CN104085861A - Device for recovering sulfuric acid from graphene acid-containing wastewater and corresponding technique thereof - Google Patents
Device for recovering sulfuric acid from graphene acid-containing 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
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 106
- 238000009833 condensation Methods 0.000 claims abstract description 84
- 230000005494 condensation Effects 0.000 claims abstract description 83
- 239000002699 waste material Substances 0.000 claims abstract description 29
- 238000004821 distillation Methods 0.000 claims abstract description 22
- 238000003860 storage Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- 239000007788 liquid Substances 0.000 claims description 31
- 230000008676 import Effects 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 18
- 239000012530 fluid Substances 0.000 claims description 12
- 239000002893 slag Substances 0.000 claims description 12
- 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
- 125000004122 cyclic group Chemical group 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 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
- 230000000694 effects Effects 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
- 239000012528 membrane Substances 0.000 description 2
- 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
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 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
- 239000002184 metal Substances 0.000 description 1
- 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
- 239000000049 pigment Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention provides a device for recovering sulfuric acid from graphene acid-containing wastewater, which can purify sulfuric acid from graphene wastewater to achieve the goal of cyclic utilization of resources. The recovery rate of the acid liquor is up to 92-95%. The device can recover most of heat in the operation process, thereby saving the electric power by about 30%. The device comprises a waste liquor storage tank, and is characterized by also comprising a condensation part and a distillation part, wherein the condensation part comprises two condensation units, a condensation rectification unit and a condensation heating unit; the two condensation units are respectively a first condensation unit and a second condensation unit; the first condensation unit and the second condensation unit are respectively provided with an inner cavity and an outer cavity; the lower outlet of the condensation rectification unit is communicated with the inlet of the inner cavity of the first condensation unit; the outlet of the inner cavity of the first condensation unit is communicated to a sulfuric acid container; the outlet of the condensation heating unit is provided with a condensation distillation flask; and the outlet of the condensation distillation flask is connected to the inlet of the inner cavity of the second condensation 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 from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, the present invention also provide a kind of from Graphene acid-bearing wastewater the technique of reclaim(ed) sulfuric acid.
Background technology
Graphene is a kind of monolayer carbon atomic plane material separating from graphite material, being the two-dirnentional structure of carbon, is a kind of " super material ", and it is of wide application, from electronic product to flak jackets and papermaking, even following space elevator can be taking Graphene as raw material.The preparation of Graphene is taking graphite, the vitriol oil, potassium permanganate, hydrogen peroxide as main raw material, in preparation process, can produce a large amount of Cleaning Wastewater, filtrate etc., therefore, in Graphene factory effluent, contain sulfuric acid content in the compositions, particularly waste water such as sulfuric acid, potassium permanganate, potassium permanganate, hydrogen peroxide and account for great proportion.For example produce the enterprise of Graphene wastewater flow rate 1000T/D, sulfuric acid content 30%-50% in waste water, just can reach 300T/D, and Graphene manufacturing enterprise will discharge after simple the waste water producing processing at present, and, process in waste water process and can add a large amount of alkali, produce thus a large amount of mud and must entrust the outer row of putting into process, do not meet resource three cyclical policies, cause the significant wastage of resource, cost.
Sulfuric acid is to be all widely used in industrial production or in agriculture production, the particularly a kind of important industrial raw material in industrial production, it can be used for manufacturing fertilizer, medicine, explosive, pigment, washing composition, store battery etc., also be widely used in purifying in the industry such as oil, Metal smelting and dyestuff, the a large amount of acid waste liquids that produce in Industrial processes, the mineral acid that contains different concns, if these spent acid solutions directly discharge, not only contaminate environment, and cause the waste of resource, therefore acid waste liquid becomes a significant problem needing now solution badly.
The method of processing at present spent acid solution both at home and abroad mainly contains method of enrichment, neutralisation, solvent extration, ion exchange method, membrane separation process etc., 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, neutralisation can not efficient recovery sulfuric acid wherein.At present more advanced solvent extration is very high to the requirement of extraction agent, is not suitable in large-scale commercial production; Ion exchange method is subject to the impact of ion exchange resin, spent acid solution intermediate ion upon adsorption is had higher requirements, once and its actual conditions determine, require the composition of stoste can not change too large; Membrane separation technique 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 from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, 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 approximately 30%.
A kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, 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, the second condensing unit, described the first condensing unit, the second condensation unit is all furnished with inner chamber, exocoel, the below outlet of described condensation rectification cell is communicated with the inner chamber import of described the first condensing unit, the inner chamber outlet of described the 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 inner chamber entrance of described the second condensing unit, the inner chamber outlet of described the second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell top exports 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, the 2nd distilling period, N distilling period, the natural number that wherein N is >=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 top 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 communicated to the entrance of the rectification cell of the 1st distilling period, the below outlet 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 top 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 communicated to the entrance of the rectification cell of the 2nd distilling period, until the outlet of the below of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the top of the each rectification cell in all distilling periods exports respectively by the heating system of the external outside of transfer of water vapour pipe.
It is further characterized in that:
The top that is 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, in the below inner chamber of described rectification cell, be provided with oblique baffle plate, described oblique baffle plate is drained to the below outlet of this rectification cell;
Described the first condensing unit, the second condensing unit are specially spiral prolong, the inner chamber of described spiral prolong is the internal cavity that is placed in the spiral tube spiralization of tube wall inside, the cavity that the outer wall that the exocoel of described spiral prolong is spiral tube and the inwall of tube wall form;
Heating unit in described condensation heating unit, distilling period is specially well heater, in the internal cavity of described well heater, is provided with heater strip;
The bottom of described well heater is provided with slag notch, on 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, in described cooling tank, is provided with recirculated water;
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 top outlet of described rectifying column is vapor outlet port, and the lower part outlet of described rectifying column is liquid exit;
Described distillation fraction can only 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 top 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 communicated to the entrance of the rectification cell of distilling period, and the below outlet of the rectification cell of distilling period is communicated to the liquid-inlet of described condensation heating unit.
A kind of from Graphene acid-bearing wastewater the technique of reclaim(ed) sulfuric acid, 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:
A waste liquid passes into after the exocoel entrance of the first condensing unit, after the hydrothermal solution heating of the inner chamber of the first condensing unit, flow into the exocoel entrance of the second condensing unit from the exocoel outlet of the first condensing unit, after the hydrothermal solution of the inner chamber of the second condensing unit heats again, flow into the entrance of distillation fraction by thrust-augmenting nozzle from the exocoel outlet of the second condensing unit;
B by the control of temperature in the heating unit internal cavity to 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 outlet of the top 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 outlet of the below 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 is first distilled 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 outlet of the top 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, in every section of distilling period, first adjust through the fluid temperature to 110 of heating unit DEG C～115 DEG C, 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, be positioned at the acid solution that the condensable predistillation of matrass of the outlet of heating unit goes out, reach the object that reduces acid solution loss, heat after about 20min～40min, heighten fluid temperature to 155 in heating unit DEG C～190 DEG C, being beneficial to acid solution steam distillates, 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 acid solution that density is larger flows into the heating unit of next section of distilling period through the lower part outlet of rectification cell lower end, until the outlet of the rectification cell of N distilling period flows into the liquid-inlet of condensation heating unit,
In c step, adjust 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 distilling out of condensation matrass of the outlet of condensation heating unit, reach the object that reduces acid solution loss, after heating 20min～40min, adjust the fluid temperature to 155 DEG C of condensation heating unit～190 DEG C, first distillate after heating is further rectifying in condensation rectification cell, and secondary distillate is collected cooling from the outlet of condensation rectification cell lower end in the first condensing unit flows into cooling tank structure.
Adopt after the present invention, acid solution is equipped with two kinds of temperature through heating unit, the condensation heating unit of every section of distilling period around time, distill out respectively water vapour and sulfuric acid vapor, improve the liquid-tight degree of recovered acid, liquid distillates through the outlet of the top of heating unit, distillates dregs and discharge through the bottom of heating unit slag notch in waste liquid; Install two sections of condensing units and have good condensation, heats, wherein cooling distillate temperature, heating process waste liquid temperature, make full use of in system and produce heat, economizes on resources; And the matrass of heating unit top all has micro-condensation.The device of this invention allows 1100 DEG C of working temperatures, chemical stability is good, 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 collect 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 approximately 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.
Brief description of the drawings
Fig. 1 is the structural representation block diagram of device specific embodiment of the present invention;
In Fig. 1, dotted arrow is that water vapour flows to, solid arrow is flow direction, and wherein the arrow of the slag notch below, bottom of primary heater 11, secondary heater 8 is that dregs are got rid of direction.
Embodiment
A kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, 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, the second condensing unit, described the first condensing unit, the second condensation unit is all furnished with inner chamber, exocoel, the below outlet of described condensation rectification cell is communicated with the inner chamber import of described the first condensing unit, the inner chamber outlet of described the 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 inner chamber entrance of described the second condensing unit, the inner chamber outlet of described the second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell top exports 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, the 2nd distilling period, N distilling period, the natural number that wherein N is >=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 top 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 communicated to the entrance of the rectification cell of the 1st distilling period, the below outlet 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 top 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 communicated to the entrance of the rectification cell of the 2nd distilling period, until the outlet of the below of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the top of the each rectification cell in all distilling periods exports respectively by the heating system of the external outside of transfer of water vapour pipe.
Specific embodiment, see Fig. 1: wherein N=1, only has one section of distilling period, 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 outlet of the first spiral prolong 5 is communicated to the exocoel entrance of the second spiral prolong 6, 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 top outlet of secondary heater 8 is communicated to the import of after-fractionating bottle 9, the outlet of after-fractionating bottle 9 is communicated to the entrance of the second rectifying column 10, the below outlet of the second rectifying column 10 is communicated to the liquid-inlet of primary heater 11, the top 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 inner chamber entrance of the second spiral prolong 6, the inner chamber outlet of the second spiral prolong 6 is communicated to the entrance of the first rectifying column 13, the first rectifying column 13, the top outlet of the second rectifying column 10 is (not shown in FIG. by the heating system of transfer of water vapour pipe 14 external outsides respectively, 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 inner chamber outlet 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, in cooling tank 16, is provided with recirculated water.
The inner chamber of the first spiral prolong 5, the second spiral prolong 6 is the internal cavity that is placed in the spiral tube spiralization of tube wall inside, the cavity that the outer wall that the exocoel of the first spiral prolong 5, the second spiral prolong 6 is spiral tube and the inwall of tube wall form; In the internal cavity of primary heater 11, secondary heater 8, be provided with heater strip; The bottom of primary heater 11, secondary heater 8 is provided with the slag notch 17 of closing in, is provided with valve 18 on slag notch 17; The top outlet that the top of the first rectifying column 13, the second rectifying column 10 is provided with valve 19, the first rectifying columns, the second rectifying column is vapor outlet port, and the lower part outlet of the first rectifying column 13, the second rectifying column 10 is liquid exit;
Being arranged as in distilling period: the top that the top of secondary heater 8 is furnished with after-fractionating bottle 9, after-fractionating bottle 9 is furnished with the second rectifying column 10, in the below inner chamber of the second rectifying column 10, be provided with oblique baffle plate 20, oblique baffle plate 20 is drained to the below outlet of the second rectifying column 10.
Secondary heater 8 in dashed rectangle in Fig. 1, after-fractionating bottle 9, the second rectifying column 10 is combined to form distilling period, a distilling period can be set in the present invention, two or more distilling periods also can be set, in every section of distilling period, be furnished with well heater, matrass and rectifying column, in the time that the quantity of distilling period is greater than 1, the quantity of setting distilling period is M, M is >=2 integer, now by every section of distilling period called after the 1st distilling period, the 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 top 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 communicated to the entrance of the rectifying column of the 1st distilling period, the below outlet of the 1st distilling period rectifying column is communicated to the liquid-inlet of the well heater of the 2nd distilling period, the top 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 communicated to the entrance of the rectifying column of the 2nd distilling period, until the outlet of the below of M distilling period rectifying column is communicated to the liquid-inlet of primary heater 11, owing to having comprised M distilling period, it makes the sulfuric acid that distills out purer.
The technique of a kind of in specific embodiment reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater, 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:
A waste liquid passes into after the exocoel entrance of the first spiral prolong 5, after the hydrothermal solution heating of the inner chamber of the first spiral prolong 5, flow into the exocoel entrance of the second spiral prolong 6 from the exocoel outlet of the first spiral prolong 5, after the hydrothermal solution heating of the inner chamber of the second spiral prolong 6, flow into the internal cavity of secondary heater 8 by thrust-augmenting nozzle 7 from the exocoel outlet of the second spiral prolong 6;
B by the control of temperature in secondary heater 8 internal cavities is first distilled 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 outlet of the top 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 cavities is first distilled 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 outlet of the top 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 adjust through the fluid temperature to 110 of secondary heater 8 DEG C～115 DEG C, 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 well heater, be positioned at the acid solution that the condensable predistillation of after-fractionating bottle 9 of the outlet of secondary heater 8 goes out, reach the object that reduces acid solution loss, heat after 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, being beneficial to acid solution steam distillates, 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 ends, the acid solution that density is larger flows into primary heater 11 through the lower part outlet of the second rectifying column 10 lower ends,
In c step, adjust 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 distilling out of the first matrass 12 of the outlet of primary heater 11, reach the object that reduces acid solution loss, after heating 20min～40min, adjust the fluid temperature to 155 DEG C of primary heater 11～190 DEG C, first distillate after heating is further rectifying in the first rectifying column 13, secondary distillate from the first rectifying column 13 lower ends outlets through the first spiral prolong 5 flow in cooling tank structure 15, collect cooling.
Claims (10)
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, the second condensing unit, described the first condensing unit, the second condensation unit is all furnished with inner chamber, exocoel, the below outlet of described condensation rectification cell is communicated with the inner chamber import of described the first condensing unit, the inner chamber outlet of described the 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 inner chamber entrance of described the second condensing unit, the inner chamber outlet of described the second condensing unit is communicated to the entrance of condensation rectification cell, described condensation rectification cell top exports 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, the 2nd distilling period, N distilling period, the natural number that wherein N is >=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 top 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 communicated to the entrance of the rectification cell of the 1st distilling period, the below outlet 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 top 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 communicated to the entrance of the rectification cell of the 2nd distilling period, until the outlet of the below of N distilling period rectification cell is communicated to the liquid-inlet of described condensation heating unit, the top of the each rectification cell in all distilling periods exports respectively by the heating system of the external outside of transfer of water vapour pipe.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, it is characterized in that: the top that is 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, in the below inner chamber of described rectification cell, be provided with oblique baffle plate, described oblique baffle plate is drained to the below outlet of this rectification cell.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, it is characterized in that: described the first condensing unit, the second condensing unit are specially spiral prolong, the inner chamber of described spiral prolong is the internal cavity that is placed in the spiral tube spiralization of tube wall inside, the cavity that the outer wall that the exocoel of described spiral prolong is spiral tube and the inwall of tube wall form.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, it is characterized in that: the heating unit in described condensation heating unit, distilling period is specially well heater, in the internal cavity of described well heater, is provided with heater strip.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, 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.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, 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 top outlet of described rectifying column is vapor outlet port, and the lower part outlet of described rectifying column is liquid exit.
As claimed in claim 1 a kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid, it is characterized in that: described distillation fraction can only 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 top 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 communicated to the entrance of the rectification cell of distilling period, and the below outlet of the rectification cell of distilling period is communicated to the liquid-inlet of described condensation heating unit.
8. the technique of a 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.
As claimed in claim 8 a kind of from Graphene acid-bearing wastewater the technique of reclaim(ed) sulfuric acid, it is characterized in that:
Its concrete technology step is as follows:
A waste liquid passes into after the exocoel entrance of the first condensing unit, after the hydrothermal solution heating of the inner chamber of the first condensing unit, flow into the exocoel entrance of the second condensing unit from the exocoel outlet of the first condensing unit, after the hydrothermal solution of the inner chamber of the second condensing unit heats again, flow into the entrance of distillation fraction by thrust-augmenting nozzle from the exocoel outlet of the second condensing unit;
B by the control of temperature in the heating unit internal cavity to 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 outlet of the top 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 outlet of the below 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 is first distilled 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 outlet of the top 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.
As claimed in claim 9 a kind of from Graphene acid-bearing wastewater the technique of reclaim(ed) sulfuric acid, it is characterized in that:
In b step, in every section of distilling period, first adjust through the fluid temperature to 110 of heating unit DEG C～115 DEG C, 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, be positioned at the acid solution that the condensable predistillation of matrass of the outlet of heating unit goes out, reach the object that reduces acid solution loss, heat after about 20min～40min, heighten fluid temperature to 155 in heating unit DEG C～190 DEG C, being beneficial to acid solution steam distillates, 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 acid solution that density is larger flows into the heating unit of next section of distilling period through the lower part outlet of rectification cell lower end, until the outlet of the rectification cell of N distilling period flows into the liquid-inlet of condensation heating unit,
In c step, adjust 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 distilling out of condensation matrass of the outlet of condensation heating unit, reach the object that reduces acid solution loss, after heating 20min～40min, adjust the fluid temperature to 155 DEG C of condensation heating unit～190 DEG C, first distillate after heating is further rectifying in condensation rectification cell, and secondary distillate is collected cooling from the outlet of condensation rectification cell lower end in the first condensing unit flows into cooling tank structure.
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