CN104085861B - A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater and corresponding technique thereof - Google Patents
A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater and corresponding technique thereof Download PDFInfo
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000002253 acid Substances 0.000 title claims abstract description 59
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 239000002351 wastewater Substances 0.000 title claims abstract description 29
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- 238000009833 condensation Methods 0.000 claims abstract description 77
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- 239000007788 liquid Substances 0.000 claims abstract description 32
- 239000002699 waste material Substances 0.000 claims abstract description 29
- 238000004821 distillation Methods 0.000 claims abstract description 20
- 230000008676 import Effects 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 238000001816 cooling Methods 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 12
- 239000002893 slag Substances 0.000 claims description 11
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000003860 storage Methods 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 4
- 230000009286 beneficial effect Effects 0.000 claims description 3
- 238000011084 recovery Methods 0.000 abstract description 4
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- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 239000012286 potassium permanganate Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
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- 238000002360 preparation method Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
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- 238000000605 extraction Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
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Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention provides a kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, its sulfuric acid of purifying from Graphene waste water, reach the object of resource circulation utilization, and the acid solution accounting rate of recovery reaches 92% ~ 95%, recyclable most of heat in the operating process of this device simultaneously, saves energy about 30%.It comprises waste liquid holding tank, it is characterized in that: it also comprises condensation portion, distillation fraction, described condensation portion comprises two condensing units, condensation rectification cell, condensation heating unit, two condensing units are respectively the first condensing unit, second condensing unit, described first condensing unit, second condensation unit is all furnished with inner chamber, exocoel, the lower exit port of described condensation rectification cell is communicated with the inner chamber import of described first condensing unit, the chamber exit of described first condensing unit is communicated to sulfuric acid apparatus for placing, the outlet of described condensation heater is furnished with condensation matrass, the outlet of described condensation matrass is connected to the lumen inlet of described second condensing unit.
Description
Technical field
The present invention relates to the technical field of reclaim(ed) sulfuric acid in waste water, be specially a kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, present invention also offers a kind of technique of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separated from graphite material, be the two-dirnentional structure of carbon, be a kind of " super material ", it is of wide application, from electronic product to flak jackets and papermaking, the even following space elevator can take Graphene as raw material.The preparation of Graphene is for main raw material with graphite, the vitriol oil, potassium permanganate, hydrogen peroxide, a large amount of Cleaning Wastewater, filtrate etc. can be produced in preparation process, therefore, great proportion is accounted for containing sulfuric acid content in the compositions, particularly waste water such as sulfuric acid, potassium permanganate, potassium permanganate, hydrogen peroxide in Graphene factory effluent.Such as produce the enterprise of Graphene wastewater flow rate 1000T/D, sulfuric acid content 30%-50% in waste water, just 300T/D can be reached, and the waste water of generation is just simply processed rear discharge by Graphene manufacturing enterprise at present, and, a large amount of alkali can be added in process waste water process, produce a large amount of mud thus and must entrust and put row relax into outward, do not meet resource three cyclical policy, cause the significant wastage of resource, cost.
Sulfuric acid is all widely used in industrial production or in agriculture production, a kind of important industrial raw material particularly in industrial production, it can be used for manufacturing fertilizer, medicine, explosive, pigment, washing composition, store battery etc., also be widely used in the industry such as purification oil, Metal smelting and dyestuff, the a large amount of acid waste liquids produced in Industrial processes, mineral acid containing different concns, if these spent acid solutions directly discharge, not only contaminate environment, and cause the waste of resource, therefore acid waste liquid becomes the significant problem needing solution now badly.
The method of process spent acid solution mainly contains method of enrichment, neutralisation, solvent extration, ion exchange method, membrane separation process etc. both at home and abroad at present, and method of enrichment and neutralisation are the main method of China's conventional process spent acid.But traditional method of enrichment is large to the corrodibility of equipment, and neutralisation can not efficient recovery sulfuric acid wherein.Solvent extration more advanced is at present very high to the requirement of extraction agent, is not suitable in large-scale commercial production; Ion exchange method, by the impact of ion exchange resin, have higher requirements, and its actual conditions is once determine, requires the composition of stoste not change too large to spent acid solution intermediate ion upon adsorption; Membrane separation technique then treatment capacity is little, and cost of investment is high.
Summary of the invention
For the problems referred to above, the invention provides a kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, its sulfuric acid of purifying from Graphene waste water, reach the object of resource circulation utilization, and its accounting rate of recovery can reach 92% ~ 95%, with the recyclable most of heat of timer, saves energy about 30%.
A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, its technical scheme is such: it comprises waste liquid holding tank, it is characterized in that: it also comprises condensation portion, distillation fraction, described condensation portion comprises two condensing units, condensation rectification cell, condensation heating unit, two condensing units are respectively the first condensing unit, second condensing unit, described first condensing unit, second condensation unit is all furnished with inner chamber, exocoel, the lower exit port of described condensation rectification cell is communicated with the inner chamber import of described first condensing unit, the chamber exit of described first condensing unit is communicated to sulfuric acid apparatus for placing, the outlet of described condensation heater is furnished with condensation matrass, the outlet of described condensation matrass is connected to the lumen inlet of described second condensing unit, the chamber exit of described second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell upper outlet is by the heating system of the external outside of transfer of water vapour pipe, described distillation fraction specifically comprises N section distilling period, be respectively the 1st distilling period, 2nd distilling period, N distilling period, wherein N is the natural number of >=1, every section of described distilling period includes heating unit, matrass, rectification cell, the exocoel outlet of the second condensing unit is communicated to the liquid-inlet of the heating unit of the 1st distilling period by thrust-augmenting nozzle, the upper outlet of the heating unit of the 1st distilling period is communicated to the import of the matrass of the 1st distilling period, the outlet of the 1st distilling period matrass is to the entrance of the rectification cell of the 1st distilling period, the lower exit port of the rectification cell of the 1st distilling period is communicated to the liquid-inlet of the heating unit of the 2nd distilling period, the upper outlet of the heating unit of the 2nd distilling period is communicated to the import of the matrass of the 2nd distilling period, the outlet of the 2nd distilling period matrass is to the entrance of the rectification cell of the 2nd distilling period, until the lower exit port of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the upper outlet of each rectification cell in all distilling periods is respectively by the heating system of the external outside of transfer of water vapour pipe.
It is further characterized in that:
The top being arranged as described heating unit of every section of described distilling period is furnished with described matrass, the top of described matrass is furnished with described rectification cell, be provided with oblique baffle plate in the below inner chamber of described rectification cell, described oblique baffle plate is drained to the lower exit port of this rectification cell;
Described first condensing unit, the second condensing unit are specially spiral prolong, the inner chamber of described spiral prolong is the internal cavity of the spiral tube spiralization being placed in tube wall inside, the outer wall that the exocoel of described spiral prolong is spiral tube and the cavity that the inwall of tube wall is formed;
Heating unit in described condensation heating unit, distilling period is specially well heater, is provided with heater strip in the internal cavity of described well heater;
The bottom of described well heater is provided with slag notch, and described slag notch is provided with valve;
Described waste liquid holding tank comprises waste liquid underground storage groove, higher memory groove, compensating groove, described waste liquid underground storage groove is communicated to the upper inlet of described higher memory groove by water pump, corresponding pipeline, the lower part outlet of described higher memory groove is communicated to the import of described compensating groove, and the outlet of described compensating groove is by the exocoel entrance of pipeline connection to the first condensing unit;
Described sulfuric acid apparatus for placing is specially cooling tank structure, and described cooling tank structure is placed in cooling tank, is provided with recirculated water in described cooling tank;
Rectification cell in described condensation rectification cell, distilling period is specially rectifying column, and the top of described rectifying column is provided with valve, and the upper outlet of described rectifying column is vapor outlet port, and the lower part outlet of described rectifying column is liquid exit;
Described distillation fraction only can comprise one section of distilling period, the exocoel outlet of the second condensing unit is communicated to the liquid-inlet of the heating unit of distilling period by thrust-augmenting nozzle, the upper outlet of the heating unit of distilling period is communicated to the import of the matrass of distilling period, the outlet of distilling period matrass is to the entrance of the rectification cell of distilling period, and the lower exit port of the rectification cell of distilling period is communicated to the liquid-inlet of described condensation heating unit.
A kind of technique of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, it is characterized in that: waste liquid adds thermal distillation through at least twice after the heating of two condensing units, make the water in waste liquid be transported to heating system by the form of water vapour, and make the sulfuric acid in waste liquid be recovered simultaneously.
Its concrete technology step is as follows:
After a waste liquid passes into the exocoel entrance of the first condensing unit, after the hydrothermal solution heating of the inner chamber of the first condensing unit, from the exocoel entrance of exocoel outlet inflow second condensing unit of the first condensing unit, after the hydrothermal solution of the inner chamber of the second condensing unit heats again, export from the exocoel of the second condensing unit the entrance being flowed into distillation fraction by thrust-augmenting nozzle;
B by the control of temperature in the heating unit internal cavity of every section of distilling period in distillation fraction first distill out water vapour, after distill out acid solution steam, dregs after heating are discharged from the slag notch of heating unit, the water vapour that density is less is discharged along the upper outlet of the rectification cell of this section of distilling period, the sulfuric acid vapor that density is larger flows into the internal cavity of the heating unit of hypomere distilling period from the lower part outlet of the rectification cell of this section of distilling period with part water, until the lower exit port of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit;
C by the control of temperature in condensation heating unit internal cavity first distill out water vapour, after distill out acid solution steam, if have dregs after heating, discharge from bottom slag notch, the water vapour that density is less is discharged along the upper outlet of condensation rectification cell, and the sulfuric acid that density is larger flows into cooling tank structure from the lower part outlet of condensation rectification cell.
It is further characterised in that:
In b step, first the fluid temperature to 110 DEG C ~ 115 DEG C through heating unit is adjusted in every section of distilling period, ensure that first water vapour distillate, water vapour is delivered to heating system by pipeline and is used, and acid solution continuous heating distillation in heating unit, the acid solution that the condensable predistillation of matrass being positioned at the outlet of heating unit goes out, reach the object reducing acid solution loss, after heating about 20min ~ 40min, heighten fluid temperature to 155 in heating unit DEG C ~ 190 DEG C, be beneficial to acid solution steam to distillate, retort gas is further rectifying in rectification cell, the retort gas that density is less can be overflowed as water vapour through rectification cell upper end, the lower part outlet of acid solution through rectification cell lower end that density is larger flows into the heating unit of next section of distilling period, until the outlet of the rectification cell of N distilling period flows into the liquid-inlet of condensation heating unit,
In step c, adjustment condensation heating unit fluid temperature to 110 DEG C ~ 115 DEG C, so that moisture distillates in first distillate, be positioned at the condensable acid solution distilled out of condensation matrass of the outlet of condensation heating unit, reach the object reducing acid solution loss, after heating 20min ~ 40min, the fluid temperature to 155 of adjustment condensation heating unit DEG C ~ 190 DEG C, first distillate after heating is further rectifying in condensation rectification cell, and secondary distillate carries out collection cooling from the outlet of condensation rectification cell lower end in the first condensing unit inflow cooling tank structure.
After adopting the present invention, acid solution is equipped with two kinds of temperature before and after the heating unit, condensation heating unit of every section of distilling period, distill out water vapour and sulfuric acid vapor respectively, improve the liquid-tight degree of recovered acid, liquid distillates through the upper outlet of heating unit, distillates dregs and discharge through the lower tapping hole of heating unit in waste liquid; Device two sections of condensing units have good condensation, heats, wherein cool distillate temperature, heating process waste liquid temperature, make full use of in system and produce heat, economize on resources; And the matrass above heating unit all has microcondenser effect.The device of this invention allows working temperature 1100 DEG C, chemical stability is excellent, under normal temperature or high temperature, except hydrofluoric acid and phosphoric acid, can resistance to various acid, chloroazotic acid, neutral salt, the erosion of sulphur and carbon, and obtain refining effect by distillation, little to equipment corrosion, divide (N+1) section distilation, accomplish that water vapour and sulfuric acid vapor are collected respectively, distillate sulfuric acid purity high, can directly apply in production, distill out water vapour for heating system, the spent acid accounting rate of recovery reaches 92% ~ 95%, simultaneously can saves energy about 30%, there is energy-efficient effect, can operate continuously, do not affect the normal operation of equipment, environmental protection and energy saving, high-level efficiency, meet cleaner production and circular economy policy.
Accompanying drawing explanation
Fig. 1 is the structural schematic block diagram of device specific embodiment of the present invention;
In Fig. 1, dotted arrow is stream of water vapor to, solid arrow is flow direction, and the arrow below the bottom slag notch of wherein primary heater 11, secondary heater 8 is that dregs get rid of direction.
Embodiment
A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, it comprises waste liquid holding tank, it is characterized in that: it also comprises condensation portion, distillation fraction, described condensation portion comprises two condensing units, condensation rectification cell, condensation heating unit, two condensing units are respectively the first condensing unit, second condensing unit, described first condensing unit, second condensation unit is all furnished with inner chamber, exocoel, the lower exit port of described condensation rectification cell is communicated with the inner chamber import of described first condensing unit, the chamber exit of described first condensing unit is communicated to sulfuric acid apparatus for placing, the outlet of described condensation heater is furnished with condensation matrass, the outlet of described condensation matrass is connected to the lumen inlet of described second condensing unit, the chamber exit of described second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell upper outlet is by the heating system of the external outside of transfer of water vapour pipe, described distillation fraction specifically comprises N section distilling period, be respectively the 1st distilling period, 2nd distilling period, N distilling period, wherein N is the natural number of >=1, every section of described distilling period includes heating unit, matrass, rectification cell, the exocoel outlet of the second condensing unit is communicated to the liquid-inlet of the heating unit of the 1st distilling period by thrust-augmenting nozzle, the upper outlet of the heating unit of the 1st distilling period is communicated to the import of the matrass of the 1st distilling period, the outlet of the 1st distilling period matrass is to the entrance of the rectification cell of the 1st distilling period, the lower exit port of the rectification cell of the 1st distilling period is communicated to the liquid-inlet of the heating unit of the 2nd distilling period, the upper outlet of the heating unit of the 2nd distilling period is communicated to the import of the matrass of the 2nd distilling period, the outlet of the 2nd distilling period matrass is to the entrance of the rectification cell of the 2nd distilling period, until the lower exit port of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the upper outlet of each rectification cell in all distilling periods is respectively by the heating system of the external outside of transfer of water vapour pipe.
Specific embodiment, see Fig. 1: wherein N=1, namely one section of distilling period is only had, it comprises waste liquid underground storage groove 1, higher memory groove 2, compensating groove 3, waste liquid underground storage groove 1 is by water pump 4, corresponding pipeline is communicated to the upper inlet of higher memory groove 2, the lower part outlet of higher memory groove 2 is communicated to the import of compensating groove 3, the outlet of compensating groove 3 is by the exocoel entrance of the spiral prolong 5 of pipeline connection to the first, the exocoel entrance of the spiral prolong 6 of exocoel outlet to the second of the first spiral prolong 5, the exocoel outlet of the second spiral prolong 6 is communicated to the liquid-inlet of secondary heater 8 by thrust-augmenting nozzle 7, the upper outlet of secondary heater 8 is communicated to the import of after-fractionating bottle 9, the entrance of outlet to the second rectifying column 10 of after-fractionating bottle 9, the lower exit port of the second rectifying column 10 is communicated to the liquid-inlet of primary heater 11, the upper outlet of the first heating 11 devices is communicated to the import of the first matrass 12, the outlet of the first matrass 12 is connected to the lumen inlet of the second spiral prolong 6, the chamber exit of the second spiral prolong 6 is communicated to the entrance of the first rectifying column 13, first rectifying column 13, the upper outlet of the second rectifying column 10 is (not shown in FIG. respectively by the heating system of the external outside of transfer of water vapour pipe 14, arrange according to practical situation), the lower part outlet of the first rectifying column 13 is communicated to the inner chamber import of the first spiral prolong 5, the chamber exit of the first spiral prolong 5 is communicated to sulfuric acid apparatus for placing.Sulfuric acid apparatus for placing is specially cooling tank structure 15, and cooling tank structure 15 is placed in cooling tank 16, is provided with recirculated water in cooling tank 16.
The inner chamber of the spiral prolong 6 of the first spiral prolong 5, second is the internal cavity of the spiral tube spiralization being placed in tube wall inside, the outer wall that the exocoel of the spiral prolong 6 of the first spiral prolong 5, second is spiral tube and the cavity that the inwall of tube wall is formed; Heater strip is provided with in the internal cavity of primary heater 11, secondary heater 8; The bottom of primary heater 11, secondary heater 8 is provided with the slag notch 17 of closing in, slag notch 17 is provided with valve 18; The top of the first rectifying column 13, second rectifying column 10 is provided with valve 19, and the upper outlet of the first rectifying column, the second rectifying column is vapor outlet port, and the lower part outlet of the first rectifying column 13, second rectifying column 10 is liquid exit;
Being arranged as in distilling period: the top of secondary heater 8 is furnished with after-fractionating bottle 9, the top of after-fractionating bottle 9 is furnished with the second rectifying column 10, be provided with oblique baffle plate 20 in the below inner chamber of the second rectifying column 10, oblique baffle plate 20 is drained to the lower exit port of the second rectifying column 10.
Secondary heater 8 in dashed rectangle in Fig. 1, after-fractionating bottle 9, second rectifying column 10 is combined to form distilling period, a distilling period can be set in the present invention, also two or more distilling period can be set, well heater is furnished with in every section of distilling period, matrass and rectifying column, when the quantity of distilling period is greater than 1, the quantity of setting distilling period is M, M is the integer of >=2, now by every section of distilling period called after the 1st distilling period, 2nd distilling period, M distilling period, the exocoel outlet of the second spiral prolong 6 is communicated to the liquid-inlet of the well heater of the 1st distilling period by thrust-augmenting nozzle 7, the upper outlet of the well heater of the 1st distilling period is communicated to the import of the matrass of the 1st distilling period, the outlet of the 1st distilling period matrass is to the entrance of the rectifying column of the 1st distilling period, the lower exit port of the 1st distilling period rectifying column is communicated to the liquid-inlet of the well heater of the 2nd distilling period, the upper outlet of the well heater of the 2nd distilling period is communicated to the import of the matrass of the 2nd distilling period, the outlet of the 2nd distilling period matrass is to the entrance of the rectifying column of the 2nd distilling period, until the lower exit port of M distilling period rectifying column is communicated to the liquid-inlet of primary heater 11, owing to including M distilling period, it makes the sulfuric acid that distills out purer.
The technique of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater in specific embodiment, waste liquid adds thermal distillation through twice after the heating of two condensing units, make the water in waste liquid be transported to heating system by the form of water vapour, and make the sulfuric acid in waste liquid be recovered simultaneously.
Its concrete technology step is as follows:
After a waste liquid passes into the exocoel entrance of the first spiral prolong 5, after the hydrothermal solution heating of the inner chamber of the first spiral prolong 5, from the exocoel entrance of the spiral prolong 6 of exocoel outlet inflow second of the first spiral prolong 5, after the hydrothermal solution heating of the inner chamber of the second spiral prolong 6, export from the exocoel of the second spiral prolong 6 internal cavity being flowed into secondary heater 8 by thrust-augmenting nozzle 7;
B by the control of temperature in secondary heater 8 internal cavity first distill out water vapour, after distill out acid solution steam, water vapour, dregs after heating are discharged from bottom slag notch, the water vapour that density is less is discharged along the upper outlet of the second rectifying column 10, and the sulfuric acid vapor that density is larger flows into the internal cavity of primary heater 11 from the lower part outlet of the second rectifying column 10 with part water;
C by the control of temperature in primary heater 11 internal cavity first distill out water vapour, after distill out acid solution steam, water vapour, if have dregs after heating, discharge from bottom slag notch, the water vapour that density is less is discharged along the upper outlet of the first rectifying column 13, and the sulfuric acid that density is larger flows into cooling tank structure 15 from the lower part outlet of the first rectifying column 13.
In b step, first the fluid temperature to 110 DEG C ~ 115 DEG C through secondary heater 8 is adjusted, ensure that first water vapour distillate, water vapour is delivered to heating system by pipeline and is used, and acid solution continuous heating distillation in the heater, the acid solution that the condensable predistillation of after-fractionating bottle 9 being positioned at the outlet of secondary heater 8 goes out, reach the object reducing acid solution loss, after heating about 20min ~ 40min, close the valve 19 on the top of the second rectifying column 10, heighten fluid temperature to 155 in secondary heater 8 DEG C ~ 190 DEG C, be beneficial to acid solution steam to distillate, retort gas is further rectifying in the second rectifying column 10, the retort gas that density is less can be overflowed as water vapour through the second rectifying column 10 upper end, the lower part outlet of acid solution through the second rectifying column 10 lower end that density is larger flows into primary heater 11,
In step c, adjustment primary heater 11 fluid temperature to 110 DEG C ~ 115 DEG C, so that moisture distillates in first distillate, be positioned at the condensable acid solution distilled out of the first matrass 12 of the outlet of primary heater 11, reach the object reducing acid solution loss, after heating 20min ~ 40min, the fluid temperature to 155 DEG C of adjustment primary heater 11 ~ 190 DEG C, first distillate after heating is further rectifying in the first rectifying column 13, secondary distillate from first rectifying column 13 lower end outlet through the first spiral prolong 5 flow in cooling tank structure 15 carry out collections cool.
Claims (9)
1. the device of a reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, it comprises waste liquid holding tank, it is characterized in that: it also comprises condensation portion, distillation fraction, described condensation portion comprises two condensing units, condensation rectification cell, condensation heating unit, two condensing units are respectively the first condensing unit, second condensing unit, described first condensing unit, second condensation unit is all furnished with inner chamber, exocoel, the lower exit port of described condensation rectification cell is communicated with the inner chamber import of described first condensing unit, the chamber exit of described first condensing unit is communicated to sulfuric acid apparatus for placing, the heating unit of described condensation heating unit is specially condensation heater, heater strip is provided with in the internal cavity of described condensation heater, the outlet of described condensation heater is furnished with condensation matrass, the outlet of described condensation matrass is connected to the lumen inlet of described second condensing unit, the chamber exit of described second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell upper outlet is by the heating system of the external outside of transfer of water vapour pipe, described distillation fraction specifically comprises N section distilling period, be respectively the 1st distilling period, 2nd distilling period, N distilling period, wherein N is the natural number of >=1, every section of described distilling period includes heating unit, matrass, rectification cell, the exocoel outlet of the second condensing unit is communicated to the liquid-inlet of the heating unit of the 1st distilling period by thrust-augmenting nozzle, the upper outlet of the heating unit of the 1st distilling period is communicated to the import of the matrass of the 1st distilling period, the outlet of the 1st distilling period matrass is to the entrance of the rectification cell of the 1st distilling period, the lower exit port of the rectification cell of the 1st distilling period is communicated to the liquid-inlet of the heating unit of the 2nd distilling period, the upper outlet of the heating unit of the 2nd distilling period is communicated to the import of the matrass of the 2nd distilling period, the outlet of the 2nd distilling period matrass is to the entrance of the rectification cell of the 2nd distilling period, until the lower exit port of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the upper outlet of each rectification cell in all distilling periods is respectively by the heating system of the external outside of transfer of water vapour pipe.
2. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, it is characterized in that: the top being arranged as described heating unit of every section of described distilling period is furnished with described matrass, the top of described matrass is furnished with described rectification cell, be provided with oblique baffle plate in the below inner chamber of described rectification cell, described oblique baffle plate is drained to the lower exit port of this rectification cell.
3. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, it is characterized in that: described first condensing unit, the second condensing unit are specially spiral prolong, the inner chamber of described spiral prolong is the internal cavity of the spiral tube spiralization being placed in tube wall inside, the outer wall that the exocoel of described spiral prolong is spiral tube and the cavity that the inwall of tube wall is formed.
4. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, is characterized in that: the heating unit in described distilling period is specially well heater, is provided with heater strip in the internal cavity of described well heater.
5. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, it is characterized in that: described waste liquid holding tank comprises waste liquid underground storage groove, higher memory groove, compensating groove, described waste liquid underground storage groove is communicated to the upper inlet of described higher memory groove by water pump, corresponding pipeline, the lower part outlet of described higher memory groove is communicated to the import of described compensating groove, and the outlet of described compensating groove is by the exocoel entrance of pipeline connection to the first condensing unit.
6. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, it is characterized in that: the rectification cell in described condensation rectification cell, distilling period is specially rectifying column, the top of described rectifying column is provided with valve, the upper outlet of described rectifying column is vapor outlet port, and the lower part outlet of described rectifying column is liquid exit.
7. the device of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 1, it is characterized in that: described distillation fraction only can comprise one section of distilling period, the exocoel outlet of the second condensing unit is communicated to the liquid-inlet of the heating unit of distilling period by thrust-augmenting nozzle, the upper outlet of the heating unit of distilling period is communicated to the import of the matrass of distilling period, the outlet of distilling period matrass is to the entrance of the rectification cell of distilling period, and the lower exit port of the rectification cell of distilling period is communicated to the liquid-inlet of described condensation heating unit.
8. the technique by device reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater according to claim 1, it is characterized in that: waste liquid adds thermal distillation through at least twice after the heating of two condensing units, make the water in waste liquid be transported to heating system by the form of water vapour, and make the sulfuric acid in waste liquid be recovered simultaneously; Its concrete technology step is as follows:
After a waste liquid passes into the exocoel entrance of the first condensing unit, after the hydrothermal solution heating of the inner chamber of the first condensing unit, from the exocoel entrance of exocoel outlet inflow second condensing unit of the first condensing unit, after the hydrothermal solution of the inner chamber of the second condensing unit heats again, export from the exocoel of the second condensing unit the entrance being flowed into distillation fraction by thrust-augmenting nozzle;
B by the control of temperature in the heating unit internal cavity of every section of distilling period in distillation fraction first distill out water vapour, after distill out acid solution steam, dregs after heating are discharged from the slag notch of heating unit, the water vapour that density is less is discharged along the upper outlet of the rectification cell of this section of distilling period, the sulfuric acid vapor that density is larger flows into the internal cavity of the heating unit of hypomere distilling period from the lower part outlet of the rectification cell of this section of distilling period with part water, until the lower exit port of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit;
C by the control of temperature in condensation heating unit internal cavity first distill out water vapour, after distill out acid solution steam, if have dregs after heating, discharge from bottom slag notch, the water vapour that density is less is discharged along the upper outlet of condensation rectification cell, and the sulfuric acid that density is larger flows into cooling tank structure from the lower part outlet of condensation rectification cell.
9. the technique of a kind of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater as claimed in claim 8, is characterized in that:
In b step, first the fluid temperature to 110 DEG C ~ 115 DEG C through heating unit is adjusted in every section of distilling period, ensure that first water vapour distillate, water vapour is delivered to heating system by pipeline and is used, and acid solution continuous heating distillation in heating unit, the acid solution that the condensable predistillation of matrass being positioned at the outlet of heating unit goes out, reach the object reducing acid solution loss, after heating 20min ~ 40min, heighten fluid temperature to 155 in heating unit DEG C ~ 190 DEG C, be beneficial to acid solution steam to distillate, retort gas is further rectifying in rectification cell, the retort gas that density is less can be overflowed as water vapour through rectification cell upper end, the lower part outlet of acid solution through rectification cell lower end that density is larger flows into the heating unit of next section of distilling period, until the outlet of the rectification cell of N distilling period flows into the liquid-inlet of condensation heating unit,
In step c, the fluid temperature to 110 of adjustment condensation heating unit DEG C ~ 115 DEG C, so that moisture distillates in first distillate, be positioned at the condensable acid solution distilled out of condensation matrass of the outlet of condensation heating unit, reach the object reducing acid solution loss, after heating 20min ~ 40min, the fluid temperature to 155 of adjustment condensation heating unit DEG C ~ 190 DEG C, first distillate after heating is further rectifying in condensation rectification cell, and secondary distillate carries out collection cooling from the outlet of condensation rectification cell lower end in the first condensing unit inflow cooling tank structure.
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| CN109319999B (en) * | 2018-11-13 | 2021-10-08 | 新疆烯金石墨烯科技有限公司 | Treatment method for resource utilization of waste liquid in graphene oxide production |
| CN110921959A (en) * | 2019-12-18 | 2020-03-27 | 淮阴师范学院 | Graphene preparation residual liquid harmless treatment system |
| CN111672153A (en) * | 2020-07-13 | 2020-09-18 | 黄石加柯环保科技有限公司 | Concentrating kettle and preparation method of sodium sulfite crystal |
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| CN101070143B (en) * | 2007-06-11 | 2010-07-14 | 浙江闰土股份有限公司 | Multi-effect concentration equipment system utilizing low-concentration waste sulfuric acid |
| CN201553609U (en) * | 2009-11-10 | 2010-08-18 | 西陇化工股份有限公司 | Sulfuric acid purifying device |
| CN203938481U (en) * | 2014-07-11 | 2014-11-12 | 昆山明宽环保节能科技有限公司 | A kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid |
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