CN113105396A - Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor - Google Patents
Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor Download PDFInfo
- Publication number
- CN113105396A CN113105396A CN201911278203.6A CN201911278203A CN113105396A CN 113105396 A CN113105396 A CN 113105396A CN 201911278203 A CN201911278203 A CN 201911278203A CN 113105396 A CN113105396 A CN 113105396A
- Authority
- CN
- China
- Prior art keywords
- evaporator
- section
- dimethyl sulfoxide
- potassium hydroxide
- vat blue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000012452 mother liquor Substances 0.000 title claims abstract description 28
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 239000007791 liquid phase Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 230000000694 effects Effects 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 238000006482 condensation reaction Methods 0.000 claims description 5
- 239000003595 mist Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 2
- KHUFHLFHOQVFGB-UHFFFAOYSA-N 1-aminoanthracene-9,10-dione Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2N KHUFHLFHOQVFGB-UHFFFAOYSA-N 0.000 abstract description 17
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 abstract description 5
- 239000000975 dye Substances 0.000 description 19
- 238000004519 manufacturing process Methods 0.000 description 19
- 238000000926 separation method Methods 0.000 description 18
- 239000007788 liquid Substances 0.000 description 17
- 238000009833 condensation Methods 0.000 description 13
- 230000005494 condensation Effects 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- 239000000047 product Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 9
- 230000009467 reduction Effects 0.000 description 9
- 238000004821 distillation Methods 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000004753 textile Substances 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 238000004043 dyeing Methods 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000984 vat dye Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000002910 solid waste Substances 0.000 description 4
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 235000019253 formic acid Nutrition 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000011265 semifinished product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 229920003043 Cellulose fiber Polymers 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 235000011837 pasties Nutrition 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
- 239000008274 jelly Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920005567 polycyclic polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- JFPIMJJOZHDWRG-UHFFFAOYSA-M potassium;methylsulfinylmethane;hydroxide Chemical compound [OH-].[K+].CS(C)=O JFPIMJJOZHDWRG-UHFFFAOYSA-M 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D241/00—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings
- C07D241/36—Heterocyclic compounds containing 1,4-diazine or hydrogenated 1,4-diazine rings condensed with carbocyclic rings or ring systems
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for treating dye vat blue RSN dimethyl sulfoxide mother liquor, which comprises the following steps: (1) evaporating and concentrating dye vat blue RSN dimethyl sulfoxide mother liquor by adopting a first section of an evaporator, separating out potassium hydroxide, filtering and separating, and allowing a liquid phase to enter a second section of the evaporator for continuous concentration; (2) returning the potassium hydroxide separated out from the second section of the evaporator to the first section of the evaporator; (3) when the temperature of the second section of the evaporator is constant to 80 ℃, the vacuum degree is 0.094Mpa, the liquid phase in which the water is completely removed is transferred to a clarifying tank connected with the second section of the evaporator, the temperature of the clarifying tank is raised to 85 ℃, the heat is preserved, and a tail gas pipe of the clarifying tank is connected to a vacuum pipe of the second section of the evaporator; (4) recovering the first section of condensed water of the evaporator; (5) obtaining dimethyl sulfoxide from a clarifying tank; the method can effectively separate potassium hydroxide, the leuco potassium salt of the vat blue RSN, the unreacted 1-aminoanthraquinone, the half-finished product of the vat blue RSN and dimethyl sulfoxide which are not completely reacted, and recover condensed water.
Description
Technical Field
The invention relates to a treatment method of dye vat blue RSN dimethyl sulfoxide mother liquor (the treatment of NN-dimethyl amide aqueous solution is also applicable), which is used for treating the dye vat blue RSN dimethyl sulfoxide 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 that 1-aminoanthraquinone is dissolved in dimethyl sulfoxide as an organic solvent, potassium hydroxide is used as a catalyst, oxidation condensation is carried out, and water is added according to the solubility for segregation. The separated product is washed and then enters a refining reduction working section.
The production reaction engineering equation is as follows:
condensation:
through the analysis of physicochemical properties and reaction mechanism of the reducing blue RSN, the main components of the separating liquid in the condensation section of the reducing blue RSN are as follows: potassium hydroxide, dimethyl sulfoxide, a small amount of leuco vat blue RSN leuco potassium salt, 1-aminoanthraquinone which does not participate in reaction and 1-aminoanthraquinone condensate which does not participate in reaction, under a certain condition, the 1-aminoanthraquinone which does not participate in reaction can complete condensation, the incomplete half product can complete condensation, and finally the vat blue RSN product is formed, but when the temperature is too high, polycyclic polymers can be formed to become production waste, so that raw materials are wasted, the product yield is reduced, and solid waste or pasty liquid waste can be generated to pollute the environment.
The separation liquid for producing the water separation by the reduction blue RSN contains high potassium hydroxide and dimethyl sulfoxide, and 16 tons of separation liquid for producing the water separation can be produced when one ton of the reduction blue RSN is produced. The production water separation liquid is firstly added into formic acid, stirred and neutralized, the neutralized mother liquid is added into a distillation still through a pump, the temperature is raised to 150 ℃ for distillation, the distilled gas enters a rectifying tower, the distilled residual liquid enters a residual liquid distillation still through vacuum pumping, the temperature is raised to 180 ℃ for secondary distillation, the distilled gas enters the rectifying tower, the distilled residual liquid is treated as solid waste, 0.57 ton of residue and 0.18 ton of jelly are generated when 1 ton of vat blue RSN is produced.
Distilled gas generated by distillation at the temperature of below 100 ℃ enters a rectifying tower to be condensed into liquid, and the liquid enters a dehydration collecting tank and is reused in a material turning kettle; distilling condensed liquid generated by distilling at 100-150 ℃ enters a receiving tank, and the condensed liquid needs to return to a mother liquor tank for redistilling because the condensed liquid contains moisture; distilling at 150 deg.C or higher to condense into liquid, and feeding into a receiving tank for feeding dimethyl sulfoxide into the condensation kettle. And waste gas generated in the distillation section is collected, sprayed and absorbed and then discharged after reaching the standard.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a treatment method of dye vat blue RSN dimethyl sulfoxide mother liquor (the treatment of the NN-dimethyl amide aqueous solution is also applicable), the operation is simple, the treatment process is purely physical, no additive is added, the operation is carried out at low temperature, no residue is left in extraction and separation materials, the energy consumption is low, the cost is low, and the continuous treatment and the automatic operation can be realized.
In order to solve the technical problem, the method for treating the dye vat blue RSN dimethyl sulfoxide mother liquor comprises the following steps:
(1) concentrating dye vat blue RSN dimethyl sulfoxide mother liquor by adopting a first section of an evaporator (sending the dye vat blue RSN dimethyl sulfoxide mother liquor to the first section of the evaporator after being preheated by adopting a preheater), separating out potassium hydroxide, filtering and separating a separated potassium hydroxide mixture (comprising potassium hydroxide, vat blue RSN leuco sylvite, 1-aminoanthraquinone which does not participate in reaction and a half-product 1-aminoanthraquinone condensate which does not complete reaction), and feeding a separated liquid phase into a second section of the evaporator for continuous concentration; the first section of the evaporator has more than 1 effect, and the second section of the evaporator has 1 effect. The evaporation and dehydration of the evaporator adopt concurrent feeding, advection feeding and cross flow material lifting. Two sections of potassium hydroxide are selected for separation, so that the viscosity of the material is reduced, the separation is facilitated, and the evaporation effect is better.
(2) And (3) returning the potassium hydroxide mixture separated out from the second section of the evaporator to the first section of the evaporator, and continuously separating the potassium hydroxide mixture by adopting the process of the step (1).
(3) When the water in the second section of the evaporator is completely removed, the dimethyl sulfoxide in the second section of the evaporator returns to the condensation reaction tank for recycling; when the temperature of the second section of the evaporator is constant to 80 ℃, the vacuum degree is 0.094Mpa, which indicates that the water in the second section of the evaporator is completely removed.
(4) And recovering the condensed water in the first section of the evaporator.
(5) And (3) sending the potassium hydroxide mixture subjected to filtration separation to a potassium hydroxide solution preparation tank for reuse, dissolving potassium hydroxide by using recovered condensed water, and sending the prepared potassium hydroxide mixed solution to a condensation reaction tank.
The second section of the evaporator is provided with a mist catcher, so that the loss caused by the volatilization of the dimethyl sulfoxide is reduced as much as possible.
The invention does not add any additive to the mother liquor treatment, and the obtained product can be returned to the production section to be used as a production raw material.
The multi-effect two-stage evaporation concentration technology is adopted, the process is mature, and the steam consumption is only 0.41 ton/ton of mother liquor.
The low-temperature evaporation dehydration recovery technology is adopted, so that the chemical reaction generated due to overhigh temperature in the evaporation dehydration process is avoided, the physical properties of the raw materials are not changed, the utilization rate of the raw materials is improved, and the energy consumption is reduced.
By adopting multi-effect two-stage evaporation, the condensate water generated in 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, evaporation adopts the technologies of forward flow feeding, advection feeding and cross flow material extraction, a first section is selected to separate potassium hydroxide, the material viscosity is reduced, a second section is used for extracting dehydrated dimethyl sulfoxide, and a mist catcher is arranged at the second section of the evaporator, so that the loss caused by volatilization of the dimethyl sulfoxide is reduced.
Separation principle:
firstly, the dimethyl sulfoxide and water can be mixed according to any ratio, and the dehydration is carried out in the distillation process without the azeotropic point principle.
Secondly, according to the principle that the potassium hydroxide can be dissolved in water but not in dimethyl sulfoxide, the potassium hydroxide is separated out along with the evaporation of water.
And thirdly, separating the potassium hydroxide at about 100 ℃ according to the fact that the viscosity of the dimethyl sulfoxide is reduced along with the rise of the temperature, and reducing the entrainment of the dimethyl sulfoxide as much as possible.
Fourthly, the dehydration process is realized according to the good thermal stability of the dimethyl sulfoxide in the alkaline environment.
And fifthly, dehydrating the 1-aminoanthraquinone and the condensed semi-finished product at the temperature of 120 ℃ in a way that the condensation direction is basically stable (the condensation is carried out to obtain the reduced blue RSN), and no unidentified condensate or polymer is generated.
And sixthly, increasing the mist catching device according to the condition that the boiling point of the dimethyl sulfoxide is higher than that of water under the same pressure environment, reducing the volatilization amount of the dimethyl sulfoxide and reducing the loss of the dimethyl sulfoxide. The treatment process has mild and stable conditions, and the water is evaporated and condensed to be used as production make-up water, so that zero discharge of the production wastewater is realized; the treatment method for treating the separation liquid generated in the production 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, automatic and industrialized large-scale treatment and energy conservation.
The invention has the beneficial effects;
preheating, dehydrating, separating and recovering liquid-phase production raw materials and auxiliary production raw materials, and improving the yield of the reduced blue RSN; and multiple-effect two-stage evaporation dehydration is adopted, so that the steam consumption is reduced as much as possible. The heating temperature is reduced, and high-temperature polymerization and solvent decomposition in the solvent recovery process are prevented or avoided. The multi-effect two-stage evaporation improves the utilization rate of steam, and the energy consumption is only below 50 percent of that of the common evaporation; the mother liquor is directly concentrated, so that the increase of the treatment cost caused by the addition of an additive is avoided; secondly, the loss of raw materials in a liquid phase is avoided; and thirdly, avoiding the instability of the raw materials caused by the change of the system environment. So that the weight and the quality of the liquid phase system are relatively stable after the separation. Dimethyl sulfoxide can be mixed with water in any ratio, and the mixed solution can be regarded as an ideal solution, which provides a favorable technical basis for separation, and in an alkaline environment, the dimethyl sulfoxide has good stability, thereby avoiding increasing a tail gas recovery device used for decomposing waste gas recovery and reducing equipment investment; the low-temperature operation is selected mainly in consideration of uncertain condensation and high-temperature polymer generation, and waste residue is avoided. The potassium hydroxide separated by the technology contains dimethyl sulfoxide, part of unreacted 1-aminoanthraquinone and condensation semi-finished products are sent into a potassium hydroxide preparation tank, condensed water is added to prepare a 50% potassium hydroxide solution, and a solid phase and a liquid phase enter the condensation tank together and enter the next production cycle to participate in the reaction again; the concentration of the extracted dimethyl sulfoxide can reach 97 percent, the requirement of a production solvent is basically met, if the concentration is higher, the separated 97 percent of dimethyl sulfoxide can be heated to 120 ℃, flash dehydration is carried out, flash gas condensation enters a system for recycling, and more than 98 percent of dimethyl sulfoxide can be used as a high-quality organic solvent. The condensed water contains a small amount of dimethyl sulfoxide, and can be directly used as potassium hydroxide dissolving water and water separation supplementing water without separation and refining. The dimethyl sulfoxide loss is mainly end-effect volatilization, the dimethyl sulfoxide enters a circulating water system through steam, the rest is completely recovered, classified and enters the system step by step according to production and feeding for recycling, no residue and no discharge are generated during solvent recovery, and zero emission is realized.
By adopting the method, potassium hydroxide, leuco sylvite of the vat blue RSN, 1-aminoanthraquinone which does not complete reaction, semifinished product of the vat blue RSN which does not complete reaction and dimethyl sulfoxide can be effectively separated, condensed water is recovered, the condensed water is used as a potassium hydroxide preparation solution dissolving agent and water separation make-up water, no waste is generated in the whole process, the utilization rate of reaction raw materials for producing the vat blue RSN is improved, the yield of the vat blue RSN is indirectly improved, and no waste residue or waste liquid is generated in a condensation working section 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 dye vat blue RSN dimethyl sulfoxide mother liquor comprises the following components:
| name (R) | Potassium hydroxide | Dimethyl sulfoxide | Leuco potassium salt of vat blue RSN | Water (W) |
| Content (wt.) | 4.15％ | 20.25％ | 1.37％ | 74.23％ |
The processing method is as shown in figure 1:
(1) evaporating and concentrating dye vat blue RSN dimethyl sulfoxide mother liquor by adopting a first section of an evaporator, precipitating potassium hydroxide, filtering and separating a precipitated potassium hydroxide mixture, and allowing a separated liquid phase to enter a second section of the evaporator for continuous concentration; the first stage of the evaporator is 3 effects (the mother liquor treatment capacity is 100 tons per day), and the second stage of the evaporator is 1 effect.
(2) And (3) returning the potassium hydroxide mixture separated out from the second section of the evaporator to the first section of the evaporator, and continuously separating the potassium hydroxide mixture by adopting the process of the step (1).
(3) When the temperature of the second section of the evaporator is constant to 80 ℃, the vacuum degree is 0.094Mpa, which shows that the water in the liquid phase is completely removed and the liquid phase is transferred to the second section of the evaporator. The second section of the evaporator is provided with a mist trap to reduce the loss and environmental pollution caused by the volatilization of dimethyl sulfoxide.
(4) And recovering the first section of condensed water of the evaporator.
(5) And (3) sending the potassium hydroxide mixture subjected to filtration separation to a potassium hydroxide solution preparation tank for reuse, dissolving potassium hydroxide by using recovered condensed water, and sending the prepared potassium hydroxide mixed solution to a condensation reaction tank.
The weight of potassium hydroxide required by the condensation reaction of the reduction blue RSN is 0.6 time of that of 1-aminoanthraquinone, the weight of dimethyl sulfoxide is 2.6 times of that of 1-aminoanthraquinone, the weight of water is 10 times of that of 1-aminoanthraquinone, the leuco potassium salt of the reduction blue RSN carried in the mother liquor is 0.21 times of that of 1-aminoanthraquinone, and by adopting the treatment method, the reduction of 1 ton of reduction blue RSN is equivalent to the reduction of 0.225 ton of 1-aminoanthraquinone raw material relative to the reduction of 0.18 time of 1-aminoanthraquinone raw material. The process has obvious economic benefit for enterprises.
The method comprises the following steps: and (3) extracting 0.664 ton of potassium hydroxide, 2.91 ton of dimethyl sulfoxide and 0.22 ton of leuco potassium salt of the reduced blue RSN when 16 tons of wastewater is generated every 1 ton of the reduced blue RSN, wherein the yield can reach 98%, 5.94 tons of condensed water is recovered, and 7.13 tons of steam is consumed. Compared with the prior art that the waste water is evaporated, concentrated and separated to mix 0.57 ton of solid waste, 0.18 ton of pasty waste, 11.88 ton of condensed water is recovered, 2.80 ton of dimethyl sulfoxide is recovered, 32.19 ton of steam is consumed, and 0.51 ton of formic acid is consumed in the method for treating the reduced blue RSN dimethyl sulfoxide mother liquor, the method saves the energy consumption by 77.85%. All components in the reducing blue RSN dimethyl sulfoxide mother liquor are completely recovered, so that the zero discharge of the solvent of the reducing blue RSN dimethyl sulfoxide mother liquor is realized; the yield of the reduced blue RSN is improved by 18 percent. At present, the market price of domestic 1-aminoanthraquinone is about 13 ten thousand yuan/ton, the market price of industrial-grade potassium hydroxide products is about 0.65 ten thousand yuan/ton, and the market price of dimethyl sulfoxide is 1.25 ten thousand yuan/ton. Formic acid 0.35 ten thousand yuan/ton, steam 0.02 ten thousand yuan/ton. The method is adopted to recover and produce 1 ton of vat blue RSN organic solvent to increase the output value: 0.664 × 0.65+2.91 × 1.25+0.22 × 13+5.94 × 6 ÷ 10000-7.13 × 0.02 ═ 6.79 ten thousand yuan.
At present, the average price for treating 1 ton of solid waste in China is 0.4 ten thousand yuan/ton, and the recovery and production of 1 ton of vat blue RSN water separation liquid reduces the production cost (increases the output value): 2.80 × 1.25+11.88 × 6 ÷ 10000- (0.57 × 0.4+0.18 × 0.2+32.19 × 0.02+0.51 × 0.35) ═ 2.42 ten thousand yuan.
The cost of one year is different according to the calculation of producing 500 tons of vat blue RSN one year: 2184.25 ten thousand yuan, and has obvious economic benefit for enterprises.
If the production scale is large, the solvent recovery amount is large, and (3+1) four-effect two-stage evaporation or (2+1) three-effect two-stage evaporation dehydration can be adopted.
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 (5)
1. The method for treating the dye vat blue RSN dimethyl sulfoxide mother liquor is characterized by comprising the following steps of:
(1) evaporating and concentrating dye vat blue RSN dimethyl sulfoxide mother liquor by adopting a first section of an evaporator, precipitating potassium hydroxide, filtering and separating a precipitated potassium hydroxide mixture, and allowing a separated liquid phase to enter a second section of the evaporator for continuous concentration;
(2) returning the potassium hydroxide mixture separated out from the second section of the evaporator to the first section of the evaporator;
(3) when the water in the second section of the evaporator is completely removed, the dimethyl sulfoxide in the second section of the evaporator returns to the condensation reaction tank for recycling;
(4) recovering the condensed water in the first section of the evaporator;
(5) the potassium hydroxide mixture separated by filtration is sent to a potassium hydroxide solution preparation tank for reuse.
2. The method for treating dye vat blue RSN dimethyl sulfoxide mother liquor as claimed in claim 1, wherein: the first section of the evaporator has more than 1 effect, and the second section of the evaporator has 1 effect.
3. The method for treating dye vat blue RSN dimethyl sulfoxide mother liquor as claimed in claim 1, wherein: the temperature of the second section of the evaporator is 80 ℃, and the vacuum degree is 0.094 Mpa.
4. The method for treating dye vat blue RSN dimethyl sulfoxide mother liquor as claimed in claim 1, wherein: the evaporation and dehydration of the evaporator adopt concurrent feeding, advection feeding and cross flow material lifting.
5. The method for treating dye vat blue RSN dimethyl sulfoxide mother liquor as claimed in claim 1, wherein: the second section of the evaporator is provided with a mist catcher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911278203.6A CN113105396A (en) | 2019-12-12 | 2019-12-12 | Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911278203.6A CN113105396A (en) | 2019-12-12 | 2019-12-12 | Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113105396A true CN113105396A (en) | 2021-07-13 |
Family
ID=76708527
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911278203.6A Pending CN113105396A (en) | 2019-12-12 | 2019-12-12 | Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113105396A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3358036A (en) * | 1964-03-12 | 1967-12-12 | Merck & Co Inc | Purification of dimethyl sulfoxide |
| CN104230769A (en) * | 2013-06-19 | 2014-12-24 | 吴嘉隆 | Method for obtaining dimethyl sulfoxide from recovered solvent in p-xylene bicyclic body production |
| CN104341797A (en) * | 2014-11-05 | 2015-02-11 | 上海华元实业总公司 | After-treatment clean process for purifying vat blue 66 dye |
-
2019
- 2019-12-12 CN CN201911278203.6A patent/CN113105396A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3358036A (en) * | 1964-03-12 | 1967-12-12 | Merck & Co Inc | Purification of dimethyl sulfoxide |
| CN104230769A (en) * | 2013-06-19 | 2014-12-24 | 吴嘉隆 | Method for obtaining dimethyl sulfoxide from recovered solvent in p-xylene bicyclic body production |
| CN104341797A (en) * | 2014-11-05 | 2015-02-11 | 上海华元实业总公司 | After-treatment clean process for purifying vat blue 66 dye |
Non-Patent Citations (1)
| Title |
|---|
| 燃料化学工业部物资供应管理局: "《燃料化学工业设备参考资料手册 化工建设项目成套设备 下》", 燃料化学工业部物资供应管理局, pages: 1403 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109851595B (en) | Process for producing furfural from bagasse | |
| CN104817481A (en) | Technological method for recovering DMSO from DMSO aqueous solution | |
| CN107628930A (en) | A kind of heat pump separation of extractive distillation methanol, the energy saving technique of isopropyl alcohol and water | |
| CN106831315B (en) | Continuous production method of chloroethane | |
| CN112142618B (en) | Low-concentration dimethylformamide wastewater recovery system and method | |
| CN105693560A (en) | Method for preparing energy-efficient H-acid | |
| CN109503424B (en) | Production equipment and method of N-cyanoethyl-N-benzyl aniline | |
| CN101182390B (en) | Method for preparing disperse red 60 | |
| CN108774110B (en) | Continuous recycling process for desalting waste liquid of BDO device produced by Rebo method after steaming | |
| CN113105396A (en) | Method for treating dye vat blue RSN dimethyl sulfoxide mother liquor | |
| CN103979577B (en) | A kind of coking desulfurization mixed salt extracts the method for sodium sulfocyanate | |
| CN106831537B (en) | Process for synthesizing permanent violet RL intermediate condensate | |
| CN111821821A (en) | Fusel oil recycling device and method in methanol production | |
| CN110004194B (en) | Method for producing xylose and furfural by utilizing bagasse enzymolysis | |
| CN214781576U (en) | Caprolactam rearrangement heat energy cyclic utilization device | |
| CN104529837A (en) | Clean production process of 1,4-diaminoanthraquinone-2-sulfonic acid | |
| CN113372572B (en) | Method for separating lignin by recycling solid organic acid | |
| CN113104865B (en) | Treatment method of vat blue RSN refining mother liquor | |
| CN109721035B (en) | Purification and concentration process of waste dilute sulfuric acid | |
| CN109942377B (en) | Process for recycling mother liquor wastewater in naphthol production | |
| CN102627551A (en) | Method for isomerizing rosin resin acid promoted by solid super acid | |
| CN105566171A (en) | Device for preparing H-acid | |
| CN1370770A (en) | Pyridine recovering process | |
| CN104671304A (en) | Comprehensive utilization method for gas-phase latent heat at top of rectifying tower | |
| CN111333084B (en) | Method for recycling caustic alkali in sulfonated alkali fusion process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20220126 Address after: 735200 No. 9, Xingfu Road, building materials chemical industry zone, East Town, Yumen City, Jiuquan City, Gansu Province Applicant after: Jiuquan Yupeng Chemical Technology Co.,Ltd. Address before: 215500 administration department, 6th floor, international clothing city, 77 Shangcheng Middle Road, Changshu City, Suzhou City, Jiangsu Province Applicant before: Lin Qikun |
|
| TA01 | Transfer of patent application right | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210713 |
|
| WD01 | Invention patent application deemed withdrawn after publication |