CN108103585B - A kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid - Google Patents

A kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid Download PDF

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CN108103585B
CN108103585B CN201711424298.9A CN201711424298A CN108103585B CN 108103585 B CN108103585 B CN 108103585B CN 201711424298 A CN201711424298 A CN 201711424298A CN 108103585 B CN108103585 B CN 108103585B
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isopropanol
sodium hydroxide
waste liquid
tower
monocrystalline silicon
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CN108103585A (en
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杨帆
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Huzhou Fluid Membrane Separation Technology Co Ltd
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Huzhou Fluid Membrane Separation Technology Co Ltd
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    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B33/00After-treatment of single crystals or homogeneous polycrystalline material with defined structure
    • C30B33/08Etching
    • C30B33/10Etching in solutions or melts
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/20Silicates
    • C01B33/32Alkali metal silicates
    • C01B33/325After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/26Treatment of water, waste water, or sewage by extraction
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/82Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32

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  • Organic Chemistry (AREA)
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  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
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  • Metallurgy (AREA)
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  • Silicon Compounds (AREA)
  • Detergent Compositions (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a kind of processing methods of fine-hair maring using monocrystalline silicon slice waste liquid, waste liquid is divided into aqueous 12.6% thick isopropanol and the mixed solution of sodium hydroxide and sodium metasilicate by slightly steaming, the mixed solution of sodium hydroxide and sodium metasilicate is separated into sodium hydroxide solution and sodium silicate solution with back extraction by extraction, sodium silicate solution is directly recycled for many industrial circles;Sodium hydroxide solution distills to form solid sodium hydroxide by nitrogen charging, as dehydrating agent for being carried out dehydrating to thick isopropanol, or be back in monocrystalline silicon making herbs into wool, the isopropanol after dehydration obtains high-purity isopropanol of the water content less than 0.5% using azeotropic distillation.The present invention realizes height reuse and the harmless discharge of fine-hair maring using monocrystalline silicon slice waste liquid, saves the consumption of chemical raw material, and reduce the discharge and processing cost of organic wastewater, protects environment while reducing production cost.

Description

A kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid
Technical field
The present invention relates to solar energy industry sewage treatment field, in particular to a kind of processing side of fine-hair maring using monocrystalline silicon slice waste liquid Method.
Background technique
Due to its safety, of low pollution, recyclable and unlimited resource excellent properties, solar energy becomes human development must be by Clean energy resource, compared with the availability of other energy, advantage is fairly obvious, Chinese photovoltaic industry since 2004 rapidly Development, solar cell yield also gradually start to walk, begin to take shape for years by the first in the world, photovoltaic power generation market at present, row Industry is integrally more and more prosperous.But the exhaust gas waste water that manufacture of solar cells process itself can generate varied complicated component is useless Slag does not meet solar energy " cleaning products " if cannot timely and effectively carry out processing can generate serious pollution to external environment Self-image.
Monocrystalline silicon cell piece be monocrystalline silicon piece is passed sequentially through to cleaning, making herbs into wool, diffusion, etching, Both Plasma Chemical Vapor sink The processes such as product, silk-screen printing are made.Wherein making herbs into wool process is to utilize the monocrystalline silicon of different crystal orientations corrosion rate in alkaline solution Different principles corrodes the monocrystalline silicon piece cleaned up in alkaline solution out similar to the pyramid flannelette knot that specification does not arrange Structure reduces the surface reflectivity of monocrystalline silicon battery, improves short circuit current, the final photoelectric conversion efficiency for improving battery.Caustic corrosion When silicon, bubble generation is had with the carry out silicon chip surface of corrosion, size and solution viscosity, the solution surface tension of bubble have It closes, diameter, density and the rate of corrosion reaction of bubble define the geometrical characteristic of silicon chip surface texture.Add in etchant solution The wetness degree of silicon and solution can be improved by entering isopropanol one, play the role of surfactant, two adjustable bubbles it is big Small and quantity, plays the role of defoaming, and concentration of the three adjustable reaction product sodium metasilicate in etchant solution is adjusted to silicon The corrosion dynamics of piece plays the role of the viscosity property for adjusting solution.And the concentration of sodium metasilicate is excessive will lead to silicon wafer and cassette Bezel contact position can generate " flower basket mark ", and the concentration of sodium metasilicate can only adjust concentration, thus making herbs into wool by discharge solution Liquid needs not stop to replace, and thus generates a large amount of making herbs into wool waste liquid, but the making herbs into wool waste liquid being discharged be not it is entirely ineffective, how will Effective component recycling therein is to reduce chemicals usage, reduces the discharge of organic sewage, alleviating environmental pressure is monocrystalline The important research direction of silicon production waste water treatment.
Summary of the invention
The object of the present invention is to provide a kind of processing methods of fine-hair maring using monocrystalline silicon slice waste liquid, can sufficiently handle and reuse system Each main component in suede waste liquid reduces the dosage of chemicals, reduces production cost, greatly reduces the discharge of organic wastewater, benefit In protection environment.
Above-mentioned technical purpose of the invention has the technical scheme that
A kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid, includes the following steps:
(A) fine-hair maring using monocrystalline silicon slice waste liquid is delivered to from waste liquid tank the thick tower that steams and carries out binary azeotropic distillation, passed through by tower top First condenser condenses to obtain the thick isopropanol of isopropanol azeotrope with water formation, obtains the water of sodium hydroxide and sodium metasilicate by tower bottom Solution;
(B) aqueous solution of sodium hydroxide obtained in step (A) and sodium metasilicate is delivered in extraction tower (4) using extraction Agent extracts sodium hydroxide, is condensed to obtain the extraction agent solution of sodium hydroxide through the second condenser by tower top, be obtained by tower bottom To the aqueous solution of sodium metasilicate;
(C) by the extraction agent solution of sodium hydroxide obtained in step (B) be delivered in stripping column using stripping agent into Row back extraction retrieves extractant used in step through the condensation of third condenser as tower top, obtains sodium hydroxide by tower bottom Back extraction agent solution;
(D) the back extraction agent solution of sodium hydroxide obtained in step (C) is subjected to nitrogen charging distillation by distiller, distillation removes Remove stripping agent, the solid sodium hydroxide after crystallisation by cooling is obtained in distiller;
(E) thick isopropanol obtained in step (A) is delivered in drain sump, uses solid hydrogen obtained in step (D) Sodium oxide molybdena is dehydrated thick isopropanol as dehydrating agent, is during which kept stirring, then stratification, respectively obtains aqueous Measure the isopropanol and sodium hydroxide solution less than 2%;
(F) isopropanol of the water content less than 2% obtained in step (E) is delivered in sequence of constant boiling and rectification tower and carries out azeotropic essence Evaporate, by tower top through the 5th condenser condense to obtain containing isopropanol, water, nonvariant boiling reagent ternary azeotrope, water content is obtained by tower bottom Isopropanol less than 0.5%;
(G) by obtained in step (F) containing isopropanol, water, nonvariant boiling reagent ternary azeotrope be delivered to liquid separator into Row layering, upper layer obtain nonvariant boiling reagent and recycle and are supplemented to sequence of constant boiling and rectification tower using, and lower layer obtains isopropanol, water and remaining The mixture of nonvariant boiling reagent;
(H) mixture of isopropanol, water and remaining nonvariant boiling reagent that step (G) obtains reboil column is delivered to carry out again Processing, by tower top through the 6th condenser condensation obtain again containing isopropanol, water, nonvariant boiling reagent ternary azeotrope and be recycled to liquid In separator, the tower bottom kettle liquid being made of isopropyl alcohol and water returns to thick steam in tower and re-starts separation.
Preferably, the tower top temperature range for slightly steaming tower in step (A) is 70~75 DEG C, column bottom temperature range is 80~85 DEG C, tower top pressure 0.05MPa, reflux temperature is 45 DEG C, and the mass concentration of water is 12.6% in thick isopropanol.
Preferably, in step (B) in the aqueous solution of sodium hydroxide and sodium metasilicate sodium hydroxide mass concentration be 17%~ 32%, extractant is saturated acetic acid potassium ethylene glycol, and the agent material mass ratio of extractant and sodium hydroxide is 1:3, extraction temperature 40 DEG C, time range is 1.5~2 hours, produces 80 DEG C of temperature.
Preferably, strippant in step (C) is pure water, the agent material mass ratio of strippant and sodium hydroxide is 3: 1, back extraction temperature is 50 DEG C, and time range is 0.5~1 hour.
Preferably, the nitrogen pressure of the distiller (6) in step (D) is 0.1MPa, temperature is 150 DEG C, time range It is 10~15 minutes.
Preferably, the mass ratio of solid sodium hydroxide used in step (E) and thick isopropanol is 1:9~1:7.
Preferably, nonvariant boiling reagent used in step (F) is one of ethylene glycol, glycerol, hexamethylene, C6 oil, azeotropic The agent material mass ratio of agent and isopropanol is 1:2, and extraction temperature is 35 DEG C, and extraction time is 2 hours, and reflux ratio is 1:0.5~1: 5, extraction temperature is 85 DEG C.
In conclusion the invention has the following advantages:
The present invention provides a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid: by slightly steam by waste liquid be divided into thick isopropanol, The mixed solution of sodium hydroxide and sodium metasilicate is separated by extraction with back extraction by the mixed solution of sodium hydroxide and sodium metasilicate Sodium hydroxide solution and sodium silicate solution, sodium silicate solution is widely used, can direct reuse in numerous areas;Sodium hydroxide solution It distills to form solid sodium hydroxide by nitrogen charging, as dehydrating agent for being carried out dehydrating thick isopropanol, after dehydration Isopropanol and sodium hydroxide solution of the water content less than 2% are obtained, sodium hydroxide solution can re-start nitrogen charging distillation supplement conduct Reuse is into monocrystalline silicon making herbs into wool after dehydrating agent or dilution, wherein extractant and the recyclable reuse of strippant;At dehydration Isopropanol after reason obtains qualified industrial isopropanol of the water content less than 0.5% using azeotropic distillation, and passes through reboil column Processing carry out nonvariant boiling reagent reuse and tail washings processing again, isopropanol obtained can reuse into monocrystalline silicon making herbs into wool or use In other industrial uses.The main component of fine-hair maring using monocrystalline silicon slice waste liquid: isopropanol, sodium hydroxide, sodium metasilicate be completely segregated with Processing, the dehydration of isopropanol, sodium hydroxide reuse into monocrystalline silicon making herbs into wool, when wherein sodium hydroxide can be used as reuse isopropanol Agent, sodium metasilicate are used for other industrial uses, height reuse and the harmless discharge of fine-hair maring using monocrystalline silicon slice waste liquid are realized, to reduce Production cost, and protect environment.
Detailed description of the invention
Fig. 1 is the process flow chart of the fine-hair maring using monocrystalline silicon slice liquid waste processing designed according to the application.
Specific embodiment
The present invention will be further described in detail for scheme with reference to the accompanying drawing and preferably.
This specific embodiment is only explanation of the invention, is not limitation of the present invention, those skilled in the art Member can according to need the modification that not creative contribution is made to the present embodiment after reading this specification, but as long as at this All by the protection of Patent Law in the scope of the claims of invention.
Embodiment 1
As shown in Figure 1, a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid, gives up fine-hair maring using monocrystalline silicon slice from waste liquid tank 1 Liquid send to the thick progress binary azeotropic distillation tower top of tower 2 that steams and obtains the thick isopropanol that water content is 12.6%, and tower bottom obtains sodium hydroxide Mass concentration range with sodium metasilicate is respectively 10%~15% and 15%~20% aqueous solution;The aqueous solution is sent into extraction tower 4 Sodium hydroxide extraction is carried out, extractant is saturated acetic acid potassium ethylene glycol, and the agent material mass ratio of extractant and sodium hydroxide is 1:3, Extraction temperature is 40 DEG C, and time range is 1.5~2 hours, produces 80 DEG C of temperature, tower top obtains the extraction of the sodium hydroxide of oily phase Agent solution, tower bottom obtain the aqueous solution of the sodium metasilicate of water phase;The extraction agent solution of sodium hydroxide send anti-to progress in stripping column 5 Extraction, strippant are pure water, and the agent material mass ratio of strippant and sodium hydroxide is 3:1, and back extraction temperature is 50 DEG C, time model Enclosing is 0.5~1 hour, and tower top retrieves extractant and is supplemented in extraction tower 4, and the stripping agent that tower bottom obtains sodium hydroxide is molten Liquid;The back extraction agent solution of sodium hydroxide, which is sent into distiller 6, carries out nitrogen charging distillation, and the nitrogen pressure of distiller 6 is 0.1MPa, temperature Degree is 150 DEG C, and time range is 10~15 minutes, distills out stripping agent and supplements back stripping column 5, obtains in distiller 6 cold But the solid sodium hydroxide after crystallizing;It is sent into solid sodium hydroxide obtained as dehydrating agent and aforementioned thick isopropanol obtained Drain sump 7 carries out thick isopropanol dehydration, and the mass ratio of solid sodium hydroxide and thick isopropanol is 1:9~1:7, is stirred, and stands, obtains Isopropanol layer and sodium hydrate aqueous solution layer to water content less than 2%;Isopropanol by water content obtained less than 2% is sent to perseverance It boils rectifying column 8 and carries out sequence of constant boiling and rectification, the nonvariant boiling reagent used is glycerol, and the agent material mass ratio of nonvariant boiling reagent and isopropanol is 1:2, rectifying Temperature is 67 DEG C~72 DEG C, and the rectifying time is 2 hours, and reflux ratio is 1:0.5~1:5, and extraction temperature is 85 DEG C, and tower top is contained Isopropanol, water, the ternary azeotrope of nonvariant boiling reagent, tower bottom distillate isopropanol of the water content less than 0.5%;Ternary azeotrope is sent into liquid It is layered in body separator 9, upper layer obtains nonvariant boiling reagent and is supplemented in sequence of constant boiling and rectification tower 8, and lower layer obtains isopropanol, water And the mixture of remaining nonvariant boiling reagent;The mixture of isopropanol, water and remaining nonvariant boiling reagent is sent into reboil column 10 again Processing, tower top retrieve ternary azeotrope and return in liquid separator 9 together with the ternary azeotrope newly distillated again Processing, tower bottom distillates isopropanol and thick steam in tower 2 of kettle liquid return of water re-starts processing.
By above step, isopropanol, sodium hydroxide, sodium metasilicate are kept completely separate, and sodium hydroxide is used as dehydrating agent Obtaining sodium hydrate aqueous solution in the Treatment for Reuse of isopropanol, after use can not only be used for raw material and rejoins in distiller again It is used to prepare solid sodium hydroxide, and in fine-hair maring using monocrystalline silicon slice technique, the recycling of isopropanol obtains direct reuse after can diluting High-purity isopropanol of the water content less than 0.5%, can also be back in fine-hair maring using monocrystalline silicon slice technique, and be applied to other industrial fields It closes, sodium silicate aqueous solution is commonly called as waterglass, can be used for being widely used in multiple fields, thus the master in fine-hair maring using monocrystalline silicon slice waste water It wants ingredient all to carry out being effectively treated and reuse, saves chemical raw material, reduce the discharge and processing cost of organic wastewater, save Cost benefits environment.
Embodiment 2
Using the process flow similar with embodiment 1, the thick tower bottom for steaming tower 2 obtains the matter of sodium hydroxide and sodium metasilicate Amount concentration range is respectively 15%~20% and 10%~15% aqueous solution;Carrying out the extractant that sodium hydroxide extraction uses is second two The agent material mass ratio of alcohol, extractant and sodium hydroxide is 1:2, and extraction temperature is 35 DEG C, and time range is 2~2.5 hours, extraction 82 DEG C of temperature;Nitrogen pressure to the distiller 6 of the back extraction agent solution progress nitrogen charging distillation of sodium hydroxide is 0.15MPa, temperature It is 150 DEG C, time range is 15~20 minutes;Solid sodium hydroxide obtained is used to take off as dehydrating agent to thick isopropanol When water, the mass ratio of solid sodium hydroxide and thick isopropanol is 1:12~1:9, is stirred, and stands, obtains water content less than 2.5% Isopropanol layer and sodium hydrate aqueous solution layer;Isopropanol by water content obtained less than 2.5% send to sequence of constant boiling and rectification tower 8 and carries out Sequence of constant boiling and rectification, the nonvariant boiling reagent used are cyclohexane, and the agent material mass ratio of nonvariant boiling reagent and isopropanol is 0.428:1, and rectification temperature is 78 DEG C~82 DEG C, the rectifying time is 2 hours, reflux ratio 1:19, and extraction temperature is 88 DEG C, and sequence of constant boiling and rectification tower tower bottom distillates aqueous Measure the isopropanol less than 0.55%.
Embodiment 3
Using the process flow similar with embodiment 1, the thick tower bottom for steaming tower 2 obtains the matter of sodium hydroxide and sodium metasilicate Amount concentration range is respectively 20%~25% and 15%~20% aqueous solution;Carrying out the extractant that sodium hydroxide extraction uses is C6 The agent material mass ratio of oil, extractant and sodium hydroxide is 1:1.5, and extraction temperature is 45 DEG C, and time range is 2.3~2.8 hours, 78 DEG C of temperature of extraction;Nitrogen pressure to the distiller 6 of the back extraction agent solution progress nitrogen charging distillation of sodium hydroxide is 0.18MPa, Temperature is 150 DEG C, and time range is 18~25 minutes;Use solid sodium hydroxide obtained as dehydrating agent to thick isopropanol into When row dehydration, the mass ratio of solid sodium hydroxide and thick isopropanol is 1:8.5~1:6.5, is stirred, and stands, it is small to obtain water content Isopropanol layer and sodium hydrate aqueous solution layer in 1.8%;Isopropanol by water content obtained less than 1.8% is sent to sequence of constant boiling and rectification Tower 8 carries out sequence of constant boiling and rectification, and the nonvariant boiling reagent used is hexamethylene, and the agent material mass ratio of nonvariant boiling reagent and isopropanol is 1:0.426, rectifying Temperature is 67 DEG C~72 DEG C, and the rectifying time is 2 hours, reflux ratio 1:19, and extraction temperature is 75 DEG C, and sequence of constant boiling and rectification tower tower bottom evaporates Isopropanol of the water content less than 0.45% out.

Claims (7)

1. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid, includes the following steps:
(A) fine-hair maring using monocrystalline silicon slice waste liquid is delivered to thick steam tower (2) from waste liquid tank (1) and carries out binary azeotropic distillation, by tower top The thick isopropanol of isopropanol azeotrope with water formation is obtained through the first condenser (31) condensation, sodium hydroxide and silicic acid are obtained by tower bottom The aqueous solution of sodium;
(B) aqueous solution of sodium hydroxide obtained in step (A) and sodium metasilicate is delivered in extraction tower (4) and uses extractant pair Sodium hydroxide is extracted, and is obtained the extraction agent solution of sodium hydroxide through the second condenser (32) condensation by tower top, is obtained by tower bottom To the aqueous solution of sodium metasilicate;
(C) the extraction agent solution of sodium hydroxide obtained in step (B) is delivered in stripping column (5) and is carried out using stripping agent Back extraction retrieves extractant used in step (B) through third condenser (33) condensation as tower top, obtains hydrogen-oxygen by tower bottom Change the back extraction agent solution of sodium;
(D) the back extraction agent solution of sodium hydroxide obtained in step (C) is subjected to nitrogen charging distillation by distiller (6), distilled It to stripping agent and supplements back stripping column (5), obtains the solid sodium hydroxide after crystallisation by cooling in distiller (6);
(E) thick isopropanol obtained in step (A) is delivered in drain sump (7), uses solid hydrogen-oxygen obtained in step (D) Change sodium to be dehydrated thick isopropanol as dehydrating agent, is during which kept stirring, then stratification, respectively obtain water content Isopropanol and sodium hydrate aqueous solution less than 2%;
(F) isopropanol of the water content less than 2% obtained in step (E) is delivered in sequence of constant boiling and rectification tower (8) and carries out azeotropic essence Evaporate, by tower top through the 4th condenser (34) condensation obtain containing isopropanol, water, nonvariant boiling reagent ternary azeotrope, contained by tower bottom Isopropanol of the water less than 0.5%;
(G) the ternary azeotrope containing isopropanol, water, nonvariant boiling reagent obtained in step (F) is delivered to liquid separator (9) progress Layering, upper layer obtain nonvariant boiling reagent and are recycled to be supplemented to sequence of constant boiling and rectification tower (8) use, and lower layer obtains isopropanol, water and residual Nonvariant boiling reagent mixture;
(H) mixture of isopropanol, water and remaining nonvariant boiling reagent that step (G) obtains reboil column (10) are delivered to carry out again Processing, by tower top through the 5th condenser (35) condensation obtain again containing isopropanol, water, nonvariant boiling reagent ternary azeotrope and be recycled to In liquid separator (9), the tower bottom kettle liquid being made of isopropyl alcohol and water returns to thick steam in tower (2) and re-starts separation.
2. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (A) The thick tower top temperature range for steaming tower (2) is 70~75 DEG C, and column bottom temperature range is 80~85 DEG C, tower top pressure 0.05MPa, is returned Flowing temperature is 45 DEG C, and the mass concentration of water is 12.6% in thick isopropanol.
3. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (B) Sodium hydroxide mass concentration is 17%~32% in the aqueous solution of sodium hydroxide and sodium metasilicate, and extractant is saturated acetic acid potassium second two The agent material mass ratio of alcohol, extractant and sodium hydroxide is 1:3, and extraction temperature is 40 DEG C, and time range is 1.5~2 hours, extraction 80 DEG C of temperature.
4. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (C) Strippant be pure water, the agent material mass ratio of strippant and sodium hydroxide is 3:1, and back extraction temperature is 50 DEG C, time range It is 0.5~1 hour.
5. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (D) Distiller (6) nitrogen pressure be 0.1MPa, temperature be 150 DEG C, time range be 10~15 minutes.
6. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (E) The mass ratio of the solid sodium hydroxide and thick isopropanol that use is 1:9~1:7.
7. a kind of processing method of fine-hair maring using monocrystalline silicon slice waste liquid according to claim 1, it is characterised in that: in step (F) The nonvariant boiling reagent used is one of ethylene glycol, glycerol, hexamethylene, C6 oil, and the agent material mass ratio of nonvariant boiling reagent and isopropanol is 1: 2, extraction temperature is 35 DEG C, and extraction time is 2 hours, and reflux ratio is 1:0.5~1:5, and extraction temperature is 85 DEG C.
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