CN113666555A - Comprehensive treatment process for anode etching liquid and high-iron waste hydrochloric acid - Google Patents
Comprehensive treatment process for anode etching liquid and high-iron waste hydrochloric acid Download PDFInfo
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- CN113666555A CN113666555A CN202110621900.8A CN202110621900A CN113666555A CN 113666555 A CN113666555 A CN 113666555A CN 202110621900 A CN202110621900 A CN 202110621900A CN 113666555 A CN113666555 A CN 113666555A
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- hydrochloric acid
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002699 waste material Substances 0.000 title claims abstract description 42
- 238000005530 etching Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000007788 liquid Substances 0.000 title claims abstract description 26
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 239000010802 sludge Substances 0.000 claims description 17
- 238000004821 distillation Methods 0.000 claims description 13
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 12
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 12
- 239000004571 lime Substances 0.000 claims description 12
- 239000008267 milk Substances 0.000 claims description 9
- 210000004080 milk Anatomy 0.000 claims description 9
- 235000013336 milk Nutrition 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 8
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000010865 sewage Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 15
- 239000002920 hazardous waste Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 150000007513 acids Chemical class 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010812 mixed waste Substances 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 2
- 229910000391 tricalcium phosphate Inorganic materials 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 238000011172 small scale experimental method Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- 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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/12—Nature of the water, waste water, sewage or sludge to be treated from the silicate or ceramic industries, e.g. waste waters from cement or glass factories
Abstract
The invention relates to the technical field of hazardous waste treatment, in particular to a comprehensive treatment process of anode etching liquid and high-iron waste hydrochloric acid, which can shorten the working hours, improve the treatment efficiency, reduce the operation cost and improve the treatment effect on waste acid, wherein the anode etching liquid produced in the OLED industry and the high-iron waste hydrochloric acid commonly seen in national class HW34 hazardous wastes are taken as treatment objects. The method for treating wastes with wastes has the characteristics of simple process and low operation cost, and has great significance for green production of hazardous waste disposal units.
Description
Technical Field
The invention relates to the technical field of hazardous waste treatment, in particular to a comprehensive treatment process of anode etching liquid and high-iron waste hydrochloric acid.
Background
Acid pickling galvanization is a common steel treatment process, aims to delay environmental corrosion of steel materials, and usually uses hydrochloric acid as a cleaning agent, generates a large amount of high-iron waste hydrochloric acid every year, contains a small amount of zinc ions, and has the characteristic of high ammonia nitrogen. The anode etching liquid is from the OLED industry, is composed of phosphoric acid, nitric acid and acetic acid, even has a smoke phenomenon due to certain high-concentration acid, and has high treatment difficulty due to the characteristics of high acidity, high total phosphorus, high total nitrogen and high COD. No matter which waste acid all has strong corrosivity, when present is handled it, all need consume a large amount of alkaline medicament and neutralize to produce a large amount of precipitations in the course of handling, follow-up direct entering landfill yard or get into the landfill yard through solidification back, can cause land resource waste, and its treatment cost is high simultaneously, and is very bottom to the utilization ratio of resource, thereby leads to its treatment effect relatively poor.
Disclosure of Invention
In order to solve the technical problems, the invention provides the comprehensive treatment process of the anodic etching liquid and the waste hydrochloric acid of the high-speed rail, which can shorten the working hours, improve the treatment efficiency, reduce the operation cost and improve the treatment effect on waste acid.
The invention relates to a comprehensive treatment process of anode etching liquid and high-iron waste hydrochloric acid, which comprises the following steps of:
s1, respectively adding the anode etching solution and the waste high-iron hydrochloric acid into a reaction kettle according to the proportion of 1: 1-1: 2, mixing, and adding water to dilute;
s2, starting stirring, adding 30% by mass of liquid caustic soda into the reaction kettle until the pH value of the whole solution reaches 3.0-6.0, and reacting for 10-20 minutes;
s3, continuously adding lime milk with the mass fraction of 10% into the reaction kettle until the pH value reaches 7.0-10.0, and reacting for 30 minutes;
s4, introducing the treated mixed liquor into a filter press for filter pressing treatment, carrying out filter pressing by the filter press, conveying the sludge to a landfill, and feeding the filtrate into a distillation system;
s5, setting the distillation temperature at 105 ℃, stopping distillation when 60-80% of distillate is distilled out, allowing the distillate to enter a sewage biochemical system through an air cooler, and conveying the residual materials to an incineration workshop for incineration treatment. E-mail
Specifically, the mixing ratio of the anode etching solution and the high-iron waste hydrochloric acid in the S1 is preferably 1: 2-3: 4.
Specifically, in the step S2, 30% by mass of liquid caustic soda is added into the reaction kettle until the pH value of the whole solution reaches 5.0-6.0.
Specifically, in the S3, lime milk with the mass fraction of 10% is added into the reaction kettle until the pH value reaches 7.5-8.5.
Specifically, after the reaction of S2 and S3 is completed, the reacted solution is sampled and detected, the solution is qualified and then enters the next operation, and if the solution is not qualified, the steps of S2 and S3 are repeated.
Specifically, in S5, the distillation temperature is set to 105 ℃, and the distillation is stopped when 75-80% of the fraction is distilled.
The comprehensive treatment process comprises the steps of respectively pumping two acids with the mass ratio (anode etching liquid: high-iron waste hydrochloric acid) of 0.5-0.75 into a reaction kettle, adding a certain amount of water for dilution, starting stirring, adding liquid alkali with the mass fraction of 30% into the reaction kettle until the pH value is 5.0-6.0, and reacting for 10-20 minutes. Continuously adding lime milk with the mass fraction of 10% into the reaction kettle until the pH value reaches 7.5-8.5, and reacting for 30 minutes. After filter pressing by a filter press, the sludge is sent to a landfill, and the filtrate enters a distillation system. Setting the distillation temperature at 105 ℃, stopping distillation when 75-80% of distillate is distilled out, allowing the distillate to enter a sewage biochemical system through an air cooler, and conveying the kettle residue to an incineration workshop for treatment.
In the test process, a large number of small-scale experiments are carried out, the single treatment scheme and the comprehensive treatment scheme of the two waste acids are compared, the comprehensive treatment scheme is determined to obviously reduce the mud yield, and the scheme is verified through actual production in a workshop, so that the problem of large mud yield is solved, the land resource utilization efficiency is improved, and the cost is reduced. Because the high-iron waste acid is mainly generated into Fe (OH) when being separately treated2Precipitating, treating the anodic etching liquid separately to mainly generate Ca3(PO4)2Precipitation, during which Fe is mainly formed3(PO4)2Precipitation, thereby saving the addition of liquid caustic soda and lime milk during comprehensive disposal, and assuming that hydrochloric acid contains 3mol/L of Fe2+The anode etching solution contains 2mol/L PO43-When 1L of hydrochloric acid and 1L of the anodic etching solution were disposed, the theoretical sludge yield was 3M (Fe (OH))2)+M(Ca3(PO4)2) The theoretical sludge yield at the time of comprehensive disposal is 3 × M (iron ions) +2 × M (phosphate radicals) ═ 3 × 56+2 × 95 ═ 358g, that is, the theoretical sludge yield can be reduced by about 38%. And the anode etching liquid and the lime cream have high reaction speed, so that a large amount of lime is wrapped in the calcium phosphate sediment and cannot completely react, the sludge yield is increased, and the waste of raw materials is also caused.
Compared with the prior art, the invention has the beneficial effects that:
when two waste acids, namely anode etching liquid and high-iron waste hydrochloric acid, are used as dangerous waste and enter a hazardous waste disposal unit, the disposal schemes of various waste acids are researched, and the method has great significance for saving cost and optimizing resource utilization rate.
The disposal method solves the problems of high sludge production, low disposal efficiency and high operation cost when two common waste acids are separately disposed, and provides a comprehensive disposal process which shortens the working hours and solves the problems of high COD and total nitrogen, large sludge production and high disposal cost when the waste acids are separately disposed;
the treatment method of the invention reduces the total sludge production by about 35 percent and the total treatment cost by about 15 percent. The method for treating wastes with wastes has the characteristics of simple process and low operation cost, and has great significance for green production of hazardous waste disposal units.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Waste hydrochloric acid produced by a certain steel processing enterprise and anode etching liquid produced by a certain electronic manufacturer are taken as examples, wherein the iron content in the waste hydrochloric acid is 120000mg/mL, the zinc content is 5000mg/mL, the phosphoric acid content in the anode etching liquid is about 4%, the COD is 43900mg/L, and the total nitrogen is 19400 mg/L.
Example 1
The single treatment process of the waste hydrochloric acid comprises the following steps: adding 5 tons of waste hydrochloric acid into a reaction kettle, adding 50 kilograms of calcium hypochlorite, adding 3.5 tons of lime milk with the concentration of 10% and 2.4 tons of liquid caustic soda with the concentration of 30%, wherein the pH value is 9.0, reacting for 60 minutes, performing filter pressing, and obtaining 2.5 tons of sludge (with the water content of 48%) after filter pressing, wherein the filtrate is colorless and transparent, and the heavy metal is qualified;
the independent treatment process of the anodic etching liquid comprises the following steps: 2 tons of anode etching liquid is added into a reaction kettle, 20 kilograms of calcium hypochlorite is added, 7.4 tons of lime milk with the concentration of 10 percent are added, the pH value is 9.0 at the moment, the reaction is carried out for 60 minutes and then is carried out by pressure filtration, 2.5 tons of sludge (the water content is 60 percent) after pressure filtration is generated, the heavy metal in the filtrate is qualified, but the COD and the total nitrogen content are high, and a large amount of sludge cannot be discharged into a biochemical system for treatment.
Example 2
The comprehensive treatment process of the mixed waste acid comprises the following steps: adding 2.2 tons of waste hydrochloric acid and 1.6 tons of anode etching solution into a reaction kettle, adding a certain amount of water for dilution, adding 3.5 tons of 30% liquid caustic soda, adjusting the pH value to 5.5, reacting for 20 minutes, adding 2 tons of 10% lime milk, adjusting the pH value to 8.0, reacting for 30 minutes, and performing filter pressing to obtain 7.3 tons of filtrate, wherein the filtrate is colorless and clear, and the water content of the sludge is 2 tons (46%) after the filter pressing. The filtrate was put into a flash tank and distilled at 105 ℃ for 15 hours to give 5.8 tons of distillate and 1.5 tons of residue.
Sample analysis data is as follows:
when the method is separately treated, each ton of waste hydrochloric acid produces 0.5 ton of mud, and each ton of anode etching solution produces 1.25 ton of mud. When the method is comprehensively treated, the sludge yield per ton of mixed waste acid is 0.52 ton, which is reduced by 36% compared with the wet sludge treated separately.
And (4) cost accounting: the liquid caustic soda with the concentration of 30% is calculated according to 1050 yuan/ton, the lime is calculated according to 800 yuan/ton, the calcium hypochlorite is calculated according to 7900 yuan/ton, steam is self-produced in an incineration workshop and is not counted into the cost, the sludge disposal cost is calculated according to 3000 yuan/ton, and the cost is reduced by 14% through the comprehensive disposal through accounting compared with the cost of single disposal.
The comprehensive treatment analysis data of the mixed waste acid are as follows:
the above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The comprehensive treatment process of the anode etching liquid and the waste hydrochloric acid of the high-speed rail is characterized by comprising the following steps of:
s1, respectively adding the anode etching solution and the waste high-iron hydrochloric acid into a reaction kettle according to the proportion of 1: 1-1: 2, mixing, and adding water to dilute;
s2, starting stirring, adding 30% by mass of liquid caustic soda into the reaction kettle until the pH value of the whole solution reaches 3.0-6.0, and reacting for 10-20 minutes;
s3, continuously adding lime milk with the mass fraction of 10% into the reaction kettle until the pH value reaches 7.0-10.0, and reacting for 30 minutes;
s4, introducing the treated mixed liquor into a filter press for filter pressing treatment, sending sludge to a landfill after filter pressing by the filter press, and feeding filtrate into a distillation system;
s5, setting the distillation temperature at 105 ℃, stopping distillation when 60-80% of distillate is distilled out, allowing the distillate to enter a sewage biochemical system through an air cooler, and conveying the residual materials to an incineration workshop for incineration treatment.
2. The comprehensive treatment process of the anodic etching solution and the high-iron waste hydrochloric acid as claimed in claim 1, wherein the mixing ratio of the anodic etching solution and the high-iron waste hydrochloric acid in S1 is preferably 1: 2-3: 4.
3. The comprehensive treatment process of the anodic etching solution and the high-iron waste hydrochloric acid as claimed in claim 1, wherein preferably, in the step S2, 30% by mass of liquid caustic soda is added into a reaction kettle until the pH value of the whole solution reaches 5.0-6.0.
4. The comprehensive treatment process of the anode etching solution and the high-iron waste hydrochloric acid as claimed in claim 1, wherein preferably, in the step S3, lime milk with the mass fraction of 10% is added into a reaction kettle until the pH value reaches 7.5-8.5.
5. The comprehensive treatment process of the anodic etching solution and the waste hydrochloric acid of the high iron according to claim 1, wherein after the reaction of S2 and S3 is completed, the reacted solution is sampled and detected, and the next operation is carried out after the solution is qualified, and if the solution is not qualified, the steps of S2 and S3 are repeated.
6. The comprehensive treatment process of the anodic etching solution and the high-iron waste hydrochloric acid as claimed in claim 1, wherein in S5, the distillation temperature is set to 105 ℃, and the distillation is stopped when 75-80% of the fraction is distilled out.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811793A (en) * | 2009-02-24 | 2010-08-25 | 宝山钢铁股份有限公司 | Pretreatment process of chromium-containing wastewater |
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2021
- 2021-06-04 CN CN202110621900.8A patent/CN113666555A/en active Pending
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| US20160060113A1 (en) * | 2013-05-02 | 2016-03-03 | Easyminging Sweden Ab | Production of Phosphate Compounds from Materials Containing Phosphorus and at Least One of Iron and Aluminium |
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