CN113104865B - Treatment method of vat blue RSN refining mother liquor - Google Patents
Treatment method of vat blue RSN refining mother liquor Download PDFInfo
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- CN113104865B CN113104865B CN201911288646.3A CN201911288646A CN113104865B CN 113104865 B CN113104865 B CN 113104865B CN 201911288646 A CN201911288646 A CN 201911288646A CN 113104865 B CN113104865 B CN 113104865B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/14—Preparation of sulfites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/30—Purification; Separation by crystallisation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B5/00—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings
- C09B5/24—Dyes with an anthracene nucleus condensed with one or more heterocyclic rings with or without carbocyclic rings the heterocyclic rings being only condensed with an anthraquinone nucleus in 1-2 or 2-3 position
- C09B5/44—Azines of the anthracene series
- C09B5/46—Para-diazines
- C09B5/48—Bis-anthraquinonediazines (indanthrone)
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Abstract
The invention discloses a method for treating vat blue RSN refining mother liquor, which comprises the following steps: (1) Introducing the refined mother liquor into a filter to remove the precipitated solid vat blue RSN; (2) Evaporating and concentrating, further oxidizing to form solid reduction blue RSN precipitate, further evaporating and concentrating, when sodium hydroxide in the solution is close to saturation, entering a heat preservation sedimentation tank to precipitate and deposit suspended sodium sulfite, and removing cold precipitation from the high-concentration sodium hydroxide solution; the mixed solid phase enters a beating tank to completely strip sodium sulfite and solid reduction blue RSN; (3) Treating the clarified liquid by a flash crystallization cold separation device to separate sodium hydroxide; (4) Pulping the mixed solid obtained in the step (2), and separating sodium sulfite and crude solid reduction blue RSN; according to the invention, the reduction blue RSN entrained in the mother liquor is recovered, the yield of the reduction blue RSN is improved, excessive sodium hydroxide in a reaction system is recovered, sodium sulfite as a byproduct is separated, zero emission of mother liquor treatment is realized, and the production cost of the reduction blue RSN is reduced.
Description
Technical Field
The invention relates to a method for treating vat blue RSN refining mother liquor, which is used for treating vat blue RSN refining mother liquor.
Background
Anthraquinone vat dyes have a long history, and vat blue RSN has been found in 1901 to over 100 years ago, and is one of important cotton dyes for manufacturing cellulose fiber advanced products or functional products. With the rapid development of national economy, the consumer demand of people gradually tends to be diversified, the demands on the functionality, the comfort and the fashion property of textiles are higher and higher, and more than half of the textile demands are expected to reach the middle-high-grade demands in 2020.
Vat dye RSN is a dye that is reduced under alkaline conditions to color the fiber, oxidized, and recovered to the original insoluble dye on the fiber for dyeing, and is used for dyeing cellulose fiber; the insoluble vat dye is prepared into sodium sulfate salt, and can be changed into soluble vat dye, and is mainly used for cotton cloth printing. The vat dye is a dye with excellent performance, has bright color, complete color spectrum, excellent dyeing effect fastness, especially high light fastness, and is an extremely important dye variety in the dyeing of various textiles with high dyeing quality at present. Can also be used as a raw material for manufacturing high-grade pigment, and can be used for military industry, automobile spraying, printing ink and the like.
China is a world-recognized large textile country, and with the rapid development of the Chinese textile industry, the requirement for dye chemicals is increased, and the interdependence of the dye industry and the textile industry shows that the market of the dye industry in China is huge. According to statistics, the total output of the dyes and the organic pigments in China reaches over 100 ten thousand tons in 2012, the total output of the dyes and the organic pigments in China exceeds 40 ten thousand tons in China, and the output, the export and the consumption of the dyes in China are listed in the first countries of the world.
The production of vat blue RSN generally comprises condensation, water separation, adding sodium hydrosulfite into alkaline solution for refining reduction, oxidation acidification for neutralization, washing and drying to obtain vat blue RSN product.
The production reaction engineering equation is as follows:
condensation:
refining and reducing:
oxidative acidification:
by analyzing physicochemical properties and reaction mechanisms of the vat blue RSN, the vat blue RSN production mother liquor mainly comprises the following components: sodium sulfite, sodium hydroxide, a small amount of leuco reduction blue RSN sodium salt and a small amount of water with 90% of leuco reduction blue RSN potassium salt.
The mother liquor for producing the reduction blue RSN has high-salt and high-BOD industrial wastewater, and 50 tons of industrial washing water can be produced per ton of reduction blue RSN. The waste water is firstly subjected to acid-base neutralization, then is desalted by a four-effect evaporation device, and mixed salt with solid content more than 80% generated by a centrifugal machine is used as solid waste to be further concentrated treated, and the generated sewage cold water and other waste water are fed into an adjusting tank together to adjust the water quality and water quantity. Because of the lack of nitrogen and phosphorus in the wastewater, a proper amount of urea and sodium dihydrogen phosphate are added to meet the balanced requirement of anaerobic and aerobic microorganism growth on nutrition (COD: N: P=100-500: 5: 1). Waste water in the regulating tank is pumped by a lifting pump and flows into a secondary UASB automatically, organic matters in the waste water are adsorbed and decomposed into methane, carbon dioxide, water and micromolecular substances by anaerobic microorganisms in the anaerobic reactor, and the biogas generated by the anaerobic reaction has small quantity and no recovery value and is discharged from a 15m high-exhaust funnel at high altitude. The effluent of the anaerobic reactor enters an anaerobic sedimentation tank, and the carried anaerobic sludge is sedimentated and flows back to the anaerobic tower. The effluent of the anaerobic tower enters a biological contact oxidation pond, a combined biological filler for microorganism growth and an aerator for providing oxygen for microorganisms are arranged in the pond, and residual organic matters in the wastewater are adsorbed, oxidized and decomposed into carbon dioxide and water by the microorganisms attached to the filler; the effluent of the biological contact oxidation pond enters a secondary sedimentation tank to precipitate the fallen biological film and activated sludge, and then the effluent reaches the standard and is discharged.
And (3) after the sludge left by the secondary sedimentation tank and the UASB anaerobic reactor enters a sludge concentration tank for concentration, the sludge is sent into a spiral-pile type sludge dehydrator for dehydration, filtrate returns to an adjusting tank, and the obtained sludge with the water content of about 80% is finally treated according to general solid waste.
Because the water quantity and the water quantity of the washing water are large, a large amount of vat blue RSN enters the production wastewater, the yield of vat blue RSN is reduced, a large amount of sodium hydroxide is neutralized by sulfuric acid, the raw material waste is serious, and the production cost is high. How to produce vat blue RSN dye intermediate is clean and pollution-free, improves the yield of vat blue RSN, and reduces the production cost, which becomes a main problem facing dye intermediate production enterprises. The difficult treatment of mother liquor (waste water) and the protection of ecological environment directly affect the development and production scale of the reduction blue RSN enterprises.
Disclosure of Invention
The invention aims to solve the technical problem of providing a treatment method for refining mother liquor of vat blue RSN (the same applies to vat bleaching blue BC), which has the advantages of simple operation, pure physics in the treatment process, no addition of any additive, no residue of extracted products, low energy consumption and low cost, and can be continuously treated.
In order to solve the technical problems, the method for treating the vat blue RSN refined mother liquor comprises the following steps:
(1) The sodium salt of leuco vat blue RSN in the refined mother liquor is oxidized to generate solid vat blue RSN, the refined mother liquor is led into a filter, the precipitated solid vat blue RSN is removed, and the clear refined mother liquor is obtained, and the solid vat blue RSN is further refined as a crude product.
(2) Evaporating and concentrating the clarified refined mother liquor (such as a four-effect evaporator or an MVR evaporator), further oxidizing leuco vat blue RSN sodium salt to form solid vat blue RSN sediment, wherein sodium sulfite is far less soluble at high temperature than sodium hydroxide, and is separated out firstly along with water evaporation, further evaporating and concentrating, the concentration of sodium hydroxide in the refined mother liquor is higher and higher, when sodium hydroxide in a system (evaporating system) solution is close to saturation, mixing solid and liquid into a heat-preserving sedimentation tank, separating and depositing sodium sulfite suspended in the system, and conveying the high-concentration sodium hydroxide solution to a cold-separation section; the mixed solid phase enters a beating tank to completely strip sodium sulfite and solid vat blue RSN, and vapor is condensed and recovered by utilizing the principle of suspension centrifugal separation.
(3) The principle that the solubility of sodium hydroxide is reduced along with the reduction of the temperature is utilized, the sodium hydroxide solution obtained in the step (2) is treated by adopting a flash crystallization cold precipitation device (for example, a three-stage flash crystallization cold precipitation device is adopted, the technical requirement of flash crystallization under the adiabatic condition is met, the spontaneous conversion of heat energy and kinetic energy is realized, the operation energy consumption is lower), the temperature is cooled from 100 ℃ to 30 ℃, the sodium sulfite solubility reaches the maximum at the moment, the quality of separated sodium hydroxide is higher, sodium hydroxide is separated, and the sodium hydroxide can be obtained after filtering and leaching and can be returned to a production section for recycling or be sold as a product after being dried and packaged.
(4) And (3) pulping the mixed solid obtained in the step (2) according to the difference of water solubility, granularity and specific gravity of the solid vat blue RSN and sodium sulfite, stripping adhered particles of different substances, and separating the sodium sulfite and the crude solid vat blue RSN by utilizing a suspension centrifugal separation principle. Sodium sulfite is filtered, leached, dried and packaged to be sold, and the product is further refined into a product after being washed by vat blue RSN or is used as a vat bleaching blue BC raw material to be used as a downstream raw material.
The method of the present invention further comprises a step of collecting condensed water produced by evaporation in step (2). When the four-effect evaporator is adopted, the I, II and III-effect condensed water is returned to the water system or is used as softened water for a production system, and the IV-effect condensed water is cooled by the mixed condenser and enters the cooling water circulation system for recycling.
The treatment method is a physical treatment technology, no additive is added, and the separated products can be returned to the production section to be used as production raw materials.
By adopting the four-effect evaporation concentration technology, the process is mature, and the steam consumption is only 0.3 ton/ton of refined mother liquor.
The technology of three-stage flash crystallizer is adopted for sodium hydroxide recovery, waste heat generated by the previous stage is converted into kinetic energy, a stirring device is reduced, investment cost is saved, energy consumption is reduced, and meanwhile, the heat loss caused by flash crystallization cold separation is supplemented, so that the technical requirement of flash crystallization under the adiabatic condition can be ensured.
By adopting four-effect evaporation, the condensate water generated by each effect can be reasonably arranged to preheat the mother liquor, so that the waste heat is recycled.
According to the physicochemical characteristics, the evaporation adopts the advection material supplementing and cross-flow material extracting technology, the second effect extraction completion liquid of the evaporator is selected, the sodium sulfite solubility is relatively low at the temperature, the sodium hydroxide solubility is relatively high, and the heat preservation sedimentation technical condition is facilitated.
The heat preservation sedimentation (heat preservation sedimentation irrigation), pulping and suspension material selection (cyclone separator) enable several materials to be separated more effectively, the purity of the product is higher, the equipment investment is lower, the occupied area is smaller, the evaporation steam consumption is basically the same as that of the MVR evaporation, and the energy consumption is reduced.
Separation principle: the solid sodium sulfite and the sodium hydroxide high concentration solution are evaporated and separated by utilizing the principle that sodium sulfite has the maximum solubility at 33.8 ℃ and much smaller solubility relative to sodium hydroxide, and the solubility of sodium hydroxide in aqueous solution is greatly changed along with the temperature and the solubility is greater as the temperature is higher. The principle that the leuco sodium salt of vat blue RSN in the mother solution is soluble in water and the vat blue RSN is insoluble in water is utilized, and the principle that the leuco sodium salt of vat blue RSN can be automatically reduced into vat blue RSN when meeting air (oxygen) is utilized, so that the leuco sodium salt of vat blue RSN can always appear and separate out in the form of vat blue RSN in the system, the separation purpose is achieved, and the vat blue RSN refined mother solution is separated and purified step by step. In the process of extracting reaction products of sodium sulfite, vat blue RSN and sodium hydroxide, water is used as production supplementing water through evaporation and condensation, so that zero emission of production wastewater is realized; the treatment method for treating the reduction blue RSN refined mother liquor has the advantages of low energy consumption, high product yield, no intervention of interference factors, simple operation, mild production conditions, easy realization of continuous and industrialized large-scale treatment, energy conservation, high-quality resource extraction and reasonable utilization.
The invention has the beneficial effects that: separating sodium sulfite which is a reaction product, extracting reduction blue RSN carried in mother liquor, recycling excessive sodium hydroxide which is an additional production raw material, and improving the yield of the reduction blue RSN; the vapor consumption is reduced as much as possible by adopting the principle of four-effect evaporation or MVR evaporation concentration. Sodium hydroxide is extracted by adopting a flash crystallization technology, and sodium sulfite and vat blue RSN are effectively separated by adopting a pulping suspension technology. The multi-effect evaporation or MVR improves the steam utilization rate, and the energy consumption is only 30% of that of the common evaporation; by adopting the flash crystallization technology, along with the temperature reduction, the sodium sulfite is unsaturated, part of water vapor is taken away by the flash crystallization (a third-stage crystallizer is connected with a mixed condenser or a steam jet pump), the sodium sulfite is always in a saturated state, the precipitation amount of sodium hydroxide is ensured, and the water supplementing and the slurry mixing of the flash crystallization can be realized, so that the purity of a precipitated sodium hydroxide product is ensured. The separated mother liquor is returned to the evaporation system for further concentration, and the separation mother liquor is circularly reciprocated, so that the purpose of extraction and separation is achieved. The precipitated product is subjected to material conversion, heat preservation, pulping and larger particle size formation, and is more beneficial to production during separation and washing. The sodium sulfite produced by the technology is sold as a product, and the vat blue RSN can be used as a vat bleaching blue BC raw material, and can be further acidified and neutralized to be sold as a product. And the recovered sodium hydroxide is directly used as a reduction blue RSN section or a reduction bleaching blue BC production raw material after centrifugation, leaching and dehydration.
According to the invention, the reduction blue RSN entrained in the mother liquor is recovered, the yield of the reduction blue RSN is improved, excessive sodium hydroxide in a reaction system is recovered, and sodium sulfite as a byproduct is separated, so that zero emission of the mother liquor treatment is realized, and the production cost of the reduction blue RSN is reduced to a great extent.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
Fig. 1 is a schematic diagram of the present invention.
Detailed Description
The vat blue RSN refining mother liquor mainly comprises sodium sulfite, vat blue RSN leuco sodium salt, sodium hydroxide and water, and comprises the following components:
| name of the name | Sodium sulfite | Sodium hydroxide | Vat blue RSN | Water and its preparation method |
| Content of | 3.5％ | 5.5％ | 0.5％ | 90.5％ |
The above purification mother liquor treatment steps are shown in fig. 1:
step one: filtering, placing the refining mother liquor in a collecting tank, oxidizing leuco vat blue RSN sodium salt in the refining mother liquor to generate solid vat blue RSN, sending the refining mother liquor to a filter, removing the precipitated solid vat blue RSN to obtain clear refining mother liquor, and further refining the solid vat blue RSN as a crude product.
Step two: the clarified refined mother liquor is sent to a four-effect evaporator (or MVR evaporator) for multi-effect evaporation (or MVR evaporation), the sodium salt of leuco reduction blue RSN is further oxidized to form solid reduction blue RSN to be precipitated, as sodium sulfite is much less soluble at high temperature than sodium hydroxide, sodium sulfite is separated out firstly along with evaporation of water, the concentration of sodium hydroxide is higher and higher, when sodium hydroxide in a system (evaporation system) solution is close to saturation, mixed solid-liquid enters a heat preservation sedimentation tank to separate and sediment suspended sodium sulfite, and high-concentration sodium hydroxide is subjected to cold separation. The mixed solid phase enters a beating tank to completely strip sodium sulfite and solid reduction blue RSN, a cyclone separator is used for separation, and evaporated and recovered condensate water is returned to a production system for recycling.
Step three: and the sodium hydroxide solution obtained in the second step is treated by a three-stage flash crystallization device (disclosed in patent document with the authority of 201775979U) by utilizing the principle that the solubility of sodium hydroxide is reduced along with the reduction of the temperature, and the temperature is cooled from 100 ℃ to 30 ℃, so that the sodium sulfite has the maximum solubility, and the quality of the separated sodium hydroxide is higher. And filtering and leaching sodium hydroxide, returning to a production section for recycling or drying and packaging, and selling as a product.
Step four: and (3) pulping the mixed solid obtained in the step two according to the difference of water solubility, granularity and specific gravity of the solid vat blue RSN and sodium sulfite, stripping adhesion particles of different substances, separating sodium sulfite and crude solid vat blue RSN by using a suspension principle, filtering, leaching, drying and packaging the sodium sulfite to obtain a product for sale, and further refining the product after washing the vat blue RSN or preparing a vat bleaching blue BC raw material for downstream raw material. The cyclone separator is adopted for suspension separation, so that the addition of a large amount of water during separation and reduction of blue RSN is avoided, the steam consumption is increased, and the equipment investment cost and the operation cost are increased.
Step five: and (3) collecting I, II and III-effect (I, II and III-effect of the four-effect evaporator) condensed water generated by evaporation in the second step, returning the condensed water to a water system or making softened water for a production system, and cooling the IV-effect (IV-effect of the four-effect evaporator) condensed water through a mixed condenser to enter a cooling water circulation system for recycling.
The sodium hydroxide adopts a three-stage flash crystallization technology to realize the free conversion of waste heat into kinetic energy and reduce the technical conditions that flash cold separation needs to be carried out under the adiabatic condition. Step separation is adopted, and the purpose is that the purity of sodium hydroxide and sodium sulfite is improved; secondly, recovering reduction blue RSN in mother liquor; thirdly, the time from precipitation of the material to the process of forming the product is increased, so that the leuco sodium salt of vat blue RSN is converted into vat blue RSN in the first operation as much as possible. The production of the extracted vat blue is equivalent to 1.14 times of 1-amino anthraquinone, the raw material conversion and filtration are improved, the crude vat blue RSN of the production product is acidified and neutralized, and the product is dried and packaged into the product or the downstream is used as the production raw material of vat bleaching blue BC. Sodium sulfite, sodium hydroxide and reducing blue RSN washing liquid enter a mother liquor pool for cyclic reciprocating evaporation to separate reaction products sodium sulfite, raw material sodium hydroxide and product reducing blue RSN condensed water, and the sodium sulfite, the raw material sodium hydroxide and the product reducing blue RSN condensed water can be used as the water for supplementing the production process, thereby realizing zero emission and improving the product yield and reducing the production cost.
The processing method is adopted: 50 tons of wastewater is generated per 1 ton of reduction blue RSN, 1.75 tons of sodium sulfite, 2.75 tons of sodium hydroxide and 0.25 ton of reduction blue RSN are extracted, the yield can reach 98 percent, 29.5 tons of recovered condensate water is recovered, and 18.4 tons of steam is consumed. Compared with the prior art, the method for treating the vat blue RSN by evaporating, concentrating and separating the mixed solid waste by 6 tons. The steam consumption is 38 tons, and the energy consumption is saved by 51.98 percent. Zero emission of the production mother liquor is realized; the yield of vat blue RSN is improved by 18 percent. At present, the market price of 1-aminoanthraquinone in China is as follows: about 13 ten thousand yuan/ton, commercial price of industrial sodium hydroxide products: about 0.5 ten thousand yuan/ton, and sodium sulfite about 0.2 ten thousand yuan/ton.
The method is adopted to increase the output value: 1.75x2000+2.75x5000+0.25x1.14x130000+29.5x6-18.4x200= 5.077 ten thousand yuan.
At present, the average price for treating 1 ton of solid waste in China is 0.4 ten thousand yuan/ton, the wastewater discharge is 6.0 yuan/1 ton, and as dye intermediates are difficult to degrade and industrial water which is at least 5 times of the dye intermediates is added in biochemical treatment, the wastewater treatment cost for treating 1 ton of vat blue RSN by adopting the traditional process is as follows: 200×6+250×6+6×4000+38×200=3.35 ten thousand yuan.
By adopting the treatment method to treat the vat blue RSN mother liquor, sodium sulfite, vat blue RSN and sodium hydroxide can be effectively separated, condensed water is recovered, the yield of vat blue RSN is improved by 15%, and zero emission in the vat blue RSN production process is realized.
The above embodiments do not limit the present invention in any way, and all technical solutions obtained by equivalent substitution or equivalent transformation fall within the protection scope of the present invention.
Claims (2)
1. The method for treating the vat blue RSN refining mother liquor is characterized by comprising the following steps of:
(1) Filtering, introducing the refined mother liquor into a filter, removing the precipitated solid vat blue RSN to obtain clarified refined mother liquor, and further refining the solid vat blue RSN as a crude product;
(2) Evaporating and concentrating the clarified refined mother liquor, wherein the evaporating and concentrating adopts a four-effect evaporator or an MVR evaporator, the evaporating process adopts advection feed supplement and crossflow material extraction, the sodium salt of leuco vat blue RSN is further oxidized to form solid vat blue RSN to precipitate, the concentration of sodium hydroxide in the refined mother liquor is further evaporated and concentrated, when the sodium hydroxide in the system solution is nearly saturated, the mixed solid and liquid enter a heat-preserving sedimentation tank, so that suspended sodium sulfite in the system is separated out and deposited, and the high-concentration sodium hydroxide solution is sent to a cold-separation working section; the mixed solid phase is sent to a beating tank, so that sodium sulfite and solid vat blue RSN are completely stripped, separation is carried out by utilizing a suspension centrifugal separation principle, and steam is condensed and recovered;
(3) Treating the sodium hydroxide solution obtained in the step (2) by adopting a flash crystallization cold precipitation device, treating by adopting a three-stage flash crystallization cold precipitation device, cooling the temperature from 100 ℃ to 30 ℃, separating out sodium hydroxide, and filtering and leaching the sodium hydroxide to obtain the sodium hydroxide;
(4) And (3) pulping the mixed solid obtained in the step (2) according to the difference of water solubility, granularity and specific gravity of the solid vat blue RSN and sodium sulfite, stripping adhered particles of different substances, and separating the sodium sulfite and the crude solid vat blue RSN by utilizing a suspension centrifugal separation principle.
2. The method for treating vat blue RSN purification mother liquor according to claim 1, wherein: and a step of collecting condensed water produced by evaporation in the step (2).
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