the method used in the prior artThe two-rotation suction and the two-rotation suction can greatly save the cost;
drying acid-making gas in a drying tower by adopting 93-95% analytically pure sulfuric acid to ensure that the water content is less than or equal to 0.1mg/m3Protecting the conversion system equipment and the catalyst, and simultaneously generating dry acid which can adjust the concentration of the absorbed acid and generate analytically pure sulfuric acid through stripping;
the SO in the converted gas is absorbed by 95-98% of analytically pure sulfuric acid in the acid-making absorption tower3Adding a medicament for oxidizing and blowing off to remove SO after supplementing dry acid and ultrapure water to adjust the concentration of the acid produced2Reducing impurities are waited, and the product quality completely reaches the index of GB/T625-2007 analytically pure sulfuric acid;
the acid making tail gas outlet of the acid making absorption tower and the stripping waste gas outlet of the degassing tower are communicated with the electric demister, and the acid making tail gas and the stripping waste gas return to the acid mist and SO2Absorption-desorption system for recovering unreacted SO2And no additional desulfurizing device is needed.
Drawings
FIG. 1 is a schematic structural diagram of a system for preparing analytically pure sulfuric acid from smelting flue gas according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a conversion system according to an embodiment of the present invention.
FIG. 3 is a process flow chart of the method for preparing analytically pure sulfuric acid from smelting flue gas in the embodiment of the present invention.
Illustration of the drawings:
1. a dynamic wave scrubber; 2. washing the cooling tower; 3. a washing acid cooler; 4. an electric demister; 5. a sulfur dioxide absorption tower; 6. a lean-rich liquid heat exchanger; 7. a sulfur dioxide desorber; 8. a reboiler; 9. a gas distribution tank; 10. a gas distribution filter; 11. a drying tower; 12. a dry acid cooler; 13. a conversion system; 14. SO (SO)3A precision filter; 15. an acid making absorption tower; 16. a acid making cooler; 17. a degassing tower; 18. an air filter; 19. a third heat exchanger; 20. a second heat exchanger; 21. a first heat exchanger; 22. heating an electric furnace; 23. a converter; 24. SO (SO)3A cooler; 25. a first conduit; 26. a second conduit; 27. a gas distribution inlet; 28. a third pipeline; 29. system for makingAn acid tail gas outlet; 30. a stripping waste gas outlet; 31. a dry acid outlet; 32. a dry acid inlet; 33. an absorption acid reflux port; 34. an absorption acid outlet; 35. an absorption acid inlet; 36. a dry acid reflux port; 37. a liquid inlet of the degassing tower; 38. an air inlet; 39. a first branch; 40. a second branch circuit; 41. a fourth conduit; 42. a third branch; 43. a fourth branch; 44. a fifth branch; 45. a rich liquid heat exchange outlet; 46. a rich liquid heat exchange inlet; 47. a rich liquid outlet; 48. a rich liquid inlet; 49. a barren liquor outlet; 50. and a barren solution inlet.
Detailed Description
The invention will be further described with reference to the drawings and specific preferred embodiments without limiting the scope of the invention.
The materials and components used in the following examples are all commercially available.
Example 1:
the utility model relates to a system for preparing analytically pure sulfuric acid by smelting flue gas, which comprises a washing cooling tower 2, an electric demister 4, a sulfur dioxide absorption tower 5, a sulfur dioxide desorption tower 7 and a gas distribution tank 9 which are communicated in sequence as shown in figure 1, the device comprises a drying tower 11, a conversion system 13, an acid making absorption tower 15 and a degassing tower 17, wherein a lean-rich liquid heat exchanger 6 which is used for sending absorption liquid rich liquid generated by the sulfur dioxide absorption tower 5 to the sulfur dioxide desorption tower 7, sending absorption liquid lean liquid generated by the sulfur dioxide desorption tower 7 to the sulfur dioxide absorption tower 5 and carrying out lean-rich liquid heat exchange is arranged between the sulfur dioxide absorption tower 5 and the sulfur dioxide desorption tower 7, the acid making absorption tower 15 is provided with an acid making tail gas outlet 29, the degassing tower 17 is provided with a stripping waste gas outlet 30, and the acid making tail gas outlet 29 and the stripping waste gas outlet 30 are respectively communicated with a gas inlet arranged on the electric demister 4.
In this embodiment, the drying tower 11 is provided with a drying acid outlet 31, a drying acid inlet 32 and an absorption acid reflux port 33, the acid making absorption tower 15 is provided with an absorption acid outlet 34, the absorption acid inlet 35 and the dry acid reflux port 36 are arranged on the degassing tower 17, the degassing tower liquid inlet 37 is arranged on the degassing tower 17, the dry acid outlet 31 is communicated with the third pipeline 28, the dry acid cooler 12 is arranged on the third pipeline 28, the third pipeline 28 is respectively provided with a first branch 39 and a second branch 40, the first branch 39 is communicated with the dry acid inlet 32, the second branch 40 is communicated with the dry acid reflux port 36, the absorption acid outlet 34 is communicated with the fourth pipeline 41, the acid making cooler 16 is arranged on the fourth pipeline 41, the fourth pipeline 41 is respectively provided with a third branch 42, a fourth branch 43 and a fifth branch 44, the third branch 42 is communicated with the absorption acid inlet 35, the fourth branch 43 is communicated with the degassing tower liquid inlet 37, and the fifth branch 44 is communicated with the absorption acid reflux port 33.
In this embodiment, the washing cooling tower 2 is provided with a liquid outlet and a liquid inlet, the liquid outlet and the liquid inlet of the washing cooling tower 2 are communicated through a first pipeline 25, and the first pipeline 25 is provided with the washing acid cooler 3.
In this embodiment, sulfur dioxide desorber 7 is equipped with rich liquid heat transfer export 45 and rich liquid heat transfer import 46, and rich liquid heat transfer export 45 communicates through second pipeline 26 with rich liquid heat transfer import 46, is equipped with reboiler 8 on the second pipeline 26.
In this embodiment, the air distribution tank 9 is provided with an air distribution inlet 27, and the air distribution inlet 27 is communicated with an air distribution filter 10.
In this embodiment, the degasser 17 is provided with an air inlet 38, the air inlet 38 being in communication with an air filter 18.
In this embodiment, the system for preparing analytically pure sulfuric acid from smelting flue gas further comprises a dynamic wave scrubber 1, and the dynamic wave scrubber 1 is communicated with an air inlet arranged on the scrubbing cooling tower 2.
In this embodiment, the system for preparing analytically pure sulfuric acid from smelting flue gas further comprises SO3SO passes through the precision filter 14, the conversion system 13 and the acid making absorption tower 153The precision filter 14 is in communication.
In this embodiment, the conversion system 13 includes a converter 23 and a heat exchange assembly which are communicated with each other, and the converter 23 is a three-stage converter. The internal structure design mode of the conversion system 13 is conventional knowledge, and as shown in fig. 2, a third heat exchanger 19, a second heat exchanger 20, a first heat exchanger 21, a temperature-raising electric furnace 22 and a first-layer (top-layer) inlet of a converter 23 are communicated in sequence and used for conveying the dried acid-making gas from the drying tower 11 to the converter 23; outlet of the first layer of the converter 23, the first heat exchanger 21, the second layer of the converter 23, the second heat exchanger 20, the converter23 third layer (bottom layer), third heat exchanger 19, SO3The coolers 24 are in turn in communication for catalytically converting the dry acid making gas to converted gas and transporting it out of the conversion system 13 to the acid making absorption tower 15.
The specific working flow of the system for preparing analytically pure sulfuric acid from smelting flue gas of the embodiment is as follows:
will contain SO2The smelting flue gas enters a dynamic wave scrubber 1 (mainly a reverse spray pipe foam area, the structure is the prior art) for pretreatment, SO that the smelting flue gas contains smoke dust (containing metal ions) and fluorine, chlorine and SO3And (trace) and other impurities are captured and removed, and simultaneously, the temperature is initially reduced to 60-70 ℃, and then the obtained product enters a washing and cooling tower 2. In the washing and cooling tower 2, the flue gas reversely contacts with the washing acid on the surface of the filler in the tower to carry out direct heat exchange and cooling, the flue gas heat absorbed by the washing acid is indirectly exchanged with the circulating cooling water of the washing acid cooler 3 to move out of the system, and the washing acid is circularly sprayed. In the utility model, the washing acid means that the flue gas is washed and the SO is absorbed at the same time3The dilute sulfuric acid produced. The dynamic wave scrubber 1 can be selectively configured according to the smelting flue gas condition, and for the condition that the flue gas temperature is higher than 120 ℃ or the smoke content in the flue gas is higher, the dynamic wave scrubber 1 needs to be configured, and for other conditions, only the washing cooling tower 2 needs to be configured.
The flue gas (also used as cooling impurity-removing gas) discharged from the washing and cooling tower 2 enters the electric demister 4, so that the acid mist in the flue gas is deflected and captured and removed when passing through an electric field generated by the honeycomb tubes of the electric demister 4, and the obtained acid mist-reducing gas enters the sulfur dioxide absorption tower 5.
The organic amine liquid in the sulfur dioxide absorption tower 5 has the function of controlling SO2The specific selectivity of the acid mist reducing agent, the SO in the acid mist gas2Absorbed and stored in the rich liquid, and the smoke, fluorine, chlorine, metal ions and SO in the acid mist reducing gas3、SO2And the pollutants are removed, and the tail gas directly reaches the standard and is discharged outside. The rich solution generated by the sulfur dioxide absorption tower 5 enters a sulfur dioxide desorption tower 7 after being preheated by a lean rich solution heat exchanger 6, the absorption liquid rich solution and the low-pressure steam of a matched reboiler 8 are subjected to indirect heat exchange and temperature rise to realize desorption, and the impurity-free ultra-pure sulfur dioxide gas is generated and absorbedAnd (5) collecting the barren solution. Ultra pure SO2Gas means SO under dry basis conditions2The purity can reach 99.99% (wt) of the gas. The absorption liquid barren solution generated in the sulfur dioxide desorption tower 7 is sent into the sulfur dioxide absorption tower 5 to continuously absorb SO after being cooled by the barren and rich solution heat exchanger 62And the process is circulated.
Mixing and distributing the ultra-pure sulfur dioxide gas and the clean air treated by the distribution filter 10 in the distribution tank 9 to form acid making gas, and adjusting the mixture ratio to ensure that the acid making gas meets the SO requirement of conversion2The concentration is kept stable, and SO in the acid making gas is prepared2SO that the mass fraction of (A) is maintained at 4 to 6% due to SO2The sulfur-containing flue gas with too low or too high concentration or unstable state can realize the acid preparation by the contact method. The gas distribution filter 10 is a precision filter and is commercially available.
The acid making gas enters a drying tower 11 for drying and water absorption, and the drying tower 11 adopts analytically pure sulfuric acid with the mass fraction of 93-95% to spray and absorb moisture in the acid making gas to obtain dry acid making gas and dry acid (concentrated sulfuric acid for drying). The heat absorbed during the drying of the acid making gas is removed out of the system through the indirect heat exchange between the drying acid cooler 12 and the circulating water, 95% -98% of the absorption acid generated by the acid making absorption tower 15 is supplemented to the drying acid with reduced concentration, part of the added drying acid is recycled for drying and water absorption, the other part of the added drying acid is sent to the acid making absorption tower 15 to be used together with the supplementing water for adjusting the concentration of the absorption acid, and the split ratio is determined according to the actual situation and is not limited. The drying tower 11 can be made of steel lined PTFE material, the packing in the drying tower 11 is made of quartz glass packing, and the drying acid cooler 12 is made of Hastelloy alloy, so that secondary pollution is avoided, but the material is not limited to the material.
The dry acid making gas enters the conversion system 13, is heated by a heat exchange assembly matched with the conversion system 13 and then enters the converter 23, and SO is reacted by a catalyst in the converter 232Conversion to SO3The conversion rate can reach more than 95 percent to obtain converted gas, and the converted gas passes through SO3The fine filter 14 performs filtration processing to remove impurities in the gas, and the gas enters the acid making absorption tower 15.
The mass fraction adopted in the acid making absorption tower 15 is 95% ~ EAbsorbing SO in converted gas by spraying 98% of analytically pure sulfuric acid3The heat absorbed by the absorption acid is indirectly transferred and removed out of the system through the circulating cooling water of the acid making cooler 16, and the temperature of the absorption acid is reduced to 60-80 ℃. Adjusting the concentration of the absorbed acid to 95-98% by using the dry acid refluxed from the drying tower 11 and the supplemented ultrapure water, and recycling the increased absorbed acid part for SO3The partial acid is sent to the drying tower 11 to adjust the concentration of the drying acid, and the rest is degassed, wherein the split ratio is determined according to the actual situation and is not limited. The acid making absorption tower 15 can be made of steel lined PTFE material, the packing of the acid making absorption tower 15 is made of quartz glass packing, and the acid making cooler 16 (which can also be a refined acid cooler) is made of Hastelloy, but the invention is not limited thereto. Both the dry acid and the absorbed acid are of analytical grade, and the acid concentration can be adjusted by mutual interaction.
Part of absorption acid generated by the acid making absorption tower 15 is sprayed into the degassing tower 17 from the upper part, clean air filtered by an air filter 18 (which can adopt an air precision filter) is introduced into the tower bottom, and the clean air and the absorption acid are in reverse contact to react on SO2Blowing off the gas, and adding an oxidizing agent to remove SO2After deep removal, the acid chroma of the finished product, the ignition residues, the contents of impurities such as fluorine, chlorine, nitrate, amine salt, metal ions, reducing substances and the like all reach the index of the analytically pure sulfuric acid, and finally, the analytically pure sulfuric acid is conveyed to an analytically pure sulfuric acid storage tank.
The tail gas of the acid making discharged from the acid making absorption tower 15 and the blow-off waste gas generated by the blow-off of the degassing tower 17 enter the electric demister 4 to ensure that the residual SO in the tail gas and the waste gas2The absorption and reuse treatment is carried out, and the discharge reaches the standard.
So far, the sulfur-containing smelting flue gas enters the system from the dynamic wave scrubber 1, and the process is completed after the whole closed cycle of purification, gas distribution, drying, conversion and absorption is completed.
An example of application of the system for preparing analytically pure sulfuric acid from smelting flue gas according to this embodiment is to prepare analytically pure sulfuric acid by using the system, where conditions of the smelting flue gas are shown in table 1, and a process flow is shown in fig. 3, and includes the following steps:
TABLE 1 astable SO2Concentration case cigaretteGas condition table
S1: pretreatment (impurity removal and temperature reduction): the sulfur-containing smelting flue gas with the temperature of 300 ℃ passes through a dynamic wave scrubber 1 and a washing cooling tower 2 in sequence, SO that the smoke dust, fluorine ions, chlorine ions and SO in the flue gas are efficiently removed3And the temperature of the flue gas is reduced to 60-70 ℃ in the dynamic wave washer 1, and is reduced to below 40 ℃, preferably 30-40 ℃ in the washing cooling tower 2.
S2: acid mist reduction: the acid mist in the flue gas discharged from the washing cooling tower 2 is reduced to 5mg/m by an electric demister 43The following.
S3: ultra pure SO2Preparation of gas: the flue gas with acid mist reduced is sent to a sulfur dioxide absorption tower 5, organic amine liquid is used as absorption liquid, and SO in the absorption liquid is absorbed by absorption liquid barren solution2To make SO2The concentration is reduced to 50mg/m3Hereinafter, the rich absorption liquid and the tail gas are obtained. Smoke and SO in tail gas2、SO3Heavy metal ions, fluorine, chlorine and the like reach the emission standard, and tail gas can be directly discharged. The absorption liquid rich solution generated by absorption enters a sulfur dioxide desorption tower 6 for desorption, and the rich solution can be heated up to realize desorption through low-pressure steam heat exchange of a reboiler 7 to obtain the ultrapure SO2Gas and absorption liquid barren solution, the absorption liquid barren solution is returned to the sulfur dioxide absorption tower 5 to continuously absorb SO2And the process is circulated.
For flue gas SO2The spraying amount of absorption liquid barren liquor in the sulfur dioxide absorption tower 5 in the high sulfur period is 70m under the condition of unstable concentration3H, the spraying amount of the absorption liquid rich solution in the sulfur dioxide desorption tower 6 is 60m3The spraying amount of absorption liquid barren liquor in the low sulfur stage sulfur dioxide absorption tower 5 is 20m3H, the spraying amount of the absorption liquid rich solution in the sulfur dioxide desorption tower 6 is 60m3H, leading SO in tail gas discharged by the sulfur dioxide absorption tower 52The concentration is always 50mg/m3The sulfur dioxide desorber 6 is then steadily desorbed to produce 2136kg/h of ultrapure SO2A gas.
S4: preparing acid-making gas: the ultra-pure SO generated by the sulfur dioxide desorption tower 62Gas and 12000m3The clean air treated by the gas distribution precision filter 9 is sent to the gas distribution tank 9 to be mixed, SO that the SO in the mixed gas2The mass fraction of (A) is stably kept at 6% as an acid-making gas.
S5: and (3) drying: sending the acid making gas into a drying tower 11, spraying and drying the acid making gas by using analytically pure sulfuric acid with the mass fraction of 95 percent to absorb water, and reducing the water content of the acid making gas to 0.1mg/m3The dry acid-producing gas and the dry acid are obtained as follows. The dried acid is recycled by heat exchange with circulating cooling water of the dried acid cooler 12 to reduce the temperature to 40 ℃, and analytically pure sulfuric acid (absorption acid) with the mass fraction of 98% generated by the acid making absorption tower 15 is supplemented to the dried acid with the reduced concentration.
S6: and (3) transformation: the dried acid making gas is heated to 420 ℃ through the hot side of a heat exchange assembly matched with the conversion system 13, then enters a converter 23 (a third-stage converter), is subjected to third-stage conversion in the converter 23 under the action of a catalyst, and is subjected to 95% SO2Conversion to SO3Obtaining reformed gas, then reducing the temperature of the reformed gas to 160 ℃ through cold air heat exchange of the heat exchange assembly, and sending the reformed gas to SO3The ultrafilter 14 is subjected to filtration treatment to remove impurities such as catalyst powder, and the filtered converted gas is sent to the acid production absorption tower 15.
Specifically, the three-stage conversion process can be implemented by using the conversion system 13 shown in fig. 2, the conversion system 13 is mainly composed of a converter 22 and a matched heat exchange assembly, the internal structure arrangement of the conversion system 13 is conventional, and the work flow is as follows: the temperature of the dried acid-making gas is sequentially increased from 65 ℃ to 275 ℃ through the 19 tube pass of the third heat exchanger, the temperature of the 20 tube pass of the second heat exchanger is increased from 275 ℃ to 315 ℃, the temperature of the 21 tube pass of the first heat exchanger is increased from 315 ℃ to 420 ℃, the dried acid-making gas enters the converter 23 for the first layer of first conversion, the temperature of the 21 shell pass of the first heat exchanger is decreased from 554 ℃ to 450 ℃, the dried acid-making gas enters the converter 23 for the second layer of second conversion, the temperature of the 20 shell pass of the second heat exchanger is decreased from 480 ℃ to 440 ℃, and the dried acid-making gas enters the converter 23 for the third layer of third conversionThen enters a third heat exchanger 19, the shell pass temperature is reduced from 446 ℃ to 245 ℃, and then enters SO3The shell side temperature of the cooler 24 is reduced from 245 ℃ to 160 ℃. The electric heating furnace 22 is used for heating the gas by electric heating when the temperature of the gas entering the converter is insufficient.
S7: preparation of absorption acid: the acid making absorption tower 15 adopts 98 percent of analytically pure sulfuric acid spray to absorb SO in the converted gas3And obtaining absorption acid and acid making tail gas. The temperature of the absorption acid is reduced to 70 ℃ for recycling through the heat exchange of circulating cooling water of the acid making cooler 16, the concentration increased by the absorption acid is regulated back through the drying acid with the mass fraction of 95% returned by the drying tower 11 and the supplemented ultrapure water, one part of the absorption acid goes to the drying tower 11 to regulate the concentration of the drying acid, and the other part of the absorption acid circularly sprays SO of the absorption conversion gas3And the rest goes to a degassing tower 17 for oxidation stripping.
S8: adding oxidant (hydrogen peroxide) into the degassing tower 17 to absorb SO in the acid2By oxidation to SO3Dissolved in the absorption acid and simultaneously blown with clean air treated by the air filter 18 to blow off the unoxidized SO2And obtaining finished acid and blow-off waste gas, wherein the finished acid is analytically pure sulfuric acid and is conveyed into an analytically pure sulfuric acid storage tank. The acid making tail gas after absorption of the acid making and the blow-off waste gas generated by the blow-off of the degassing tower 17 are returned to the electric demister 4 in the step S2, mixed with the cooling impurity-removing gas for acid mist reduction, and then the unconverted SO in the acid making tail gas is absorbed by the sulfur dioxide absorption tower 52And stripping SO in the exhaust gas2。
In this embodiment, the acid production system produces 3 tons of analytically pure sulfuric acid per hour, the annual production of the analytically pure sulfuric acid reaches 24000 tons, the quality of the finished product acid completely reaches the indexes of the analytically pure sulfuric acid, and the detection parameters are as shown in the following table 2:
TABLE 2 comparison table of acid detection parameters of finished products produced by system and indexes of GB/T625-2007 analytically pure sulfuric acid
| Name (R) | GB/T625-2007 analytically pure sulfuric acid | Systematic production of finished acid |
| Content (H)2SO4).ω/％ | 95.0-98.0 | 96.5 |
| Chroma. Hazen unit | ≤10 | 2 |
| Ignition residue (in sulfate salt). omega/% ] | ≤0.001 | 0.0007 |
| Chloride (Cl). omega/%) | ≤0.00003 | 0.00002 |
| Nitrate (NO)3).ω/％ | ≤0.00005 | 0.00003 |
| Amine liquid (NH)4).ω/％ | ≤0.0002 | 0.0001 |
| Iron (Fe). omega/% ] | ≤0.00005 | 0.00002 |
| Copper (Cu). omega/%) | ≤0.00001 | —— |
| Arsenic (As), omega/%) | ≤0.000003 | —— |
| Lead (Pb). omega/% ] | ≤0.00001 | 0.000001 |
| Reduction of potassium permanganate species (with SO)2Meter), ω/%) | ≤0.0005 | 0.0003 |
For other SO2Under the condition of flue gas with too low and too high concentration, the scales of the sulfur dioxide absorption tower 5 and the sulfur dioxide desorption tower 7 and the spraying amount thereof are designed and adjusted, so that the acid making gas can always meet the acid making condition of a contact method, and tail gas directly reaches the standard and is discharged when various kinds of flue gas are used for preparing and analyzing pure sulfuric acid.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Although the present invention has been described with reference to the preferred embodiments, it is not intended to limit the present invention. Those skilled in the art can make numerous changes and modifications to the disclosed embodiments, or modify equivalent embodiments, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments by the technical entity of the present invention all still belong to the protection scope of the technical solution of the present invention.
Claims (9)
1. A system for preparing analytically pure sulfuric acid from smelting flue gas is characterized by comprising a washing cooling tower (2), an electric demister (4), a sulfur dioxide absorption tower (5), a sulfur dioxide desorption tower (7), a gas distribution tank (9), a drying tower (11), a conversion system (13), an acid production absorption tower (15) and a degassing tower (17) which are sequentially communicated, wherein a lean-rich solution heat exchanger (6) for conveying absorption liquid rich solution generated by the sulfur dioxide absorption tower (5) to the sulfur dioxide desorption tower (7), conveying absorption liquid lean solution generated by the sulfur dioxide desorption tower (7) to the sulfur dioxide absorption tower (5) and carrying out lean solution heat exchange is arranged between the sulfur dioxide absorption tower (5) and the sulfur dioxide desorption tower (7), the acid production absorption tower (15) is provided with an acid production tail gas outlet (29), the degassing tower (17) is provided with a stripping waste gas outlet (30), the acid making tail gas outlet (29) and the stripping waste gas outlet (30) are respectively communicated with a gas inlet arranged on the electric demister (4).
2. The system for preparing analytically pure sulfuric acid from smelting flue gas according to claim 1, wherein the drying tower (11) is provided with a drying acid outlet (31), a drying acid inlet (32) and an absorption acid return port (33), the acid production absorption tower (15) is provided with an absorption acid outlet (34), an absorption acid inlet (35) and a drying acid return port (36), the degassing tower (17) is provided with a degassing tower liquid inlet (37), the drying acid outlet (31) is communicated with a third pipeline (28), the third pipeline (28) is provided with a drying acid cooler (12), the third pipeline (28) is respectively provided with a first branch (39) and a second branch (40), the first branch (39) is communicated with the drying acid inlet (32), the second branch (40) is communicated with the drying acid return port (36), and the absorption acid outlet (34) is communicated with a fourth pipeline (41), be equipped with system acid cooler (16) on fourth pipeline (41), fourth pipeline (41) branch is equipped with third branch road (42), fourth branch road (43) and fifth branch road (44), third branch road (42) with absorption acid import (35) intercommunication, fourth branch road (43) with degasser inlet (37) intercommunication, fifth branch road (44) with absorption acid backward flow mouth (33) intercommunication.
3. The system for preparing and analyzing pure sulfuric acid from smelting flue gas according to claim 1 or 2, wherein the washing and cooling tower (2) is provided with a liquid outlet and a liquid inlet, the liquid outlet and the liquid inlet of the washing and cooling tower (2) are communicated through a first pipeline (25), and the first pipeline (25) is provided with a washing acid cooler (3).
4. The system for preparing analytically pure sulfuric acid from smelting flue gas according to claim 1 or 2, wherein the sulfur dioxide desorption tower (7) is provided with a rich liquid heat exchange outlet (45) and a rich liquid heat exchange inlet (46), the rich liquid heat exchange outlet (45) is communicated with the rich liquid heat exchange inlet (46) through a second pipeline (26), and the second pipeline (26) is provided with a reboiler (8).
5. The system for preparing analytically pure sulfuric acid from metallurgical off-gas according to claim 1 or 2, wherein the gas distribution tank (9) is provided with a gas distribution inlet (27), and the gas distribution inlet (27) is communicated with a gas distribution filter (10).
6. A system for the preparation of analytically pure sulfuric acid from metallurgical off-gas according to claim 1 or 2, characterized in that the degassing tower (17) is provided with an air inlet (38), which air inlet (38) is in communication with an air filter (18).
7. The system for preparing analytically pure sulfuric acid from smelting flue gas according to claim 1 or 2, further comprising a dynamic wave scrubber (1), wherein the dynamic wave scrubber (1) is communicated with an air inlet arranged on the scrubbing cooling tower (2).
8. The system for preparing analytically pure sulfuric acid from smelting flue gas of claim 1 or 2 further comprising SO3A precision filter (14), wherein SO passes between the conversion system (13) and the acid making absorption tower (15)3The precision filter (14) is communicated.
9. A system for producing analytically pure sulfuric acid from metallurgical off-gas according to claim 1 or 2, characterized in that the conversion system (13) comprises a converter (23) and a heat exchange assembly in communication with each other, the converter (23) being a three-stage converter.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111115587A (en) * | 2020-01-19 | 2020-05-08 | 长沙华时捷环保科技发展股份有限公司 | Method and system for preparing analytically pure sulfuric acid from smelting flue gas |
| CN113148962A (en) * | 2021-01-19 | 2021-07-23 | 昆明理工大学 | Device and method for preparing acid from smelting flue gas by using hydrogen peroxide and activated carbon |
| CN113213434A (en) * | 2021-04-27 | 2021-08-06 | 太和县大华能源科技有限公司 | Dry absorption conversion system for refined sulfuric acid |
| CN113233434A (en) * | 2021-07-13 | 2021-08-10 | 联仕(昆山)化学材料有限公司 | Production process and production device of electronic-grade nitric acid |
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2020
- 2020-01-19 CN CN202020124151.9U patent/CN211521596U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111115587A (en) * | 2020-01-19 | 2020-05-08 | 长沙华时捷环保科技发展股份有限公司 | Method and system for preparing analytically pure sulfuric acid from smelting flue gas |
| CN113148962A (en) * | 2021-01-19 | 2021-07-23 | 昆明理工大学 | Device and method for preparing acid from smelting flue gas by using hydrogen peroxide and activated carbon |
| CN113213434A (en) * | 2021-04-27 | 2021-08-06 | 太和县大华能源科技有限公司 | Dry absorption conversion system for refined sulfuric acid |
| CN113233434A (en) * | 2021-07-13 | 2021-08-10 | 联仕(昆山)化学材料有限公司 | Production process and production device of electronic-grade nitric acid |
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