CN110054164A - A kind of dilute sulfuric acid system for concentrating and recycling - Google Patents
A kind of dilute sulfuric acid system for concentrating and recycling Download PDFInfo
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- CN110054164A CN110054164A CN201910435634.2A CN201910435634A CN110054164A CN 110054164 A CN110054164 A CN 110054164A CN 201910435634 A CN201910435634 A CN 201910435634A CN 110054164 A CN110054164 A CN 110054164A
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- Prior art keywords
- sulfuric acid
- dilute sulfuric
- outlet
- entrance
- concentrating
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 353
- 238000004064 recycling Methods 0.000 title claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims description 53
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 37
- 239000000460 chlorine Substances 0.000 claims description 37
- 229910052801 chlorine Inorganic materials 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 29
- 239000010808 liquid waste Substances 0.000 claims description 17
- 239000002699 waste material Substances 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 5
- 239000005864 Sulphur Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 28
- 238000005265 energy consumption Methods 0.000 abstract description 13
- 238000011084 recovery Methods 0.000 abstract description 8
- 230000003247 decreasing effect Effects 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 27
- 238000001704 evaporation Methods 0.000 description 12
- 230000008901 benefit Effects 0.000 description 11
- 238000006298 dechlorination reaction Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 7
- 238000009835 boiling Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002918 waste heat Substances 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000002309 gasification Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- WBLXMRIMSGHSAC-UHFFFAOYSA-N [Cl].[Cl] Chemical compound [Cl].[Cl] WBLXMRIMSGHSAC-UHFFFAOYSA-N 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007806 chemical reaction intermediate Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- -1 medicine or dyeing Chemical class 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/68—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/88—Concentration of sulfuric acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
- B01D2257/206—Organic halogen compounds
- B01D2257/2064—Chlorine
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Biomedical Technology (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The present invention relates to dilute sulfuric acid concentration technique fields, more particularly to a kind of dilute sulfuric acid system for concentrating and recycling, including dilute sulfuric acid preheating device, vacuum concentrating apparatus and concentrated sulfuric acid recyclable device, dilute sulfuric acid preheating device includes heat exchanger and primary heater, vacuum concentrating apparatus includes concentration kettle, the first entrance of heat exchanger with dilute sulfuric acid source for connecting, the first outlet of heat exchanger is connected to the entrance of primary heater, the outlet of primary heater is connected to the entrance of concentration kettle, the outlet of concentration kettle is connected to the second entrance of heat exchanger, the second outlet of heat exchanger is connected to concentrated sulfuric acid recyclable device.The second level preheating device and vacuum concentrating apparatus that the present invention passes through effectively are concentrated dilute sulfuric acid, process is short, equipment is few, while guaranteeing to reach dilute sulfuric acid concentration and recovery required temperature, ensure that the concentrated sulfuric acid mass fraction formed after being concentrated reaches required technological standards, energy consumption is greatly decreased, highly effective enhances the scope of application and stability of technique.
Description
Technical field
The present invention relates to dilute sulfuric acid concentration technique field more particularly to a kind of dilute sulfuric acid system for concentrating and recycling.
Background technique
Sulfuric acid is important basic chemical raw materials at present, extensive in industrial applications such as chemical industry, steels, is industrially usually used in doing
Dehydrating agent, reaction intermediate, cleaning agent, catalyst etc..It is reduced by the usual concentration of the sulfuric acid used or as impure dilute
Sulfuric acid cannot be further continued for for producing, so the sulfuric acid that many industrial process use finally is disposed or passed through simply in a manner of spent acid
It is discharged after processing, causes the serious wasting of resources and problem of environmental pollution.
With the development of the chemical industry and the demand to environmental protection, generally dilute sulfuric acid is carried out in present chemical industry dense
It retracts and receives, recycles.The technique for also having sulfuric acid concentrate in the past, such as cooking-pot type concentration, burning concentration, high temperature concentration method and low temperature
Concentration method etc., but due to the strong corrosive of sulfuric acid often prevents high temperature concentration technology from practical, then due to sulfuric acid concentrate
Energy source consumption is high, so that recovery value is not high, causes most of user would rather be as offal treatment, some enterprises are even
Unprocessed direct emission, seriously pollutes environment.Low temperature concentration method is only applicable to sulfuric acid mass fraction concentration less than 60%
Dilute sulfuric acid is concentrated, and the sulfuric acid mass fraction concentration after concentration is also not more than 60%, requires not to be able to satisfy to many techniques.
Current chlor-alkali enterprises are mainly sold to the dry Waste Sulfuric Acid of chlorine and PVC enterprise to the dry Waste Sulfuric Acid of hydrogen chloride
The enterprise for producing chemical fertilizer neutralizes for the production of chemical fertilizer or for carbide slurry, is converted into outside gypsum and sells.Due in the dry spent acid of chlorine
Dissolved with 0.2% or so chlorine, hydrogen chloride dries the hydrogen chloride gas in Waste Sulfuric Acid containing 0.13% or so, and what is made is dilute
The utilization of sulfuric acid is restricted, so there is stronger corrosivity than finished product sulfuric acid, the chlorine to volatilize in transport, use process
Environment is seriously polluted with hydrogen chloride.
Summary of the invention
(1) technical problems to be solved
Dense sulphur the technical problem to be solved by the present invention is to the energy consumption of existing dilute sulfuric acid system for concentrating and recycling is high, and after being concentrated
Acid mass fraction is not up to standard, is unable to satisfy the problem of technique requires.
(2) technical solution
In order to solve the above-mentioned technical problems, the present invention provides a kind of dilute sulfuric acid system for concentrating and recycling, including dilute sulfuric acid are pre-
Thermal, vacuum concentrating apparatus and concentrated sulfuric acid recyclable device, the dilute sulfuric acid preheating device include heat exchanger and primary heater,
The vacuum concentrating apparatus includes concentration kettle, and the first entrance of the heat exchanger with dilute sulfuric acid source for connecting, the heat exchanger
First outlet be connected to the entrance of the primary heater, outlet and the entrance of the concentration kettle of the primary heater connect
Logical, the outlet of the concentration kettle is connected to the second entrance of the heat exchanger, the second outlet of the heat exchanger and the dense sulphur
Acid-restoring plant connection.
Wherein, the concentration kettle includes the rectifying enriching section set gradually along the flow direction of the dilute sulfuric acid inside it and adds
Thermal concentration section, the entrance of the rectifying enriching section and the outlet of the primary heater, the liquid of the rectifying enriching section
It exports and is connected to the entrance of the heating enriching section, the outlet of the heating enriching section and the second entrance of the heat exchanger connect
It is logical.
Wherein, the bottom of the heating enriching section is equipped with heating component.
Wherein, the vacuum concentrating apparatus further includes condenser and drainer, the entrance of the condenser and the rectifying
The gas vent of enriching section is connected to, and the outlet of the condenser is connected to the entrance of the drainer.
It wherein, further include liquid waste treating apparatus, the outlet of the drainer is connected to the liquid waste treating apparatus, described useless
Liquid processing device is equipped with detector and alkali injection tube road, and the detector is used to detect the acid of waste liquid in the liquid waste treating apparatus
Basicity, the alkali injection tube road is for infusing alkaline agent into the liquid waste treating apparatus.
Wherein, the drainer is equipped with liquid-ring vacuum pump, forms negative pressure state in the vacuum concentrating apparatus for making,
The inlet of the liquid-ring vacuum pump is connect with the outlet of the drainer, the liquid outlet of the liquid-ring vacuum pump and the waste liquid
Processing unit connection.
Wherein, the concentrated sulfuric acid recyclable device includes the first cooler, the second outlet of the heat exchanger and described first
Cooler connection.
It wherein, further include dilute sulfuric acid pretreatment unit, the dilute sulfuric acid pretreatment unit includes dechlorinator, the dechlorinator
Top be equipped with gas outlet for being passed through the inlet of the dilute sulfuric acid containing chlorine and for chlorine to be discharged, bottom is equipped with for being passed through pressure
The air inlet of contracting gas and the liquid outlet of discharge dilute sulfuric acid, the liquid outlet are connected to the first entrance of the heat exchanger.
Wherein, the dilute sulfuric acid pretreatment unit further includes circulating pump and secondary heater, and the circulating pump takes off with described
The liquid outlet of chlorine tower connects, for heating the dechlorinator as described in the dilute sulfuric acid blowback flowed out in the dechlorinator, described second
Device is set on the pipeline that the circulating pump is connected to the inlet of the dechlorinator.
Wherein, the dilute sulfuric acid pretreatment unit further includes emission-control equipment, and the emission-control equipment includes second
The entrance of cooler and chlorine tourie, second cooler is connected to the gas outlet of the dechlorinator, second cooler
Outlet connect with the chlorine tourie, sig water is contained in the chlorine tourie.
(3) beneficial effect
Above-mentioned technical proposal of the invention has the advantages that dilute sulfuric acid system for concentrating and recycling of the invention, dilute sulfuric acid into
Enter dilute sulfuric acid preheating device preheating, first pass through heat exchanger carry out level-one heating, then by primary heater progress second level heating, two
The preheating device of grade heating can sufficiently improve the temperature of moisture in dilute sulfuric acid, reduce subsequent concentration heating energy consumption, be preheating to certain
The dilute sulfuric acid of temperature enters in the concentration kettle of vacuum concentrating apparatus, and concentration kettle keeps negative-pressure operation, because of concentration in vacuo
Dilute sulfuric acid can effectively reduce temperature required for evaporation, so further reduced concentration kettle heating energy consumption, dilute sulfuric acid is being concentrated
It is constantly heated up during flowing in kettle, the moisture in dilute sulfuric acid constantly gasifies discharge, and then concentration forms the concentrated sulfuric acid
It is discharged into heat exchanger again by the outlet of concentration kettle, exchanges heat with the dilute sulfuric acid entered in heat exchanger, provided as dilute sulfuric acid
Level-one heating, makes full use of waste heat, and energy saving finally flows into the concentration and recovery that concentrated sulfuric acid recyclable device completes dilute sulfuric acid.This
It invents the second level preheating device passed through and vacuum concentrating apparatus is effectively concentrated dilute sulfuric acid, process is short, and equipment is few, is protecting
While card reaches dilute sulfuric acid concentration and recovery required temperature, it is ensured that required for the concentrated sulfuric acid mass fraction formed after concentration reaches
Technological standards, are greatly decreased energy consumption, and highly effective enhances the scope of application and stability of technique, reduces dilute sulfuric acid and be concentrated back
The construction cost and operating cost of receipts system improve the economic benefit and social benefit of dilute sulfuric acid recycling, have extensive suitable
Ying Xing.
In addition to it is described above present invention solves the technical problem that, constitute technical solution technical characteristic and have this
Except advantage brought by the technical characteristic of a little technical solutions, other technical characteristics of the invention and these technical characteristic brings
Advantage will be further illustrated in conjunction with attached drawing.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of dilute sulfuric acid system for concentrating and recycling of the embodiment of the present invention；
Fig. 2 is the dilute sulfuric acid pretreatment unit structural schematic diagram of dilute sulfuric acid system for concentrating and recycling of the embodiment of the present invention.
In figure: 1: dilute sulfuric acid preheating device；2: vacuum concentrating apparatus；3: concentrated sulfuric acid recyclable device；4: liquid waste treating apparatus；
5: dilute sulfuric acid pretreatment unit；6: dilute sulfuric acid containing chlorine；7: compressed gas；11: heat exchanger；12: primary heater；21: concentration kettle；
22: condenser；23: drainer；24: liquid-ring vacuum pump；31: the first coolers；41: detector；42: alkali injection tube road；51: dechlorination
Tower；52: circulating pump；53: secondary heater；54: emission-control equipment；211: rectifying enriching section；212: heating enriching section；213:
Heating component；541: the second coolers；542: chlorine tourie.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
Member's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that unless otherwise clearly defined and limited, term " installation ", " phase
Even ", " connection " shall be understood in a broad sense, for example, it may be being fixedly connected, may be a detachable connection, or be integrally connected；It can
To be mechanical connection, it is also possible to be electrically connected；It can be directly connected, can also can be indirectly connected through an intermediary
Connection inside two elements.For the ordinary skill in the art, above-mentioned term can be understood at this with concrete condition
Concrete meaning in invention.
In addition, in the description of the present invention, unless otherwise indicated, " multiple ", " more ", " multiple groups " be meant that two or
Two or more, " several ", " several ", " several groups " are meant that one or more.
As shown in Figure 1, dilute sulfuric acid system for concentrating and recycling provided in an embodiment of the present invention, including it is dilute sulfuric acid preheating device 1, true
Empty enrichment facility 2 and concentrated sulfuric acid recyclable device 3, dilute sulfuric acid preheating device 1 include heat exchanger 11 and primary heater 12, and vacuum is dense
Compression apparatus 2 includes concentration kettle 21, the first entrance of heat exchanger 11 for connect with dilute sulfuric acid source, the first outlet of heat exchanger 11 and
The entrance of primary heater 12 is connected to, and the outlet of primary heater 12 is connected to the entrance of concentration kettle 21, the outlet of concentration kettle 21
It is connected to the second entrance of heat exchanger 11, the second outlet of heat exchanger 11 is connected to concentrated sulfuric acid recyclable device 3.
Dilute sulfuric acid system for concentrating and recycling of the invention, dilute sulfuric acid enter the preheating of dilute sulfuric acid preheating device, first pass through heat exchanger
Level-one heating is carried out, then second level heating is carried out by primary heater, the preheating device of two-step heating can sufficiently improve dilute sulfuric acid
The temperature of middle moisture, reduces subsequent concentration heating energy consumption, and the dilute sulfuric acid for being preheating to certain temperature enters the dense of vacuum concentrating apparatus
In contracting kettle, concentration kettle keeps negative-pressure operation, because concentration in vacuo dilute sulfuric acid can effectively reduce temperature required for evaporation,
So further reduced concentration kettle heating energy consumption, dilute sulfuric acid is constantly heated up during flowing in concentration kettle, dilute
Moisture in sulfuric acid constantly gasifies discharge, and then is concentrated and forms the concentrated sulfuric acid and be discharged into heat exchanger again by the outlet of concentration kettle,
It exchanges heat with the dilute sulfuric acid entered in heat exchanger, provides level-one heating as dilute sulfuric acid, make full use of waste heat, energy saving, most
The concentration and recovery that concentrated sulfuric acid recyclable device completes dilute sulfuric acid is flowed into afterwards.The second level preheating device and vacuum concentration dress that the present invention passes through
Dilute sulfuric acid is concentrated with being set effective, process is short, and equipment is few, is guaranteeing to reach the same of dilute sulfuric acid concentration and recovery required temperature
When, it is ensured that the concentrated sulfuric acid mass fraction formed after concentration reaches required technological standards, is greatly decreased energy consumption, highly effective,
The scope of application and stability for enhancing technique, reduce the construction cost and operating cost of dilute sulfuric acid system for concentrating and recycling, improve
The economic benefit and social benefit of dilute sulfuric acid recycling, have extensive adaptability.
In the present embodiment, heat exchanger can be used input and output material heat exchanger, primary heater can be used hot water, low-pressure steam or in
The heating methods such as steam are pressed, if place device there are other available waste heats that can pay the utmost attention to utilize.
In one embodiment, concentration kettle 21 includes the rectifying enriching section set gradually along the flow direction of dilute sulfuric acid inside it
211 and heating enriching section 212, the outlet of the entrance of rectifying enriching section 211 and primary heater 12, rectifying enriching section 211
Liquid outlet with heating enriching section 212 entrance be connected to, heat enriching section 212 outlet and heat exchanger 11 second entrance company
It is logical.Dilute sulfuric acid enters in concentration kettle after pre-heating temperature elevation in dilute sulfuric acid preheating device, and concentration kettle can further heat up dilute sulfuric acid
Heating carries out the abjection of moisture and the removing of impurity, and dilute sulfuric acid flows to heating enriching section by rectifying enriching section, under condition of negative pressure,
Partial moisture in dilute sulfuric acid, which gasifies, to be discharged, and the dilute sulfuric acid that initial concentration is obtained in rectifying enriching section enters back into heating concentration
Duan Jixu heating concentration, can reduce the load of concentration kettle in this way, can also make full use of waste heat energy saving.In the present embodiment
Rectifying enriching section is located at heating enriching section top, and rectifying enriching section can be rectifying column, and heating enriching section can be evaporating kettle, dilute sulfuric acid
Enter rectifying column after pre-heating temperature elevation, the discharge of part moisture vaporization, remaining liquid phase material flow downward along rectifying column in dilute sulfuric acid
Into evaporating kettle, by continuous heat temperature raising in moving process, moisture constantly gasifies liquid phase material, gaseous phase materials along rectifying column to
Upper operation contacts with the dilute sulfuric acid run down and carries out caloic exchange, by the sulfuric acid of gasification and the SO decomposited3Steaming is taken back in absorption
Kettle is sent out, the concentration in moving process of the sulfuric acid in evaporating kettle constantly increases, and is finally reached and requires the concentrated sulfuric acid of concentration from evaporating kettle
The outlet of bottom flows out and enters heat exchanger by the second entrance of heat exchanger, by heat exchanger after exchanging heat with the dilute sulfuric acid of charging
Second outlet is expelled to concentrated sulfuric acid recyclable device.
In the present embodiment, plate column or packed tower, preferably ceramic packed tower is can be used in rectifying column, and plate column uses valve tower
Disk, sieve pore tower tray, bubble cap tray, 3~8 pieces of number of trays, preferably 4~6 pieces.Filler in packed column 500~2000mm of height, preferably
800~1200mm.Evaporating kettle is horizontal vessel, and inside setting heating tube, heating efficiency is gradually reinforced along liquid flow direction.
In one embodiment, the bottom for heating enriching section 212 is equipped with heating component 213.In the bottom of heating enriching section
Heating component is set, can make to form certain gliding temperature gradient by bottom to the top of rectifying enriching section of heating enriching section,
Moisture in cooperation rectifying enriching section after gasification is the temperature that rectifying enriching section provides, and makes to reach equalized temperature in concentration kettle.This
Heating tube can be selected in heating component in embodiment, using high temperature heat conductive oil or electrically heated heat form, if place device
There are other available waste heats that can pay the utmost attention to utilize.
In one embodiment, vacuum concentrating apparatus 2 further includes condenser 22 and drainer 23, the entrance of condenser 22 with
The gas vent of rectifying enriching section 211 is connected to, and the outlet of condenser 22 is connected to the entrance of drainer 23.Dilute sulfuric acid is in concentration kettle
Rectifying enriching section in after heat temperature raising, part moisture vaporization is expelled to by the gas vent at the top of rectifying enriching section in dilute sulfuric acid
In condenser, condenser forms liquid after carrying out heat exchange to gas, and liquid is flowed into drainer by condensator outlet into one
Walk exothermic condensation.In the present embodiment, condenser is gas phase condenser, and recirculated water or chilled water can be used in condenser and drainer
Equal coolant medias.
In one embodiment, dilute sulfuric acid system for concentrating and recycling further includes liquid waste treating apparatus 4, the outlet of drainer 23 with
Liquid waste treating apparatus 4 is connected to, and liquid waste treating apparatus 4 is equipped with detector 41 and alkali injection tube road 42, and detector 41 is useless for detecting
The pH value of waste liquid in liquid processing device 4, alkali injection tube road 42 is for infusing alkaline agent into liquid waste treating apparatus 4.Have in drainer and arranges
Liquid out enters liquid waste treating apparatus, and the waste water that dilute sulfuric acid concentration process is discharged in liquid waste treating apparatus is recycled,
By the way that detector is arranged in non-also processing unit, the pH value of the waste water of entrance is detected, alkali injection tube road direction liquid waste processing is passed through
Injection ammonium hydroxide or lye carry out acid-base neutralization in device, and waste water is neutralized to after neutrality and is in an organized way discharged into sewage disposal system
Carry out processing up to standard.In the present embodiment, PH on-line monitoring system, real-time control alkaline agent injection rate is can be used in detector, it is ensured that outer
Draining is neutral, does not influence sewage disposal system.
In one embodiment, drainer 23 is equipped with liquid-ring vacuum pump 24, negative for making to be formed in vacuum concentrating apparatus 2
The inlet of pressure condition, liquid-ring vacuum pump 24 is connect with the outlet of drainer 23, at the liquid outlet and waste liquid of liquid-ring vacuum pump 24
Device 4 is managed to connect.The temperature that concentrated sulfuric acid evaporation needs under normal pressure is more than 300 DEG C or more, concentrated sulfuric acid evaporating temperature under vacuum state
About 60~80 DEG C can be reduced, not only improves equipment selection and service life in this way, operation energy consumption can also be reduced, improves economic effect
Benefit.Such as 85% concentrated sulfuric acid atmospheric boiling point be 227 DEG C, and boiling point is about 160 DEG C under absolute pressure 10kPa pressure；90% concentrated sulfuric acid
Atmospheric boiling point is 259 DEG C, and boiling point is about 190 DEG C under absolute pressure 10kPa pressure, and 95% concentrated sulfuric acid atmospheric boiling point is 301 DEG C, and
Boiling point is about 230 DEG C under absolute pressure 10kPa pressure.Therefore liquid-ring vacuum pump is connect with drainer, to keep concentration kettle, gas phase cold
Air-flow in condenser, drainer and liquid-ring vacuum pump forms access, needed for thus liquid-ring vacuum pump provides for vacuum concentrating apparatus
The vacuum condition wanted guarantees that concentration kettle keeps negative-pressure operation, effectively reduces operation temperature and selection difficulty.Liquid-ring vacuum pump
Pendular ring medium preferentially selects the evaporation condensed water isolated from drainer, on the one hand can guarantee vacuum degree, on the other hand may be used
With a small amount of processing medium for utilizing and recycling the moisture evaporated in concentration process and take out of, outer pollution discharging environment is avoided.
In one embodiment, concentrated sulfuric acid recyclable device 3 includes the first cooler 31, the second outlet of heat exchanger 11 and the
The connection of one cooler 31.The concentrated sulfuric acid by being discharged in heating enriching section is flowed into after heat exchanger and charging dilute sulfuric acid heat exchange
First cooler of concentrated sulfuric acid recyclable device enters concentrated sulfuric acid storage tank after the further circulating water of the first cooler,
It is used as process system feedstock circulation.
In one embodiment, dilute as shown in Fig. 2, dilute sulfuric acid system for concentrating and recycling further includes dilute sulfuric acid pretreatment unit 5
Sulfur acid pretreatment device 5 includes dechlorinator 51, and the top of dechlorinator 51 is equipped with inlet and use for being passed through dilute sulfuric acid containing chlorine 6
In the gas outlet of discharge chlorine, bottom is equipped with the liquid outlet of air inlet and discharge dilute sulfuric acid for being passed through compressed gas 7, out liquid
Mouth is connected to the first entrance of heat exchanger 11.Different pretreatments technique can be selected according to dilute sulfuric acid source difference, mainly remove
Impurity in dilute sulfuric acid, it is ensured that the stable operation of follow-up system, dilute sulfuric acid is before entering dilute sulfuric acid preheating device in the present embodiment
Dilute sulfuric acid pretreatment unit is first passed through, dechlorination processing first is carried out to dilute sulfuric acid, subsequently into evaporation and concentrating system.Dilute sulfuric acid containing chlorine
Enter dechlorinator from the inlet of dechlorinator's upper side, compressed gas enters dechlorination from the air inlet of dechlorinator middle and lower part side
Tower, dilute sulfuric acid containing chlorine flow downward, and compressed gas flows up, and the two inversely contacts, and compressed gas will be in dilute sulfuric acid containing chlorine
Chlorine is taken away, and is discharged from the gas outlet at the top of dechlorinator, and the dilute sulfuric acid of dechlorination qualification is discharged from the liquid outlet of dechlorination tower bottom, with this
The dechlorination to dilute sulfuric acid is completed to handle.
In the present embodiment, compressed gas can with filler or column plate can be set in nitrogen perhaps air dechlorinator,
Preferential Ceramics class or resinae random packing.The position of inlet and air inlet is respectively provided with distributor in dechlorinator, so as to
Dilute sulfuric acid containing chlorine and compressed air into after tower can more uniform distribution dispersing contact, improve dechlorination effect.
In one embodiment, dilute sulfuric acid pretreatment unit 5 further includes circulating pump 52 and secondary heater 53, circulating pump 52
It is connect with the liquid outlet of dechlorinator 51, for dechlorinator 51, secondary heater will to be returned by the dilute sulfuric acid pump flowed out in dechlorinator 51
53 are set on the pipeline that circulating pump 52 is connected to the inlet of dechlorinator 51.For the dechlorination effect for ensuring the dilute sulfuric acid containing chlorine, increase
If external circulating pump, the inlet of the dilute sulfuric acid pump that the liquid outlet of dechlorination tower bottom is flowed out chlorine top of tower back off, and pass through
Secondary heater heats the dilute sulfuric acid pumped out by circulating pump before entering dechlorinator, enters dechlorinator's process repeatedly with this
With inversely contacting repeatedly for compressed gas, keep dilute sulfuric acid dechlorination more thorough.In the present embodiment, the heat medium of secondary heater
Hot water can be selected or exchanged heat with other waste heats, 50~100 DEG C, preferably 60~80 DEG C are heated to.
In one embodiment, dilute sulfuric acid pretreatment unit 5 further includes emission-control equipment 54, and emission-control equipment 54 wraps
The second cooler 541 and chlorine tourie 542 are included, the entrance of the second cooler 541 is connected to the gas outlet of dechlorinator 51, and second is cold
But the outlet of device 541 is connect with chlorine tourie 542, and sig water is contained in chlorine tourie 542.Dilute sulfuric acid containing chlorine and compressed air pair
After punching contact, chlorine-containing gas is discharged into the second cooler by the gas outlet of dechlorinator, and the second cooler carries out chlorine-containing gas
After heat exchange cooling down, chlorine-containing gas enters chlorine tourie, the chlorine absorbing material such as sig water is held in rate tourie, by chlorine
The dechlorination of tourie acts on, and chlorine-containing gas purification becomes purified gas, completes exhaust-gas treatment by being discharged in chlorine tourie, it is ensured that de-
The not outer pollution discharging environment of chlorine out guarantees the environmental protection of dilute sulfuric acid pretreatment work.
Different pretreating process can be taken for different useless dilute sulfuric acids, such as medicine or dyeing, it is organic
Reacting the useless dilute sulfuric acid generated first can carry out oxidation processes to dilute sulfuric acid；The useless dilute sulfuric acid of steel industry will be first filtered
Removal of impurities processing etc..
In conclusion dilute sulfuric acid system for concentrating and recycling of the invention, dilute sulfuric acid enters the preheating of dilute sulfuric acid preheating device, first leads to
It crosses heat exchanger and carries out level-one heating, then second level heating is carried out by primary heater, the preheating device of two-step heating can be mentioned sufficiently
The temperature of moisture in high dilute sulfuric acid, reduces subsequent concentration heating energy consumption, and the dilute sulfuric acid for being preheating to certain temperature enters vacuum concentration
In the concentration kettle of device, concentration kettle keeps negative-pressure operation, because concentration in vacuo dilute sulfuric acid can effectively reduce needed for evaporation
The temperature wanted constantly is added during dilute sulfuric acid flows in concentration kettle so further reduced concentration kettle heating energy consumption
Heat heating, the moisture in dilute sulfuric acid constantly gasify discharge, and then are concentrated to form the concentrated sulfuric acid and pass through the outlet of concentration kettle and be discharged into again
It in heat exchanger, exchanges heat with the dilute sulfuric acid entered in heat exchanger, provides level-one heating as dilute sulfuric acid, make full use of waste heat, save
About energy consumption finally flows into the concentration and recovery that concentrated sulfuric acid recyclable device completes dilute sulfuric acid.Second level preheating device that the present invention passes through and
Vacuum concentrating apparatus is effectively concentrated dilute sulfuric acid, and process is short, and equipment is few, is guaranteeing to reach needed for dilute sulfuric acid concentration and recovery
While temperature, it is ensured that the concentrated sulfuric acid mass fraction formed after concentration reaches required technological standards, and energy consumption is greatly decreased, high
It imitates practical, enhances the scope of application and stability of technique, reduce the construction cost and running cost of dilute sulfuric acid system for concentrating and recycling
With, improve dilute sulfuric acid recycling economic benefit and social benefit, have extensive adaptability.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of dilute sulfuric acid system for concentrating and recycling, it is characterised in that: including dilute sulfuric acid preheating device, vacuum concentrating apparatus and dense sulphur
Acid-restoring plant, the dilute sulfuric acid preheating device include heat exchanger and primary heater, and the vacuum concentrating apparatus includes concentration
Kettle, the first entrance of the heat exchanger with dilute sulfuric acid source for connecting, the first outlet of the heat exchanger and first heating
The entrance of device is connected to, and the outlet of the primary heater is connected to the entrance of the concentration kettle, the outlet of the concentration kettle and institute
The second entrance connection of heat exchanger is stated, the second outlet of the heat exchanger is connected to the concentrated sulfuric acid recyclable device.
2. dilute sulfuric acid system for concentrating and recycling according to claim 1, it is characterised in that: the concentration kettle includes along described dilute
Rectifying enriching section that the flow direction of sulfuric acid inside it is set gradually and heating enriching section, the entrance of the rectifying enriching section with it is described
The outlet of primary heater, the liquid outlet of the rectifying enriching section is connected to the entrance of the heating enriching section, described
The outlet of heating enriching section is connected to the second entrance of the heat exchanger.
3. dilute sulfuric acid system for concentrating and recycling according to claim 2, it is characterised in that: the bottom of the heating enriching section is set
There is heating component.
4. dilute sulfuric acid system for concentrating and recycling according to claim 2, it is characterised in that: the vacuum concentrating apparatus further includes
Condenser and drainer, the entrance of the condenser are connected to the gas vent of the rectifying enriching section, and the condenser goes out
Mouth is connected to the entrance of the drainer.
5. dilute sulfuric acid system for concentrating and recycling according to claim 4, it is characterised in that: it further include liquid waste treating apparatus, institute
The outlet for stating drainer is connected to the liquid waste treating apparatus, and the liquid waste treating apparatus is equipped with detector and alkali injection tube road,
The detector is used to detect the pH value of waste liquid in the liquid waste treating apparatus, and the alkali injection tube road is used for at the waste liquid
It manages and infuses alkaline agent in device.
6. dilute sulfuric acid system for concentrating and recycling according to claim 5, it is characterised in that: it is true that the drainer is equipped with pendular ring
Sky pump, forms negative pressure state for making in the vacuum concentrating apparatus, the inlet of the liquid-ring vacuum pump and the drainer
Outlet connection, the liquid outlet of the liquid-ring vacuum pump connect with the liquid waste treating apparatus.
7. dilute sulfuric acid system for concentrating and recycling according to claim 1, it is characterised in that: the concentrated sulfuric acid recyclable device includes
First cooler, the second outlet of the heat exchanger are connected to first cooler.
8. dilute sulfuric acid system for concentrating and recycling described in -7 any one according to claim 1, it is characterised in that: further include dilute sulfuric acid
Pretreatment unit, the dilute sulfuric acid pretreatment unit includes dechlorinator, and the top of the dechlorinator is equipped with dilute containing chlorine for being passed through
The inlet of sulfuric acid and gas outlet for chlorine to be discharged, bottom are equipped with the air inlet for being passed through compressed gas and dilute sulphur are discharged
The liquid outlet of acid, the liquid outlet are connected to the first entrance of the heat exchanger.
9. dilute sulfuric acid system for concentrating and recycling according to claim 8, it is characterised in that: the dilute sulfuric acid pretreatment unit is also
Including circulating pump and secondary heater, the circulating pump is connect with the liquid outlet of the dechlorinator, and being used for will be by the dechlorinator
Dechlorinator described in the dilute sulfuric acid blowback of middle outflow, the secondary heater are set to the feed liquor of the circulating pump Yu the dechlorinator
On the pipeline of mouth connection.
10. dilute sulfuric acid system for concentrating and recycling according to claim 9, it is characterised in that: the dilute sulfuric acid pretreatment unit
It further include emission-control equipment, the emission-control equipment includes the second cooler and chlorine tourie, second cooler
Entrance is connected to the gas outlet of the dechlorinator, and the outlet of second cooler is connect with the chlorine tourie, and the chlorine is inhaled
Sig water is contained in closed cans.
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| CN111068495A (en) * | 2019-12-09 | 2020-04-28 | 中国恩菲工程技术有限公司 | Treatment method of sulfur-containing tail gas |
| CN111359242A (en) * | 2020-04-07 | 2020-07-03 | 苏州汉浩分离技术有限公司 | Falling film evaporator |
| CN111874874A (en) * | 2020-07-28 | 2020-11-03 | 安徽东至广信农化有限公司 | Waste sulfuric acid recovery and concentration process |
| CN112044240A (en) * | 2020-08-27 | 2020-12-08 | 临海市建新化工有限公司 | Methyl bromide purifier |
| CN112494969A (en) * | 2020-11-10 | 2021-03-16 | 衡阳丰联精细化工有限公司 | Dilute sulfuric acid concentration device and system thereof |
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| CN207918433U (en) * | 2018-03-06 | 2018-09-28 | 响水恒利达科技化工有限公司 | A kind of concentration systems of recycling dilute sulfuric acid |
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| CN207918433U (en) * | 2018-03-06 | 2018-09-28 | 响水恒利达科技化工有限公司 | A kind of concentration systems of recycling dilute sulfuric acid |
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| CN111068495A (en) * | 2019-12-09 | 2020-04-28 | 中国恩菲工程技术有限公司 | Treatment method of sulfur-containing tail gas |
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| CN111874874A (en) * | 2020-07-28 | 2020-11-03 | 安徽东至广信农化有限公司 | Waste sulfuric acid recovery and concentration process |
| CN112044240A (en) * | 2020-08-27 | 2020-12-08 | 临海市建新化工有限公司 | Methyl bromide purifier |
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| CN112494969A (en) * | 2020-11-10 | 2021-03-16 | 衡阳丰联精细化工有限公司 | Dilute sulfuric acid concentration device and system thereof |
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| CN110054164B (en) | 2024-06-21 |
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