CN113529442A - Method for recycling inorganic salt in dyeing of reactive dye - Google Patents
Method for recycling inorganic salt in dyeing of reactive dye Download PDFInfo
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- CN113529442A CN113529442A CN202110904185.9A CN202110904185A CN113529442A CN 113529442 A CN113529442 A CN 113529442A CN 202110904185 A CN202110904185 A CN 202110904185A CN 113529442 A CN113529442 A CN 113529442A
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- inorganic salt
- reactive dye
- salt
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- 238000004043 dyeing Methods 0.000 title claims abstract description 114
- 229910017053 inorganic salt Inorganic materials 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000000985 reactive dye Substances 0.000 title claims abstract description 45
- 238000004064 recycling Methods 0.000 title claims abstract description 35
- 239000002351 wastewater Substances 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 19
- 238000001914 filtration Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000003957 anion exchange resin Substances 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 10
- 238000005189 flocculation Methods 0.000 claims abstract description 9
- 230000016615 flocculation Effects 0.000 claims abstract description 9
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 8
- 239000008394 flocculating agent Substances 0.000 claims abstract description 5
- 239000000975 dye Substances 0.000 claims description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 238000001179 sorption measurement Methods 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 6
- 229920000289 Polyquaternium Polymers 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims 1
- 238000004042 decolorization Methods 0.000 abstract description 12
- 230000008901 benefit Effects 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000004744 fabric Substances 0.000 description 12
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 description 10
- 235000011152 sodium sulphate Nutrition 0.000 description 10
- 239000012267 brine Substances 0.000 description 9
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 229920000742 Cotton Polymers 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 238000001556 precipitation Methods 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 5
- 230000001376 precipitating effect Effects 0.000 description 5
- 239000011780 sodium chloride Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 150000003863 ammonium salts Chemical group 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005349 anion exchange Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002306 biochemical method Methods 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/673—Inorganic compounds
- D06P1/67333—Salts or hydroxides
- D06P1/6735—Salts or hydroxides of alkaline or alkaline-earth metals with anions different from those provided for in D06P1/67341
- D06P1/67358—Halides or oxyhalides
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
- C02F2001/422—Treatment of water, waste water, or sewage by ion-exchange using anionic exchangers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a method for recycling inorganic salt in reactive dye dyeing, which comprises the steps of adjusting the pH value of reactive dye dyeing residual liquid containing inorganic salt, adding a flocculating agent for flocculation, and filtering to obtain supernatant; adding anion exchange resin into the supernatant, stirring, and filtering to obtain colorless salt-containing wastewater; detecting the concentration of inorganic salt in the colorless salt-containing wastewater, adjusting the concentration of the inorganic salt in the colorless salt-containing wastewater to meet the subsequent dyeing requirement, and using the adjusted colorless salt-containing wastewater for dyeing and processing the cellulose fiber product; repeating the steps to realize the recycling of the inorganic salt for dyeing the reactive dye; the method is simple and convenient to operate, has no special requirement on equipment, can realize high-efficiency decolorization treatment on the dyeing residual liquid of the reactive dye, enables the inorganic salt added in the dyeing link to be recycled in subsequent dyeing process, greatly reduces the discharge amount of the inorganic salt to the environment in the dyeing process of the reactive dye, has a certain water-saving advantage, and has very outstanding environmental protection advantages.
Description
Technical Field
The invention belongs to the field of post-treatment of dyeing wastewater, and particularly belongs to a method for recycling inorganic salt of reactive dye.
Background
In the dyeing process of the reactive dye, a large amount of inorganic salt (sodium sulfate or sodium chloride) is needed to be used for accelerating dyeing, a fixation alkaline agent is needed to be used for accelerating the bonding reaction of the dye and fibers, and the discharged wastewater after dyeing contains not only the undyed dye and hydrolyzed dye, but also a large amount of salt and alkali. Generally, the treatment of dyeing wastewater mainly aims at waste dyes and organic auxiliary agents added in the dyeing process, and reduces the chromaticity, COD value, BOD and other pollution indexes of the wastewater through flocculation precipitation and biochemical methods, so as to reach the wastewater discharge index and discharge the wastewater into the environment. Inorganic salt can not be effectively removed in the treatment of dyeing wastewater, and the inorganic salt and the alkaline agent used in the dyeing link are finally discharged to the environment in the form of inorganic salt. The discharge of the waste water with high salt content can cause the salinization of fresh water and the salinization of land, and has the problem of environmental pollution. Therefore, the inorganic salt is recycled in the reactive dye dyeing, the emission of the inorganic salt in the dyeing process to the environment is reduced, the aim of clean dyeing process is fulfilled, and the method has important environmental protection significance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for recycling inorganic salt in reactive dye dyeing, which is used for removing the reactive dye in dyeing residual liquid to obtain colorless reuse water containing high-concentration inorganic salt, and the reuse water is used as a dyeing medium for subsequent dyeing processing of cellulose fiber products to realize recycling of the inorganic salt in reactive dye dyeing.
In order to achieve the purpose, the invention provides the following technical scheme: a method for recycling inorganic salt dyed by reactive dye comprises the following steps:
s1, adjusting the pH value of the dyeing residual liquid of the reactive dye containing inorganic salt, adding a flocculating agent for flocculation, and filtering to obtain a supernatant;
s2, adding anion exchange resin into the supernatant, stirring, and filtering to obtain colorless salt-containing wastewater;
s3, detecting the concentration of inorganic salt in the colorless salt-containing wastewater, adjusting the concentration of inorganic salt in the colorless salt-containing wastewater to meet the subsequent dyeing requirement, and using the adjusted colorless salt-containing wastewater for dyeing cellulose fiber products;
s4 repeating the steps S1-S2 to realize the recycling of the inorganic salt for dyeing the reactive dye.
Further, in step S1, the concentration of the inorganic salt in the dyeing raffinate of the reactive dye containing the inorganic salt is more than or equal to 20 g/L.
Further, in step S1, an acid solution is used to adjust the pH of the reactive dye dyeing residual liquid containing inorganic salts to 6.5-7.5.
Further, in step S1, the acid solution is sulfuric acid or hydrochloric acid.
Further, in step S1, the flocculant is a polymeric flocculant of a polyquaternium, and the molecular weight range is 500 to 200000.
Further, in step S1, adding a flocculating agent, stirring for 20-60 min, standing and precipitating for 2-4 h; the flocculant is generally added in an amount of:
dosage of the flocculant is X g/L
The dye concentration in the dyeing residual liquid is Y g/L
The effective content of the flocculant is 40%, X is Y (0.7-1.2) is 1, and the dye concentration Y is calculated according to the dye absorbance and a standard curve.
Further, in step S2, the anion exchange resin is a weakly basic macroporous adsorption resin.
Further, in step S2, the dosage of the anion exchange resin is 16-40 g/L, and the adsorption time is 1.5-2 h.
Further, in step S3, the concentration of inorganic salt in the wastewater containing colorless salt is detected by a drying and weighing method.
Further, in step S3, the dyeing process is a conventional dyeing process of cellulose fiber reactive dyes.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a method for recycling inorganic salt in reactive dye dyeing, which can realize high-efficiency decoloration treatment on residual liquid in reactive dye dyeing, so that the inorganic salt in the residual liquid can be recycled in subsequent dyeing processing, the consumption of the inorganic salt in the reactive dye dyeing processing can be greatly reduced, the water consumption in the dyeing process can be saved, and the method has the advantages of resource saving, emission reduction and environmental protection; the method provided by the invention is simple and convenient to operate, has low requirements on equipment and has strong practicability.
Detailed Description
The present invention will be further described with reference to specific embodiments, which are provided for illustration only and are not intended to limit the scope of the present invention. Various changes and modifications can be made by one skilled in the art without departing from the spirit and scope of the invention, and equivalents thereof fall within the scope of the invention as defined by the appended claims.
The invention provides a method for recycling inorganic salt in dyeing of reactive dye, which comprises the following steps:
(1) collecting the dyeing residual liquid of the reactive dye containing inorganic salt in a container, adding acid to neutralize the color-fixing alkaline agent added during dyeing, and adjusting the pH value to 6.5-7.5;
(2) adding a flocculating agent, stirring for 20-60 min, standing and precipitating for 2-4 h;
(3) filtering and separating supernatant liquor, adding anion exchange resin, stirring for 1.5-2 h, and filtering and separating to obtain colorless salt-containing wastewater;
(4) testing the salt concentration in the colorless salt-containing wastewater;
(5) according to the requirement of the subsequent dyeing procedure, the concentration of inorganic salt in the colorless salt-containing wastewater reaches the subsequent dyeing requirement by adding a small amount of salt or adding water for dilution, so that the inorganic salt is reused for dyeing processing of the cellulose fiber product;
(6) and (5) repeating the steps (1) to (5).
Preferably, the inorganic salt in the step (1) is sodium sulfate or sodium chloride, and the concentration is more than or equal to 20 g/L.
Preferably, the acid in step (1) is sulfuric acid or hydrochloric acid.
Preferably, the fixing alkaline agent in step (1) is sodium hydroxide, sodium carbonate, sodium silicate or any combination of the three.
Preferably, the flocculant in the step (2) is a polyquaternary ammonium salt polymeric flocculant, and the molecular weight range is 500-200000.
Preferably, the flocculant is added in the step (2) in an amount of:
dosage of the flocculant is X g/L
The dye concentration in the dyeing residual liquid is Y g/L
The effective content of the flocculant is 40%, X: Y is 0.7-1.2: 1, and the dye concentration Y is calculated according to the dye absorbance and a standard curve.
Preferably, the anion exchange resin in step (3) is a weakly basic macroporous adsorption resin.
Preferably, the dosage of the anion exchange resin in the step (3) is generally 16-40 g/L.
Preferably, the test in step (4) is a drying-weighing method, in which 10ml of the treated wastewater is taken in a petri dish, and the change m in mass of the petri dish before and after drying is weighed, thereby calculating the concentration of the inorganic salt.
Preferably, the dyeing process in step (5) is a conventional dyeing process for cellulose fiber reactive dyes.
According to the method, most of the dye in the dyeing residual liquid is subjected to flocculation and precipitation in a mode that a cationic group in the flocculant and an active dye anion are subjected to electrostatic combination, but the amount of the flocculant which is put into the dyeing residual liquid is far less than that of the dye, the content of the flocculant in the obtained clear liquid is very little after precipitation and filtration, and the subsequent dyeing of the recycled brine is hardly influenced; then, adsorbing a small amount of residual dye in the filtered clear liquid by using anion exchange between the weakly basic macroporous adsorption resin and the dye to obtain colorless salt-containing water; the recovered aqueous inorganic salt solution can be used directly in the dyeing process. Through the repeated operation from the step (1) to the step (5), the cyclic utilization of high-concentration inorganic salt in the reactive dye dyeing residual liquid can be realized, the direct discharge of high-concentration salt-containing wastewater is avoided, and the method has obvious environmental protection benefits.
Example 1
Measuring the absorbance of 1L of reactive red 3BS dyeing residual liquid to obtain the concentration Yg/L of dye (the dye is 5.0% (owf) during dyeing, the concentration of sodium sulfate is 70g/L, and the mixed alkali of sodium carbonate and sodium hydroxide is 2.5g/L), adding sulfuric acid into the reactive red 3BS dyeing residual liquid to neutralize until the pH value of the dyeing residual liquid is 6.5-7.5, then adding 1.5g of polyquaternary ammonium salt polymeric flocculant (molecular weight is 500-1000), stirring for 30min, standing and precipitating for 3h, wherein X: Y is 1.2: 1. And filtering and separating supernatant liquor, adding 16g of alkalescent macroporous adsorption resin, stirring and adsorbing for 2 hours, and filtering to obtain a colorless inorganic salt water solution. The saline water is reused for dyeing pure cotton knitted fabrics, 10g of the fabrics, 5 percent (owf) of active red 3BS dye is used, the bath ratio is 10:1, through detection, the decolorization rate of a flocculation precipitation stage is 97.89 percent, the decolorization rate of a resin adsorption stage is 95.19 percent, the comprehensive decolorization rate is 99.89 percent, the concentration of inorganic sodium salt in the obtained saline wastewater is 69.6g/L, 0.4g of sodium sulfate needs to be added during reuse dyeing, an X-Rite Color i7 Color measuring Color matching instrument is adopted to compare and test the Color accuracy of a dyed product, and the rubbing Color fastness test and the soaping Color fastness test are carried out, and the results are shown in Table 1.
TABLE 1 dyeing effect of reactive Red 3BS dye for inorganic salt recycling
According to the data in the table 1, the color and the color fastness index of the pure cotton knitted fabric dyed by the reuse water dyeing are consistent with those of the new water dyed sample.
Example 2
Measuring the absorbance of 1L of reactive yellow 3RS dyeing wastewater to obtain the concentration Yg/L of dye (the dye is 5.0% (owf) in dyeing working hours, the concentration of sodium sulfate is 70g/L, and the mixed alkali of sodium silicate and sodium hydroxide is 2.0g/L), adding sulfuric acid into the reactive yellow 3RS dyeing wastewater to neutralize the pH value to be 6.5-7.5, then adding 0.5g of polyquaternary ammonium salt polymer flocculant (molecular weight is 30000-50000), stirring for 20min, standing and precipitating for 2h, wherein X: Y is 0.7: 1. Separating supernatant, adding 24.0g alkalescent macroporous adsorbent resin, stirring for 2 hr, and filtering to obtain colorless inorganic salt water solution. The salt-containing wastewater is reused for dyeing pure cotton knitted fabrics, 10g of the fabrics, 5% (owf) of active yellow 3RS dye, 10:1 of bath ratio, 95.11% of decolorization rate in a flocculation precipitation stage, 94.29% of decolorization rate in a resin adsorption stage and 99.72% of comprehensive decolorization rate through detection, the concentration of sodium sulfate in the obtained salt-containing wastewater is 69.2g/L, 0.8g of sodium sulfate needs to be added during reuse dyeing, an X-Rite Color i7 Color matching instrument is adopted for contrast test of Color accuracy of a dyed product, and a friction Color fastness test and a soaping Color fastness test are carried out, and the results are shown in Table 2.
TABLE 2 dyeing effect of reactive yellow 3RS dye for inorganic salt recycling
According to the data in the table 2, the color and the color fastness index of the pure cotton knitted fabric dyed by the reuse water dyeing are consistent with those of the new water dyeing.
Example 3
Measuring the absorbance of 1L of active black WNN dyeing wastewater to obtain the concentration Yg/L of dye (5.0% (owf) of the dye added in the dyeing process, 70g/L of sodium sulfate, and 2.0g/L of mixed alkali of sodium carbonate, sodium silicate and sodium hydroxide), adding sulfuric acid to neutralize the dye to obtain the pH value of 6.5-7.5, then adding 0.8g of polyquaternary ammonium salt polymer flocculant (with the molecular weight of 100000-200000), stirring for 60min, standing and precipitating for 4h, wherein X: Y is 1: 1. Separating supernatant, adding 40g of weakly alkaline macroporous adsorption resin, stirring for 2h, and filtering to obtain colorless inorganic salt water solution. The salt-containing wastewater is reused for dyeing pure cotton knitted fabrics, 10g of the fabrics, 5 percent (owf) of active black WNN dye and 10:1 of bath ratio are detected, the decolorization rate of a flocculation precipitation stage is 88.89 percent, the decolorization rate of a resin adsorption stage is 97.85 percent, the comprehensive decolorization rate is 99.76 percent, the concentration of sodium sulfate in the obtained salt-containing wastewater is 68.9g/L, 1.1g of sodium sulfate needs to be added during reuse dyeing, an X-Rite Color i7 Color matching instrument is adopted to compare and test the Color accuracy of a dyed product, and the friction Color fastness test and the soaping Color fastness test are carried out, and the results are shown in Table 3.
TABLE 3 dyeing effect of reactive black W/NN dye inorganic salt recycling
According to the data in the table 3, the color and the color fastness index of the pure cotton knitted fabric dyed by the reuse water dyeing are consistent with those of the new water dyeing.
Example 4
Dyeing pure cotton knitted fabrics by using reactive red 3BS dye, wherein 5g of the fabric, 6.0% (owf) of the reactive red 3BS dye, 70g/L of anhydrous sodium sulfate, 60 ℃ of color fixing temperature and 60min of color fixing time are adopted, dyeing residual liquid is collected, the steps (1) to (5) are repeated, brine is reused in reactive dye dyeing processing for many times, the recycling of inorganic salt is carried out, the change of the recycling times of the brine and the content of the inorganic salt is shown in a table 4, the influence of the recycling times of the brine on dyeing quality is shown in a table 5, and the reduction of the recycling times of the brine and the emission of the inorganic salt is shown in a table 6.
TABLE 4 salt water reuse times and inorganic salt contents thereof
As can be seen from Table 4, the purification treatment effect of the dyeing raffinate of the reactive red 3BS dye with different recycling times is relatively stable, the flocculation decolorization rate is kept about 97%, the resin decolorization rate is more than 93%, and the chroma of recycled water is reduced to less than 10 times. On the other hand, in the whole dyeing processing and water treatment and purification process, the loss of inorganic salt is basically little, and the retention rate of the inorganic salt in the recycled water can reach more than 95%.
TABLE 5 relationship between saline water reuse times and dyeing effect
As can be seen from the comparison of the recycling dyeing effects in the table 5, under the condition of proper dyeing conditions, the K/S value of the dyed product is not obviously reduced when the wastewater containing high-concentration inorganic salt is recycled for dyeing processing for multiple times, and the color difference between the recycled water and the new water dyed product is relatively small. In addition, after multiple rounds of recycling dyeing and treatment processes, the reactive dye fabric obtained by the recycling water dyeing also has relatively good friction color fastness and soaping color fastness.
TABLE 6 relationship between reuse frequency of brine and reduction of inorganic salt discharge
| Number of times of reuse (times) | 1 | 2 | 3 | 4 |
| Saving ratio of inorganic salt (%) | 44.74 | 59.31 | 66.57 | 70.79 |
As can be seen from Table 6, since the waste dyes in the dyeing raffinate are mainly removed in the process of purifying the dyeing raffinate by the polyquaternium flocculant and the anionic resin, the inorganic salts added during dyeing can be largely retained. Therefore, the salt saving rate is gradually increased along with the increase of the recycling times of the inorganic salt in the reactive dye dyeing process, and the addition amount of the inorganic salt in the dyeing process can be reduced by 70.79% after the inorganic salt is recycled for 4 times, so that the discharge amount of the inorganic salt is greatly reduced.
The invention is adopted to carry out decoloration treatment on the dyeing residual liquid of the reactive dye to obtain purified brine, and the purified brine is reused for dyeing, and the result shows that the dyeing effect of the recycled brine and the dyeing effect of new water are basically consistent, the recycling of inorganic salt for dyeing is realized, the discharge of inorganic salt for dyeing processing can be obviously reduced, and the invention has obvious environmental protection benefit.
Claims (10)
1. A method for recycling inorganic salt dyed by reactive dye is characterized by comprising the following steps:
s1, adjusting the pH value of the dyeing residual liquid of the reactive dye containing inorganic salt, adding a flocculating agent for flocculation, and filtering to obtain a supernatant;
s2, adding anion exchange resin into the supernatant, stirring, and filtering to obtain colorless salt-containing wastewater;
s3, detecting the concentration of inorganic salt in the colorless salt-containing wastewater, adjusting the concentration of inorganic salt in the colorless salt-containing wastewater to meet the subsequent dyeing requirement, and using the adjusted colorless salt-containing wastewater for dyeing cellulose fiber products;
s4 repeating the steps S1-S2 to realize the recycling of the inorganic salt for dyeing the reactive dye.
2. The method for recycling inorganic salt in reactive dye dyeing according to claim 1, wherein in step S1, the concentration of inorganic salt in the dyeing raffinate of reactive dye containing inorganic salt is not less than 20 g/L.
3. The method for recycling inorganic salt in reactive dye dyeing according to claim 1, wherein in step S1, the pH value of the residual liquid of reactive dye dyeing containing inorganic salt is adjusted to 6.5-7.5 by using acid solution.
4. The method for recycling inorganic salts dyed by reactive dyes according to claim 3, wherein in step S1, the acid solution is sulfuric acid or hydrochloric acid.
5. The method for recycling inorganic salt dyed by reactive dye according to claim 1, wherein in step S1, the flocculant is a polymeric flocculant of polyquaternium type, and the molecular weight range is 500-200000.
6. The method for recycling inorganic salt in dyeing of reactive dye according to claim 1, wherein in step S1, the flocculant is added and stirred for 20-60 min, and then the mixture is left to stand for 2-4 h; the flocculant is generally added in an amount of:
dosage of the flocculant is X g/L
The dye concentration in the dyeing residual liquid is Y g/L
The effective content of the flocculant is 40%, and X is (0.7-1.2) and Y is (1).
7. The method for recycling inorganic salt dyed by reactive dye according to claim 1, wherein in step S2, the anion exchange resin is weakly basic macroporous adsorption resin.
8. The method for recycling inorganic salt dyed by reactive dye according to claim 1, wherein in step S2, the dosage of the anion exchange resin is 16 g/L-40 g/L, and the adsorption time is 1.5 h-2 h.
9. The method for recycling inorganic salt dyed by reactive dye according to claim 1, wherein in step S3, the concentration of inorganic salt in the wastewater containing colorless salt is detected by drying and weighing method.
10. The method for recycling inorganic salt in reactive dye dyeing according to claim 1, wherein in step S3, the dyeing process is a conventional dyeing process of reactive dye for cellulose fiber.
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| CN116102207A (en) * | 2023-02-13 | 2023-05-12 | 广东溢达纺织有限公司 | Method for simultaneously recycling dyed brine and softened regenerated brine |
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