CN114604901A - Method for treating waste acid generated in dye sulfonation - Google Patents
Method for treating waste acid generated in dye sulfonation Download PDFInfo
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- CN114604901A CN114604901A CN202210273953.XA CN202210273953A CN114604901A CN 114604901 A CN114604901 A CN 114604901A CN 202210273953 A CN202210273953 A CN 202210273953A CN 114604901 A CN114604901 A CN 114604901A
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- waste acid
- dye
- sulfonation
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- acid
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- 239000002699 waste material Substances 0.000 title claims abstract description 62
- 239000002253 acid Substances 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000006277 sulfonation reaction Methods 0.000 title claims description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000001179 sorption measurement Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- 238000003795 desorption Methods 0.000 claims description 10
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 8
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 8
- 235000011151 potassium sulphates Nutrition 0.000 claims description 8
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- 229920005989 resin Polymers 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 2
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 2
- 235000010344 sodium nitrate Nutrition 0.000 claims description 2
- 239000004317 sodium nitrate Substances 0.000 claims description 2
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 238000004090 dissolution Methods 0.000 claims 1
- 238000006116 polymerization reaction Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 11
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- 238000011084 recovery Methods 0.000 description 3
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000986 disperse dye Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910001414 potassium ion Inorganic materials 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000001055 blue pigment Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 239000008394 flocculating agent Substances 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 239000000985 reactive dye Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/009—Compounds containing iron, with or without oxygen or hydrogen, and containing two or more other elements
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
A process for reclaiming the waste sulfonated dye acid includes such steps as pretreating, removing impurities, adsorbing, concentrating, cooling and crystallizing, and acid dissolving and polymerizing reaction of red mud in the presence of oxidant to obtain the resultant water treating agent. The method solves the problems of large amount of accumulated red mud and potential pollution risk, realizes the reduction of the red mud, and realizes the resource utilization of the dye sulfonated waste acid.
Description
Technical Field
The invention relates to the technical field of waste acid treatment, in particular to a treatment method of dye sulfonated waste acid.
Background
China is a large sulphuric acid consumption country and relates to various industries such as titanium dioxide, dye, petroleum processing, steel pickling, aromatic hydrocarbon nitration and the like. With the continuous increase of the consumption of sulfuric acid, the production amount of domestic industrial waste sulfuric acid is increased year by year, and the recycling of the waste sulfuric acid gradually receives wide attention. The dye industry is one of the acid households in China, and sulfuric acid or fuming sulfuric acid is used in the production process of various dyes such as reactive dyes, disperse dyes and the like and intermediates thereof, but is finally transferred into dye waste water, such as sulfonated waste acid, phthalocyanine blue pigment waste acid, disperse dye waste acid and the like.
The waste sulfonated dye acid has low concentration and complex components, is rich in organic substances and salt substances, only a few large-scale enterprises adopt a concentration process to recover sulfuric acid, and most of the enterprises adopt a lime neutralization method to treat, so that the waste sulfonated dye acid cannot be effectively recovered and reused. In recent years, the treatment method and comprehensive utilization of the sulfonated waste acid have attracted much attention and have been studied to some extent, mainly including treatment of waste with waste, recovery and reuse of acid, and specific methods include a roasting method, an evaporation method, a membrane treatment method, an ion exchange method, a chemical conversion method, and the like.
The red mud is polluting waste residue discharged when aluminum oxide is extracted in the aluminum industry, and generally 1.0-2.0 tons of red mud are additionally generated when 1 ton of aluminum oxide is produced on average. China, as the 4 th alumina producing country in the world, discharges up to millions of tons of red mud every year. A large amount of red mud cannot be fully and effectively utilized, and can only be stacked by a large-area yard, thereby occupying a large amount of land and causing serious pollution to the environment. At present, the cement is fired by using the red mud, which is an effective way for recycling the waste slag, but the limited utilization rate still cannot relieve the heavy burden of the red mud on the society and the environment relative to the huge discharge amount of the red mud.
Disclosure of Invention
The invention aims to provide a method for treating dye sulfonated waste acid and a method for preparing a polymeric aluminum ferric sulfate flocculating agent by reusing the dye sulfonated waste acid.
The technical scheme adopted by the invention comprises the following steps:
step one, pretreatment: carrying out pretreatment impurity removal on the sulfonated waste acid to remove mechanical impurities and residual solid suspended matters in the sulfonated waste acid;
step two, adsorption: the pretreated waste acid enters an adsorption system, a special material is used for adsorbing COD in the feed liquid, meanwhile, the water chroma is reduced, the flow rate is controlled to be 1-2 BV/h, and the adsorbed waste acid solution is collected;
step three, desorption: after the adsorption resin is used, methanol desorption liquid is adopted for desorption, and the desorption liquid is repeatedly applied to an adsorption system;
step four, concentration: concentrating the waste acid solution generated in the step two after adsorption by adopting double-effect evaporation;
step five, cooling: cooling the concentrated waste acid, and removing sulfate substances in the waste acid by a crystallization method;
step six, centrifugal separation: conveying the cooled materials to a centrifugal machine by a pump for solid-liquid separation, and returning salt substances to the dye production process for reuse;
step seven, recycling waste acid: and reacting the centrifuged waste acid with red mud, preparing polymeric aluminum ferric sulfate under the action of an oxidant, and filtering the reaction to obtain reddish brown liquid, namely the product.
In the first step, the concentration of sulfuric acid in the waste acid is 25% -35%, the COD content is 10000-20000 mg/L, and the salt substance is mainly potassium sulfate, and the content of the salt substance is 5% -15%.
In the first step, the pretreatment and impurity removal are completed by adopting a security filter.
In the second step, the adopted special material is COD special resin.
In the third step, the content of the methanol in the methanol desorption solution is 60 to 100 percent.
In the fourth step, the sulfuric acid content in the concentrated waste acid is 35-50%.
In the seventh step, the solid-to-liquid ratio of the waste acid to the red mud is 2: 1-8: 1, the reaction temperature is 90-120 ℃, and the reaction time is 60-150 min.
In the seventh step, the oxidant in the reaction process comprises one or more of hydrogen peroxide, ozone, oxygen, sodium nitrate, sodium chlorate and sodium hypochlorite, and the adding amount is 5-50 g/L.
Drawings
FIG. 1 is a schematic flow chart of a treatment method of waste acid from dye sulfonation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The sulfuric acid concentration in the sulfonated waste acid is 28%, the COD content is 13000mg/L, and the potassium sulfate content is 8%. The sulfonated waste acid is pretreated by a security filter to remove impurities, a COD special resin adsorption column adopts the speed of 1BV/h for adsorption, and the COD content in the treated waste acid is reduced to 1500 mg/L; concentrating the waste acid by double-effect evaporation, cooling to room temperature, precipitating potassium sulfate crystals, centrifugally separating, and analyzing the potassium ion content in the filtrate to determine that the potassium sulfate recovery rate reaches 82%; controlling the solid-to-solid ratio of the concentrated solution to the red mud to be 4:1, the reaction temperature to be 103 ℃, the reaction time to be 90min, and adding 5g/L of sodium chlorate to obtain the polymeric ferric aluminum sulfate with the total iron content of 6.2 percent and the aluminum oxide content of 3.4 percent.
Example 2
The sulfuric acid concentration in the sulfonated waste acid is 30%, the COD content is 15000mg/L, and the potassium sulfate content is 10%. The sulfonated waste acid is pretreated by a security filter to remove impurities, a COD special resin adsorption column adopts the speed of 1.5BV/h for adsorption, and the COD content in the treated waste acid is reduced to 2500 mg/L; concentrating the waste acid by double-effect evaporation, cooling to room temperature, precipitating potassium sulfate crystals, centrifugally separating, and analyzing the potassium ion content in the filtrate to determine that the potassium sulfate recovery rate reaches 88%; controlling the solid-to-solid ratio of the concentrated solution to the red mud to be 5:1, the reaction temperature to be 110 ℃, the reaction time to be 100min, and adding 3g/L of sodium chlorate to obtain the polymeric ferric aluminum sulfate with the total iron content of 5.3% and the aluminum oxide content of 2.9%.
Claims (7)
1. A method for treating waste acid generated by sulfonation of dye is characterized in that the waste acid generated by pretreatment, impurity removal, adsorption, concentration, cooling and crystallization is subjected to acid dissolution and polymerization reaction under the action of an oxidant by using red mud as a raw material to prepare a polymeric ferric aluminum sulfate water treatment agent, so that the resource utilization of the waste acid generated by sulfonation of dye is realized, and the process of treating the waste acid generated by sulfonation is as follows:
step one, pretreatment: carrying out pretreatment impurity removal on the sulfonated waste acid to remove mechanical impurities and residual solid suspended matters in the sulfonated waste acid;
step two, adsorption: the pretreated waste acid enters an adsorption system, a special material is used for adsorbing COD in the feed liquid, meanwhile, the water chroma is reduced, the flow rate is controlled to be 1-2 BV/h, and the adsorbed waste acid solution is collected;
step three, desorption: after the adsorption resin is used, methanol desorption liquid is adopted for desorption, and the desorption liquid is repeatedly applied to an adsorption system;
step four, concentration: concentrating the waste acid solution generated in the step two after adsorption by adopting double-effect evaporation;
step five, cooling: cooling the concentrated waste acid, and removing sulfate substances in the waste acid by a crystallization method;
step six, centrifugal separation: conveying the cooled materials to a centrifugal machine by a pump for solid-liquid separation, and returning salt substances to the dye production process for reuse;
step seven, recycling waste acid: and reacting the centrifuged waste acid with red mud, preparing polymeric aluminum ferric sulfate under the action of an oxidant, and filtering the reaction to obtain reddish brown liquid, namely the product.
2. The method for treating the dye sulfonation waste acid as claimed in claim 1, wherein the concentration of sulfuric acid in the waste acid is 25% -35%, the COD content is 10000-20000 mg/L, and the salt substance is mainly potassium sulfate, and the content of the salt substance is 5% -15%.
3. The method for treating waste acid generated by sulfonating dye according to claim 1, wherein the special material is COD special resin.
4. The method for treating the dye sulfonation waste acid as claimed in claim 1, wherein the methanol desorption solution contains 60% to 100% of methanol.
5. The method for treating the dye sulfonation waste acid as claimed in claim 1, wherein the sulfuric acid content of the concentrated waste acid is 35-50%.
6. The method for treating dye sulfonation waste acid as claimed in claim 1, wherein the solid-to-solid ratio of the reaction liquid of the waste acid to the red mud is 2: 1-8: 1, the reaction temperature is 90-120 ℃, and the reaction time is 60-150 min.
7. The method for treating dye sulfonation waste acid according to claim 1, wherein an oxidant in the reaction process comprises one or more of hydrogen peroxide, ozone, oxygen, sodium nitrate, sodium chlorate and sodium hypochlorite, and the adding amount is 5-50 g/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210273953.XA CN114604901A (en) | 2022-03-20 | 2022-03-20 | Method for treating waste acid generated in dye sulfonation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210273953.XA CN114604901A (en) | 2022-03-20 | 2022-03-20 | Method for treating waste acid generated in dye sulfonation |
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| Publication Number | Publication Date |
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| CN114604901A true CN114604901A (en) | 2022-06-10 |
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| CN202210273953.XA Pending CN114604901A (en) | 2022-03-20 | 2022-03-20 | Method for treating waste acid generated in dye sulfonation |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775808A (en) * | 2012-08-23 | 2012-11-14 | 楚源高新科技集团股份有限公司 | Process for recycling ammonium sulfate and synthesizing acidic dye by T-acid mother liquor wastewater |
| CN104829505A (en) * | 2015-04-24 | 2015-08-12 | 黎明化工研究设计院有限责任公司 | Method for separating anthraquinone sulfonic acid from waste acid generated during production process of anthraquinone and derivatives thereof |
| WO2018090167A1 (en) * | 2016-11-15 | 2018-05-24 | 江苏双能太阳能有限公司 | Waste acid treatment process |
| CN110436600A (en) * | 2019-08-21 | 2019-11-12 | 天津理工大学 | A kind of method that red mud disposes production Ti-enriched slag and water purification agent with ferrous waste acid jointly |
-
2022
- 2022-03-20 CN CN202210273953.XA patent/CN114604901A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102775808A (en) * | 2012-08-23 | 2012-11-14 | 楚源高新科技集团股份有限公司 | Process for recycling ammonium sulfate and synthesizing acidic dye by T-acid mother liquor wastewater |
| CN104829505A (en) * | 2015-04-24 | 2015-08-12 | 黎明化工研究设计院有限责任公司 | Method for separating anthraquinone sulfonic acid from waste acid generated during production process of anthraquinone and derivatives thereof |
| WO2018090167A1 (en) * | 2016-11-15 | 2018-05-24 | 江苏双能太阳能有限公司 | Waste acid treatment process |
| CN110436600A (en) * | 2019-08-21 | 2019-11-12 | 天津理工大学 | A kind of method that red mud disposes production Ti-enriched slag and water purification agent with ferrous waste acid jointly |
Non-Patent Citations (1)
| Title |
|---|
| 方标等: "低含量染料废酸综合利用工艺研究", 《化工生产与技术》, vol. 17, no. 2, pages 36 - 39 * |
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