CN114314929A - Comprehensive treatment method for printing and dyeing wastewater of reactive dye - Google Patents
Comprehensive treatment method for printing and dyeing wastewater of reactive dye Download PDFInfo
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- CN114314929A CN114314929A CN202210005397.8A CN202210005397A CN114314929A CN 114314929 A CN114314929 A CN 114314929A CN 202210005397 A CN202210005397 A CN 202210005397A CN 114314929 A CN114314929 A CN 114314929A
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- 239000002351 wastewater Substances 0.000 title claims abstract description 43
- 238000004043 dyeing Methods 0.000 title claims abstract description 33
- 239000000985 reactive dye Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 85
- 238000005406 washing Methods 0.000 claims abstract description 36
- 239000012452 mother liquor Substances 0.000 claims abstract description 31
- 239000002699 waste material Substances 0.000 claims abstract description 31
- KXZJHVJKXJLBKO-UHFFFAOYSA-N chembl1408157 Chemical compound N=1C2=CC=CC=C2C(C(=O)O)=CC=1C1=CC=C(O)C=C1 KXZJHVJKXJLBKO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000001914 filtration Methods 0.000 claims abstract description 25
- 239000000975 dye Substances 0.000 claims abstract description 20
- 239000012065 filter cake Substances 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000011780 sodium chloride Substances 0.000 claims abstract description 14
- 239000012528 membrane Substances 0.000 claims abstract description 12
- 239000000986 disperse dye Substances 0.000 claims abstract description 11
- 238000001471 micro-filtration Methods 0.000 claims abstract description 4
- 238000001728 nano-filtration Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 20
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 16
- DOBRDRYODQBAMW-UHFFFAOYSA-N copper(i) cyanide Chemical compound [Cu+].N#[C-] DOBRDRYODQBAMW-UHFFFAOYSA-N 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 8
- 235000010288 sodium nitrite Nutrition 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 5
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 5
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 5
- 229940045803 cuprous chloride Drugs 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 239000012267 brine Substances 0.000 claims description 3
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical group [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 claims description 3
- 239000012466 permeate Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000004042 decolorization Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000007599 discharging Methods 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- UIEBGVDTKLYGTN-UHFFFAOYSA-J tetrasodium;7-[[2-(carbamoylamino)-4-[[4-chloro-6-[3-(2-sulfonatooxyethylsulfonyl)anilino]-1,3,5-triazin-2-yl]amino]phenyl]diazenyl]naphthalene-1,3,6-trisulfonate Chemical compound [Na+].[Na+].[Na+].[Na+].C=1C=C(N=NC=2C(=CC3=CC(=CC(=C3C=2)S([O-])(=O)=O)S([O-])(=O)=O)S([O-])(=O)=O)C(NC(=O)N)=CC=1NC(N=1)=NC(Cl)=NC=1NC1=CC=CC(S(=O)(=O)CCOS([O-])(=O)=O)=C1 UIEBGVDTKLYGTN-UHFFFAOYSA-J 0.000 description 1
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Abstract
The invention discloses a comprehensive treatment method of printing and dyeing wastewater of reactive dyes, belonging to the field of printing and dyeing wastewater, and the comprehensive treatment method of printing and dyeing wastewater of reactive dyes comprises the following steps: separating the mother liquor into 0.5-2% waste saline A with molecular weight less than 80 and waste dye B with molecular weight more than 80 by using a nanofiltration membrane; separating the waste saline A into waste saline G with the concentration of 18-20% and waste saline H with the concentration of 0.2-1% by using a microfiltration membrane, and discharging or using the waste saline H as dyeing water after biochemical treatment; the waste dye water B is hydrolyzed reactive dye with the concentration of 15-20%; and (3) reacting the separated reactive dye B with sodium cyanide to synthesize a disperse dye which is insoluble in water, filtering after the reaction is finished, and washing with water and hot water to obtain a filter cake, mother liquor water D and washing water, wherein the filter cake is the disperse dye C. The method realizes the reduction of the dye content in the wastewater from the printing and dyeing production of the reactive dye, leads the wastewater to reach the discharge standard, and greatly reduces the pollution to the water environment.
Description
Technical Field
The invention relates to the field of printing and dyeing wastewater, in particular to a comprehensive treatment method of reactive dye printing and dyeing wastewater.
Background
The dyeing yield of the reactive dye is 65-85%, 15-35% is in the waste water, so the dye exists in the waste water, the concentration of the dye is 0.5-1%, and the concentration of the salt is 0.5-2%. At present, the yield of reactive dyes in the world is 50 ten thousand tons, the yield of Chinese reactive dyes is 25 ten thousand tons, the domestic use amount in China is 20 ten thousand tons, and the concentration of waste dyes in wastewater is 2 ten thousand tons.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a comprehensive treatment method of reactive dye printing and dyeing wastewater, which can recycle the dye in the reactive dye printing and dyeing production wastewater, so that the dye can reach the dischargeable standard, and the pollution to the water environment is greatly reduced.
In order to solve the above problems, the present invention adopts the following technical solutions.
A comprehensive treatment method of reactive dye printing and dyeing wastewater comprises the following steps:
(1) separating the mother liquor into waste brine A with the molecular weight less than 80 and waste dye water B with the molecular weight more than 80 by using a nanofiltration membrane; the waste dye water B is hydrolyzed reactive dye with the concentration of 15-20%; separating the waste saline A into waste saline G with the concentration of 18-20% and waste saline H with the concentration of 0.2-1% by using a microfiltration membrane; the waste water salt H is discharged after biochemical treatment or used as dyeing water;
(2) reacting the waste dye water B in the step (1) with excessive sodium cyanide to synthesize a disperse dye which is insoluble in water, filtering after the reaction reaches the end point, washing with hot water for 1-N times, and reusing washing water for 2-N times to obtain washing water for the (N + 1) th time, and simultaneously obtaining a filter cake, mother liquor water D and first washing water M, wherein the filter cake is the disperse dye C.
(3) And (3) adding cuprous chloride into the mother liquor water D and the first washing water M in the step (2) to react with redundant sodium cyanide to synthesize cuprous cyanide which is insoluble in water, and then filtering, wherein the filter cake is cuprous cyanide, and the mother liquor water E contains trace cuprous cyanide and sodium cyanide solution.
(4) And (4) adding a sodium sulfide solution into the mother liquor water E obtained in the step (3) to react to remove cuprous cyanide, filtering, wherein a filter cake is cuprous sulfide, and a filtrate is mother liquor water F.
(5) And (4) adding sodium nitrite into the mother liquor F in the step (4) to remove sodium cyanide.
(6) And (3) mixing the waste water salt G with the concentration of 18-20% in the step (1) with the mother liquor water F treated by the sodium nitrite in the step (5), and adding sodium hypochlorite to completely remove the sodium cyanide.
(7) And (4) adding activated carbon into the treated solution obtained in the step (6) for decolorization, filtering, and spraying the filtrate to dry to obtain the industrial salt.
Further, the reaction product, namely the water-insoluble disperse dye, is spotted on the filter paper in the step (2), no solution permeates out, and the reaction is ended when the water ring is colorless.
Further, when the waste dye water B reacts with sodium cyanide in the step (2), the pH is controlled to be 9.5-11, the temperature is controlled to be 70-100 ℃, and the reaction time is 1-4 hours.
Further, in the step (3), the pH value is controlled to be 8.5-10, the temperature is controlled to be 30-70 ℃, the reaction time is 1-4 hours in the cuprous chloride adding process, and sodium cyanide with the concentration of more than 98% is removed through filtration.
Further, in the step (4), the pH value is controlled to be 9.0-11, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours in the process of adding the sodium sulfide solution, and more than 99% of cuprous cyanide in the sodium sulfide solution is removed by filtering.
Further, in the step (5), the pH is controlled to be 9.0-12 in the process of adding the sodium nitrite solution, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours, and the filtration is carried out, wherein the sodium cyanide in the filtrate is less than 400 PPM.
Further, in the step (6), the pH value is controlled to be 8.0-10 in the process of adding the sodium hypochlorite solution, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours, and the filtration is carried out, wherein the sodium cyanide in the filtrate is less than 6 PPM.
Further, in the step (7), the pH is controlled to be 7.5-10, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours in the process of adding the active carbon, and the mixture is filtered and then sprayed to be dry.
Further, the specific steps are (1) separating the mother liquor into waste brine A with the molecular weight less than 80 and waste dye water B with the molecular weight more than 80 by using a nanofiltration membrane; the waste dye water B is hydrolyzed reactive dye with the concentration of 15-20%; separating the waste saline A into waste saline G with the concentration of 18-20% and waste saline H with the concentration of 0.2-1% by using a microfiltration membrane; the waste water salt H is discharged after biochemical treatment or used as dyeing water;
(2) reacting the waste dye water B in the step (1) with excessive sodium cyanide at the pH value of 9.5-11 and the temperature of 70-100 ℃ for 3 hours to synthesize a water-insoluble disperse dye, taking a reaction product, namely the water-insoluble disperse dye to be spotted on filter paper, enabling no solution to permeate out, reacting to the end point when a water ring is colorless, filtering after the reaction to the end point, washing with hot water for 1-N times, and reusing washing water for 2-N times to obtain washing water for the (N + 1) th time, and simultaneously obtaining a filter cake, mother liquor water D and first washing water M, wherein the filter cake is disperse dye C;
(3) and (3) adding cuprous chloride into the mother liquor water D and the first washing water M in the step (2) to react with redundant sodium cyanide at the temperature of 30-70 ℃ for 1-4 hours at the pH of 8.5-10 to synthesize cuprous cyanide which is insoluble in water, and then filtering to obtain cuprous cyanide filter cake, wherein the mother liquor water E contains cuprous cyanide and sodium cyanide solution.
(4) And (4) adding a sodium sulfide solution into the mother liquor water E in the step (3) to react for 1-3 hours at the pH of 9.0-11 and the temperature of 20-50 ℃, removing cuprous cyanide through reaction, filtering, wherein a filter cake is cuprous sulfide, and a filtrate is mother liquor water F.
(5) And (4) reacting the mother liquor F and sodium nitrite in the step (4) at the pH of 9.0-12 and the temperature of 20-50 ℃ for 1-3 hours to remove sodium cyanide in the mother liquor.
(6) Mixing the waste water salt G with the concentration of 18-20% in the step (1) with the mother liquor water F treated by the sodium nitrite in the step (5), adding sodium hypochlorite, and reacting for 1-3 hours at the temperature of 20-50 ℃ and the pH of 8.0-10 to completely remove the sodium cyanide.
(7) Adding activated carbon into the treated solution obtained in the step (6), controlling the pH value to be 7.5-10, the temperature to be 20-50 ℃, reacting for 1-3 hours, filtering after decoloring, and spraying the filtrate to dry to obtain the industrial salt.
Compared with the prior art, the invention has the advantages that:
the scheme can reduce the dye content in the reactive dye production wastewater, so that the reactive dye production wastewater can reach the dischargeable standard that sodium cyanide is less than 6PPM, and the pollution to the water environment is greatly reduced.
Drawings
FIG. 1 is a schematic diagram of the comprehensive treatment method of reactive dye printing and dyeing wastewater of the invention.
Detailed Description
Example 1:
cyanidation reaction equation after separation and concentration of reactive yellow 145 printing and dyeing wastewater:
concentrating 0.275 ‰ 1000L 145 yellow printing and dyeing wastewater to 19% 145 yellow printing and dyeing wastewater 1450ML by membrane treatment, adding 200ML into 500ML three-neck flask, adjusting pH to 10-11, adding 7 g sodium cyanide at 25-40 deg.C, heating to 65-70 deg.C, controlling pH 10-11 to react for 2 hours, heating to 95-100 deg.C, controlling pH 10-11 to react until the material is insoluble in water (the slurry is on the filter paper, and the water ring has no color), filtering after the reaction is finished, washing the filter cake with 1000 g 80-90 deg.C water for 5 times, mixing the first washing water into the mother liquor, separately washing the other washing times, and finally washing with new 200 g 80-90 deg.C water.
Example 2:
the cyanidation reaction equation after separation and concentration of 195 red dyeing wastewater is as follows:
0.15 per thousand 1000L of 195 red printing wastewater is concentrated to 15 percent of 195 red printing wastewater 1000ML through membrane treatment, 200ML is taken out and added into a 500ML three-neck flask, the pH value is adjusted to 10-11, 12 grams of sodium cyanide is added at 25-40 ℃, then the temperature is raised to 65-70 ℃, the pH value is controlled to 10-11 for reaction for 2 hours, then the temperature is raised to 95-100 ℃, the pH value is controlled to 10-11 for reaction until the material is insoluble in water (the slurry is dotted on filter paper, and no color exists in a water ring), the filtration is carried out after the reaction is finished, a filter cake is uniformly divided into 5 times by 1000 grams of 80-90 ℃ water for washing, the washing water for the first time is mixed into mother liquor, the other washing for the next time is separately carried out, and finally the washing is carried out by using new 200 grams of 80-90 ℃ water for washing for the last time.
Example 3:
the cyanidation reaction equation after separation and concentration of blue 222 printing and dyeing wastewater is as follows:
concentrating the 222 blue printing wastewater of 0.175 per thousand 1000L to 17.5 percent of 1000ML by membrane treatment, adding 200ML into a 500ML three-neck flask, adjusting the pH value to 10-11, adding 15 grams of sodium cyanide at 25-40 ℃, heating to 65-70 ℃, controlling the pH value to 10-11, reacting for 2 hours, heating to 95-100 ℃, controlling the pH value to 10-11, reacting until the material is insoluble in water (the slurry is dotted on a filter paper, and the water ring has no color), filtering after the reaction is finished, uniformly dividing the filter cake into 5 times by using 1000 grams of 80-90 ℃ water, mixing the first washing water into the mother liquor, separately washing the other times when washing the next time, and finally washing the last time by using new 200 grams of 80-90 ℃ water.
Example 4:
the cyaniding reaction equation after separation and concentration of the black WNN printing and dyeing wastewater is as follows:
concentrating 0.275 ‰ 1000L black WNN printing and dyeing wastewater to 19% black WNN printing and dyeing wastewater 1450ML by membrane treatment, adding 200ML into 500ML three-neck flask, adjusting pH to 10-11, adding 7 g sodium cyanide at 25-40 deg.C, heating to 65-70 deg.C, controlling pH 10-11 to react for 2 hours, heating to 95-100 deg.C, controlling pH 10-11 to react until the material is insoluble in water (the slurry is dotted on the filter paper, and the water ring has no color), filtering after the reaction is finished, washing the filter cake with 1000 g 80-90 deg.C water for 5 times, mixing the first washing water into the mother liquor, separately washing the other washing times, and finally washing with new 200 g 80-90 deg.C water.
Claims (8)
1. A comprehensive treatment method of reactive dye printing and dyeing wastewater is characterized by comprising the following steps: the method comprises the following steps:
(1) separating the mother liquor into waste brine A with the molecular weight less than 80 and waste dye water B with the molecular weight more than 80 by using a nanofiltration membrane; the waste dye water B is hydrolyzed reactive dye with the concentration of 15-20%; separating the waste saline A into waste saline G with the concentration of 18-20% and waste saline H with the concentration of 0.2-1% by using a microfiltration membrane; the waste water salt H is discharged after biochemical treatment or used as dyeing water;
(2) reacting the waste dye water B in the step (1) with excessive sodium cyanide to synthesize a disperse dye which is insoluble in water, filtering after the reaction reaches the end point, washing with hot water for 1-N times, and reusing washing water for 2-N times to obtain washing water for the (N + 1) th time, and simultaneously obtaining a filter cake, mother liquor water D and first washing water M, wherein the filter cake is the disperse dye C;
(3) adding cuprous chloride into the mother liquor water D and the first washing water M in the step (2) to react with redundant sodium cyanide to synthesize cuprous cyanide which is insoluble in water, and then filtering, wherein the filter cake is cuprous cyanide, and the mother liquor water E contains cuprous cyanide and sodium cyanide solution;
(4) adding a sodium sulfide solution into the mother liquor water E obtained in the step (3) to react to remove cuprous cyanide, filtering, wherein a filter cake is cuprous sulfide, and a filtrate is mother liquor water F;
(5) removing sodium cyanide from the mother liquor F and sodium nitrite in the step (4);
(6) mixing the waste water salt G with the concentration of 18-20% in the step (1) with the mother liquor water F treated by the sodium nitrite in the step (5), and adding sodium hypochlorite to completely remove the sodium cyanide;
(7) and (4) adding activated carbon into the treated solution obtained in the step (6) for decolorization, filtering, and spraying the filtrate to dry to obtain the industrial salt.
2. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: and (3) taking a reaction product, namely water-insoluble disperse dyes, in the step (2), spotting the reaction product on filter paper, wherein no solution permeates out, and the reaction product is reacted to the end point when a water ring is colorless.
3. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: and (3) when the waste dye water B reacts with sodium cyanide in the step (2), controlling the pH to be 9.5-11, controlling the temperature to be 70-100 ℃, and controlling the reaction time to be 1-4 hours.
4. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: in the step (3), the pH is controlled to be 8.5-10, the temperature is controlled to be 30-70 ℃, the reaction time is 1-4 hours in the cuprous chloride adding process, and filtering is carried out.
5. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: in the step (4), the pH is controlled to be 9.0-11 in the process of adding the sodium sulfide solution, the temperature is 20-50 ℃, the reaction time is 1-3 hours, and the filtration is carried out.
6. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: in the step (5), the pH is controlled to be 9.0-12, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours in the process of adding the sodium nitrite solution, and the filtration is carried out.
7. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: in the step (6), the pH value is controlled to be 8.0-10, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours in the process of adding the sodium hypochlorite solution, and the filtration is carried out.
8. The comprehensive treatment method of reactive dye printing and dyeing wastewater according to claim 1, characterized in that: in the step (7), the pH is controlled to be 7.5-10, the temperature is controlled to be 20-50 ℃, the reaction time is 1-3 hours, and the mixture is filtered and then sprayed to dry.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115583750A (en) * | 2022-10-10 | 2023-01-10 | 浙江亿得新材料股份有限公司 | Brine treatment method |
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| US20100219082A1 (en) * | 2006-06-21 | 2010-09-02 | Juan Jorge Diaz Gonzalez Alcocer | Method and integral system for treating water for cooling towers and processess requiring removal of silica from the water |
| CN112851523A (en) * | 2021-01-22 | 2021-05-28 | 浙江亿得新材料股份有限公司 | Method for synthesizing 2, 4-dinitro-6-bromoaniline from bromamine acid product wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100219082A1 (en) * | 2006-06-21 | 2010-09-02 | Juan Jorge Diaz Gonzalez Alcocer | Method and integral system for treating water for cooling towers and processess requiring removal of silica from the water |
| CN112851523A (en) * | 2021-01-22 | 2021-05-28 | 浙江亿得新材料股份有限公司 | Method for synthesizing 2, 4-dinitro-6-bromoaniline from bromamine acid product wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115583750A (en) * | 2022-10-10 | 2023-01-10 | 浙江亿得新材料股份有限公司 | Brine treatment method |
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Application publication date: 20220412 |