CN113104865A - Method for treating refined mother liquor of vat blue RSN - Google Patents
Method for treating refined mother liquor of vat blue RSN Download PDFInfo
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- CN113104865A CN113104865A CN201911288646.3A CN201911288646A CN113104865A CN 113104865 A CN113104865 A CN 113104865A CN 201911288646 A CN201911288646 A CN 201911288646A CN 113104865 A CN113104865 A CN 113104865A
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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 refined mother liquor of vat blue RSN, which comprises the following steps: (1) introducing the refined mother liquor into a filter to remove precipitated solid reduced blue RSN; (2) evaporating and concentrating, further oxidizing to form solid reducing blue RSN to precipitate, further evaporating and concentrating, when sodium hydroxide in the solution is nearly saturated, entering a heat-preservation settling tank to separate out and deposit suspended sodium sulfite, and cooling and separating out a high-concentration sodium hydroxide solution; the mixed solid phase enters a pulping tank, so that the sodium sulfite and the solid reducing blue RSN are completely stripped; (3) treating the clear 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; the method has the advantages of recovering the vat blue RSN carried in the mother liquor, improving the yield of the vat blue RSN, recovering the excessive sodium hydroxide in the reaction system, separating the by-product sodium sulfite, realizing zero emission of the mother liquor treatment and reducing the production cost of the vat blue RSN.
Description
Technical Field
The invention relates to a method for treating vat blue RSN refined mother liquor, which is used for treating the vat blue RSN refined mother liquor.
Background
Anthraquinone vat dyes have a long history, and vat blue RSN has been discovered in 1901 for over 100 years so far, and is one of important cotton dyes for manufacturing cellulose fiber advanced products or functional products. With the rapid development of national economy, the consumption demands of people gradually tend to diversify, the requirements on the functionality, comfort and fashion of textiles are higher and higher, and more than half of the textile demands are expected to meet the requirements of medium-high grade in 2020.
The vat dye RSN is used for dyeing cellulose fibers by being reduced under the alkaline condition to color the fibers and then being oxidized to restore the original insoluble dye on the fibers for dyeing; the insoluble vat dye is made into sodium sulfate, and can be changed into soluble vat dye, which is mainly used for cotton cloth printing. The vat dye is a dye with excellent performance, bright color light, complete color spectrum, excellent dyeing effect fastness, especially high light fastness, and is an extremely important dye variety in dyeing of various textiles which require high dyeing quality at present. It can also be used as raw material for high-grade pigment, and can be used for military industry, automobile spraying, printing ink, etc.
China is a world-recognized large textile country, the demand of dye chemicals is improved along with the rapid development of the textile industry in China, 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 dyes and organic pigments in China in 2012 reaches over 100 ten thousand tons, the total import and export amount of dyes in China exceeds 40 ten thousand tons, and the output, export amount and consumption amount of dyes in China are listed as the first of all countries in the world.
The production of the vat blue RSN is generally carried out by condensation, elutriation, adding into alkaline solution, adding into sodium hydrosulfite, refining, reduction, oxidation, acidification, neutralization, washing and drying to obtain the product of the vat blue RSN.
The production reaction engineering equation is as follows:
condensation:
refining and reducing:
oxidation and acidification:
through the analysis of physicochemical properties and reaction mechanism of the vat blue RSN, the mother liquor for producing the vat blue RSN mainly comprises the following components: sodium sulfite, sodium hydroxide, a small amount of leuco vat blue RSN sodium salt and a trace amount of leuco vat blue RSN potassium salt 90% water.
The mother liquor for producing the vat blue RSN has high salt and high BOD industrial wastewater, and 50 tons of industrial washing water can be produced for each ton of production of the vat blue RSN. The waste water is firstly neutralized by acid and alkali, and then desalted by a four-effect evaporation device, the mixed salt with the solid content of more than 80 percent generated by a centrifuge is used as solid waste for further centralized treatment, and in addition, the generated sewage cold water and other waste water enter a regulating tank together to regulate the water quality and water quantity. Because the wastewater is lack of nitrogen and phosphorus, 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 is 100-500: 5: 1). The waste water in the regulating reservoir is sent into the first-level UASB by a lifting pump and automatically flows into the second-level UASB, organic matters in the waste water are absorbed and decomposed into methane, carbon dioxide, water and micromolecule substances by anaerobic microorganisms in the anaerobic reactor, the amount of the methane generated by anaerobic treatment is small, the methane has no recycling value, and the methane is discharged in the high air through a 15m high exhaust funnel. And the effluent of the anaerobic reactor enters an anaerobic sedimentation tank, and the anaerobic sludge brought out is settled and flows back to the anaerobic tower. The effluent of the anaerobic tower enters a biological contact oxidation tank, combined biological filler for the growth of microorganisms and an aerator for providing oxygen for the microorganisms are arranged in the tank, 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 tank enters a secondary sedimentation biomembrane and activated sludge which are separated off, and then the effluent reaches the standard and is discharged.
And the residual sludge of the secondary sedimentation tank and the UASB anaerobic reactor enters a sludge concentration tank for concentration, then is sent into a stacked spiral sludge dehydrator for dehydration, the filtrate returns to the regulating tank, and the obtained sludge with the water content of about 80 percent is finally treated according to common solid waste.
Because the amount of washing water is large, a large amount of the vat blue RSN enters the production wastewater, the yield of the 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 clean and pollution-free the production of the vat blue RSN dye intermediate, improving the yield of the vat blue RSN and reducing the production cost becomes a main problem for dye intermediate production enterprises. The difficulty in treating the mother liquor (wastewater) and the protection of the ecological environment directly influence the development and production scale of the blue-reducing RSN enterprises.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for treating the refining mother liquor of vat blue RSN (the method is also suitable for vat blue BC), which has the advantages of simple operation, pure physical treatment process, no addition of any additive, no residue of extracted products, low energy consumption, low cost and continuous treatment.
In order to solve the technical problem, the method for treating the refining mother liquor of vat blue RSN comprises the following steps:
(1) and (3) oxidizing the leuco vat blue RSN sodium salt in the refined mother liquor to generate solid vat blue RSN, introducing the refined mother liquor into a filter, removing the precipitated solid vat blue RSN to obtain clear refined mother liquor, and further refining the solid vat blue RSN serving as a crude product.
(2) Evaporating and concentrating the clarified refined mother liquor (for example, adopting a four-effect evaporator or MVR evaporator), further oxidizing the sodium salt of the leuco vat blue RSN to form solid vat blue RSN to precipitate, wherein the sodium sulfite has much lower solubility at high temperature relative to sodium hydroxide, and the sodium sulfite can be firstly separated out along with the evaporation of water, further evaporating and concentrating, the concentration of sodium hydroxide in the refined mother liquor is higher and higher, when the sodium hydroxide in the solution of a system (evaporation system) is close to saturation, the mixed solid-liquid enters a heat-preserving settling tank to separate out and deposit the sodium sulfite suspended in the system, and the high-concentration sodium hydroxide solution is sent to a cold-separation working section; the mixed solid phase enters a pulping tank, so that the sodium sulfite and the solid reducing blue RSN are completely stripped, and the steam is condensed and recovered by utilizing the suspension centrifugal separation principle.
(3) And (2) treating the sodium hydroxide solution obtained in the step (2) by using a flash crystallization cold separation device (for example, a three-stage flash crystallization cold separation device is adopted to meet the technical requirement of flash crystallization under an adiabatic condition, realize the spontaneous conversion of heat energy and kinetic energy and lower operation energy consumption) by utilizing the principle that the solubility of sodium hydroxide is reduced along with the reduction of the temperature, cooling the temperature from 100 ℃ to 30 ℃, and then obtaining the maximum solubility of sodium sulfite, separating the sodium hydroxide with higher quality, separating the sodium hydroxide, filtering and leaching the sodium hydroxide to obtain the sodium hydroxide, and returning the sodium hydroxide to a production section for recycling or drying and packaging the sodium hydroxide to be sold as a product.
(4) According to different water solubility, granularity and specific gravity of the solid reducing blue RSN and the sodium sulfite, pulping the mixed solid obtained in the step (2) to strip different substances from adhered particles, and separating the sodium sulfite and the crude solid reducing blue RSN by using a suspension centrifugal separation principle. Filtering, leaching, drying and packaging the sodium sulfite into a product for sale, washing the vat blue RSN, and then further refining into a product or using the product as a vat blue BC raw material to serve as a downstream raw material.
The method also comprises a step of collecting the condensed water generated by evaporation in the step (2). When the four-effect evaporator is adopted, the I-effect condensate water, the II-effect condensate water and the III-effect condensate water are returned to a water system or used as softened water for a production system, and the IV-effect condensate water is cooled by the mixing condenser and enters a cooling water circulating 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 workshop section to be used as production raw materials.
The four-effect evaporation concentration technology is adopted, the process is mature, and the steam consumption is only 0.3 ton/ton of refined mother liquor.
The sodium hydroxide recovery adopts a three-stage flash crystallizer technology, the waste heat generated by the previous stage is converted into kinetic energy, a stirring device is reduced, the investment cost is saved, the energy consumption is reduced, simultaneously, the flash cold separation lost heat is supplemented, and the technical requirement of flash crystallization under the adiabatic condition can be met.
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 can be recycled.
According to the physical and chemical characteristics, the evaporation adopts advection feed supplement and cross flow material extraction technology, the second effect extraction completion liquid of the evaporator is selected, the solubility of sodium sulfite is relatively low and the solubility of sodium hydroxide is relatively high at the temperature, and the technical conditions of heat preservation and sedimentation are facilitated.
The heat preservation and sedimentation (heat preservation and sedimentation filling), pulping and suspension material selection (cyclone separator) enable the materials to be separated more effectively, the product purity is higher, the equipment investment is lower, the occupied area is smaller, the evaporation steam consumption is basically the same as that of the selected MVR evaporation, and the energy consumption is reduced.
Separation principle: the method utilizes the characteristics that the solubility of sodium sulfite is maximum at 33.8 ℃ and is much smaller than that of sodium hydroxide, and the principle that the solubility of sodium hydroxide in an aqueous solution changes greatly with the temperature and is higher at higher temperature to evaporate and separate solid sodium sulfite and high-concentration sodium hydroxide solution. The separation aim is achieved by utilizing the principle that the leuco sodium salt of the vat blue RSN in the mother liquor is soluble in water and the vat blue RSN is insoluble in water and the principle that the leuco sodium salt of the vat blue RSN can be automatically reduced into the vat blue RSN when meeting air (oxygen), and the leuco sodium salt of the vat blue RSN always appears and is separated out in the form of the vat blue RSN when running in a system, and the refined mother liquor of the vat blue RSN is separated and purified step by step. In the process of extracting the reaction products of sodium sulfite, vat blue RSN and sodium hydroxide, water is used as production make-up water through evaporation and condensation, so that zero discharge of production wastewater is realized; the method for treating the refined mother liquor of the vat blue RSN has the advantages of low energy consumption, high product yield, no interference factor intervention of products, 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 reaction product sodium sulfite, extracting vat blue RSN carried in mother liquor, recovering excessive additional production raw material sodium hydroxide, and improving the yield of vat blue RSN; the vapor consumption is reduced as much as possible by adopting a four-effect evaporation or MVR evaporation concentration principle. The sodium hydroxide is extracted by adopting a flash crystallization technology, and the sodium sulfite and the vat blue RSN are effectively separated by adopting a pulping suspension technology. The multi-effect evaporation or MVR improves the utilization rate of the steam, and the energy consumption is only 30% of that of the common evaporation; by adopting the flash crystallization technology, the sodium sulfite is unsaturated along with the temperature reduction, the flash crystallization takes away a part of water vapor (the third-stage crystallizer is connected with a mixing condenser or a steam jet pump), the sodium sulfite is always in a saturated state, the precipitation amount of the sodium hydroxide is ensured, water can be supplemented into the flash crystallizer for size mixing, and the purity of the precipitated sodium hydroxide product is ensured. The separated mother liquor returns to the evaporation system for further concentration and is circulated to achieve the purpose of extraction and separation. The separated product is subjected to material transferring, heat preservation and pulping to form larger granularity, and is more beneficial to production during separation and washing. The sodium sulfite produced by the technology can be sold as a product, and the vat blue RSN can be used as a vat blue BC raw material, and can also be further acidified and neutralized to be sold as a product. The recovered sodium hydroxide is directly used as a raw material for producing the reducing blue RSN working section or the reducing blue BC after being centrifuged, leached and dehydrated.
The method has the advantages of recovering the vat blue RSN carried in the mother liquor, improving the yield of the vat blue RSN, recovering the excessive sodium hydroxide in the reaction system, separating the by-product sodium sulfite, realizing zero discharge of the mother liquor treatment and greatly reducing the production cost of the vat blue RSN.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
Fig. 1 is a schematic diagram of the present invention.
Detailed Description
The vat blue RSN refined mother liquor mainly comprises sodium sulfite, vat blue RSN leuco sodium salt, sodium hydroxide and water, and comprises the following components:
| name (R) | Sodium sulfite | Sodium hydroxide | Vat blue RSN | Water (W) |
| Content (wt.) | 3.5％ | 5.5％ | 0.5％ | 90.5％ |
The purification mother liquor treatment steps are shown in figure 1:
the method comprises the following steps: filtering, placing the refined mother liquor in a collecting pool, oxidizing the sodium salt of leuco vat blue RSN in the refined mother liquor to generate solid vat blue RSN, sending the refined mother liquor to a filter, removing the precipitated solid vat blue RSN to obtain clear refined 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) to carry out multi-effect evaporation (or MVR evaporation), the leuco vat blue RSN sodium salt is further oxidized to form solid vat blue RSN to be precipitated, the sodium sulfite has much lower solubility at high temperature relative to sodium hydroxide, and the sodium sulfite is firstly separated out along with the evaporation of water, the concentration of the further evaporation and concentration of the sodium hydroxide is higher and higher, when the sodium hydroxide in the solution of a system (evaporation system) is close to saturation, the mixed solid-liquid enters a heat-preserving settling tank to separate out and deposit the suspended sodium sulfite, and the high-concentration sodium hydroxide is cooled and separated out. And (3) the mixed solid phase enters a pulping tank, so that the sodium sulfite and the solid reducing blue RSN are completely stripped, a cyclone separator is adopted for separation, and the condensed water is evaporated and recovered and returned to the production system for recycling.
Step three: and (3) treating the sodium hydroxide solution obtained in the step two by using a three-stage flash crystallization device (disclosed by an authorized publication number of 201775979U) by utilizing the principle that the solubility of sodium hydroxide is reduced along with the reduction of the temperature, cooling the temperature from 100 ℃ to 30 ℃, and then, maximizing the solubility of sodium sulfite, so that the quality of the separated sodium hydroxide is higher. And filtering and leaching the sodium hydroxide, and returning the sodium hydroxide to the production section for recycling or drying and packaging the sodium hydroxide to be sold as a product.
Step four: and (3) pulping the mixed solid obtained in the step two according to different water solubility, granularity and specific gravity of the solid reducing blue RSN and the sodium sulfite to strip off different substances from adhered particles, separating the sodium sulfite and the crude solid reducing blue RSN by utilizing a suspension principle, filtering, leaching and drying the sodium sulfite to package the product for sale, washing the reducing blue RSN, and further refining the product or using the reducing blue BC as a reducing blue BC raw material to serve as a downstream raw material. And the cyclone separator is adopted for suspension separation, so that the addition of a large amount of water during the separation of the vat 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 the I, II and III effect (I, II and III effects of the four-effect evaporator) condensate water generated by evaporation in the step two, returning the condensate water to a water system or using the condensate water as softened water for a production system, and cooling the IV effect (IV effect of the four-effect evaporator) condensate water by using a mixing condenser to enter a cooling water circulation system for recycling.
The sodium hydroxide adopts a three-stage flash crystallization technology, so that the process of freely converting waste heat into kinetic energy is realized, and the technical condition that flash cold separation needs to be carried out under the adiabatic condition is reduced. The method adopts step-by-step separation, and aims to improve the purity of sodium hydroxide and sodium sulfite; secondly, recovering the vat blue RSN in the mother liquor; and thirdly, increasing the time from the precipitation of the materials to the formation of the product, so that the leuco sodium salt of the vat blue RSN is converted into vat blue RSN in the first round of operation as much as possible. The production and extraction of the reduction blue is equivalent to 1.14 times of 1-aminoanthraquinone, the conversion and filtration of raw materials are improved, the crude reduction blue RSN of the produced product is acidified and neutralized, and the product is dried and packaged into a product or is taken as a production raw material of the reduction blue BC at the downstream. Sodium sulfite, sodium hydroxide and reducing blue RSN washing liquid enter a mother liquor pool to be circularly and repeatedly evaporated so as to achieve the purposes of separating a reaction product sodium sulfite, raw material sodium hydroxide and product reducing blue RSN condensate water, using the separated reaction product sodium sulfite as production process make-up water, realizing zero discharge, improving product yield and reducing production cost.
The processing method comprises the following steps: 50 tons of wastewater is generated when every 1 ton of reduced blue RSN is produced, 1.75 tons of sodium sulfite, 2.75 tons of sodium hydroxide and 0.25 ton of reduced blue RSN are extracted, the yield can reach 98 percent, 29.5 tons of condensed water is recovered, and 18.4 tons of steam is consumed. Compared with the prior art, the method for treating the vat blue RSN has the advantages that 6 tons of mixed solid waste is evaporated, concentrated and separated from the waste water in the method for treating the vat blue RSN. 38 tons of steam are consumed, and the energy consumption is saved by 51.98%. Zero discharge of production mother liquor is realized; the yield of the reduced blue RSN is improved by 18 percent. At present, the price of the domestic 1-aminoanthraquinone market is as follows: about 13 ten thousand yuan/ton, the market selling price of industrial sodium hydroxide products: about 0.5 ten thousand yuan/ton, and 0.2 ten thousand yuan/ton of sodium sulfite.
The treatment method is adopted to increase the yield value: 1.75 × 2000+2.75 × 5000+0.25 × 1.14 × 130000+29.5 × 6-18.4 × 200 ═ 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 waste water discharge is 6.0 yuan/1 ton, and because the dye intermediate is difficult to degrade, and the biochemical treatment is to add at least 5 times of industrial water, the treatment cost for treating waste water for producing 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 mother liquor of the vat blue RSN, the sodium sulfite, the vat blue RSN and the sodium hydroxide can be effectively separated, the condensed water is recycled, the yield of the vat blue RSN is improved by 15 percent, and zero emission in the production process of the vat blue RSN is realized.
The above embodiments do not limit the present invention in any way, and all technical solutions obtained by means of equivalent substitution or equivalent transformation fall within the protection scope of the present invention.
Claims (6)
1. The method for treating the refining mother liquor of the vat blue RSN is characterized by comprising the following steps:
(1) filtering, introducing the refined mother liquor into a filter, removing the precipitated solid reducing blue RSN to obtain clarified refined mother liquor, and further refining the solid reducing blue RSN serving as a crude product;
(2) evaporating and concentrating the clarified refined mother liquor, further oxidizing the sodium salt of the leuco vat blue RSN to form solid vat blue RSN, precipitating, further evaporating and concentrating, wherein the concentration of sodium hydroxide in the refined mother liquor is higher and higher, when the sodium hydroxide in the system solution is close to saturation, the mixed solid-liquid enters a heat-preservation settling tank, so that the suspended sodium sulfite in the system is separated out and deposited, and the high-concentration sodium hydroxide solution is sent to a cold precipitation working section; sending the mixed solid phase to a pulping tank, completely stripping sodium sulfite and solid reducing blue RSN, separating by using a suspension centrifugal separation principle, and condensing and recovering steam;
(3) treating the sodium hydroxide solution obtained by the heat-insulating settling tank in the step (2) by adopting a flash crystallization cold separation device, separating out sodium hydroxide, and filtering and leaching the sodium hydroxide to obtain the sodium hydroxide;
(4) according to different water solubility, granularity and specific gravity of the solid reducing blue RSN and the sodium sulfite, pulping the mixed solid obtained in the step (2) to strip different substances from adhered particles, and separating the sodium sulfite and the crude solid reducing blue RSN by using a suspension centrifugal separation principle.
2. The method for treating a mother liquor for purification of vat blue RSN as claimed in claim 1, wherein: and (3) collecting the condensed water generated by evaporation in the step (2).
3. The method for treating a mother liquor for purification of vat blue RSN as claimed in claim 1, wherein: the evaporation concentration adopts a four-effect evaporator or an MVR evaporator.
4. The method for treating a mother liquor for purification of vat blue RSN as claimed in claim 1, wherein: treating with flash crystallization cold separation device, and cooling from 100 deg.C to 30 deg.C.
5. The method for treating a mother liquor for purification of vat blue RSN as claimed in claim 1, wherein: the evaporation process adopts advection feed supplement and cross flow material extraction.
6. The method for treating a mother liquor for purification of vat blue RSN as claimed in claim 1, wherein: a three-stage flash crystallization cold separation device is adopted.
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