CN112110589B - Harmless treatment method of high-concentration buffer hydrofluoric acid etching waste liquid - Google Patents
Harmless treatment method of high-concentration buffer hydrofluoric acid etching waste liquid Download PDFInfo
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- CN112110589B CN112110589B CN202011034072.XA CN202011034072A CN112110589B CN 112110589 B CN112110589 B CN 112110589B CN 202011034072 A CN202011034072 A CN 202011034072A CN 112110589 B CN112110589 B CN 112110589B
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- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F9/00—Multistage treatment of water, waste water or sewage
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
The invention relates to a harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid, belonging to the field of industrial wastewater treatment. The method comprises the following steps: and simultaneously adding the waste liquid and the soluble calcium compound solution into the slightly-soluble calcium compound suspension, and filtering and separating the obtained product after reaction to obtain filter residue and filtrate. The method provided by the invention is used for treating the high-concentration buffered hydrofluoric acid etching waste liquid, the concentration of the obtained fluoride ions in the filtrate meets the first-level standard in Integrated wastewater discharge Standard (GB8978-1996), no ammonia gas escapes in the treatment process, the treatment efficiency is high, and the treatment cost is low.
Description
Technical Field
The invention relates to a harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid, belonging to the field of industrial wastewater treatment.
Background
The buffer hydrofluoric acid etching solution achieves the purpose of etching by removing the part of the oxide layer of the semiconductor silicon wafer film which is not covered by the photoresist, and is widely applied to the manufacture of microstructures and silicon-based light-emitting devices. The chemical reaction equation is as follows:
4HF+SiO 2 →SiF 4 +2H 2 O
SiF 4 +2HF→H 2 SiF 6
during the chemical etching production process, HF is continuously mixed with SiO 2 The chemical reaction is carried out, so that a large amount of H is generated 2 SiF 6 . When H is in the etching solution 2 SiF 6 When the content reaches 10-15%, the viscosity of the etching solution is increased, so that the treatment effect is reduced, and the production requirement cannot be met. During the etching process, due to pure HF and SiO 2 The etching rate of the chemical reaction is difficult to control, so that a certain amount of NH is added into the etching solution by some enterprises 4 HF 2 As a buffer, the consumed fluoride can be replenished to ensure the stability of the etching rate. The waste liquid generated in the production process is fluorine-containing and ammonia-containing waste liquid. According to the first-level standard regulation in the integrated wastewater discharge Standard (GB8978-1996) of China, the maximum allowable discharge concentration of F ions is 10mg/L, and the maximum allowable discharge concentration of ammonia nitrogen is 15mg/L, so that the waste liquid needs to be treated, and the concentration of the waste liquid is reduced to be lower than the maximum allowable discharge concentration before being discharged.
For such waste liquid treatment methods are: precipitation, adsorption, electrodialysis, ion exchange resin, coagulation, freezing, ultrafiltration, etc. Among them, electrodialysis equipment is expensive and the operating level requirement is high; the ion exchange method has complex regeneration and is not suitable for waste liquid with high fluorine content; the coagulant is used independently for treating the fluorine-containing wastewater, so that the medicament cost is high, and the problem of secondary pollution of waste residues exists; the freezing method and the ultrafiltration method have high treatment cost; the adsorption method is suitable for treating low-concentration waste liquid. Therefore, such waste liquid treatment methods are mainly precipitation methods.
The precipitation method mainly comprises a calcium salt precipitation method, a potassium salt precipitation method, a sodium salt precipitation method and the like. Wherein, the fluorine concentration in the filtrate after the potassium salt and sodium salt precipitation treatment is high, and the filtrate can not be discharged after reaching the standard. The calcium salt precipitation method is mainly characterized in that lime, calcium carbonate and calcium chloride are added into waste liquid. When lime and calcium carbonate are added into the waste liquid, fluorine ions and calcium ions react to generate CaF 2 Precipitation, the reaction of the waste liquid can be finished under the alkaline condition, and the waste liquid contains ammonium which can escape in the form of ammonia under the alkaline condition to seriously pollute the environment; directly adding calcium chloride into the waste liquid to react to generate CaF 2 Crystals, more than 60% of which have a particle size of less than 3 μm and are difficult to filter, in order to ensure CaF 2 The crystal has large grain size and is easy to filter, the calcium chloride solution is slowly added into the waste liquid, the method must strictly control the concentration and the adding speed of the fluorinion in the waste liquid, the filtrate separated from the waste liquid within 22 hours can reach the standard, the treatment efficiency is low, and the crystal is treated into the calcium chlorideThe cost is high.
Disclosure of Invention
In order to solve the technical problems, the invention provides a harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid. The method comprises the following steps: and simultaneously adding the waste liquid and the soluble calcium compound solution into the slightly soluble calcium compound suspension, and filtering and separating the obtained product after reaction to obtain filter residue and filtrate.
The principle of the invention is as follows: when the concentration of fluorine ions and calcium ions in the solution is high, calcium fluoride microcrystals with small particle size are instantaneously generated and are difficult to filter. In the suspension of the slightly soluble calcium compound prepared by the invention, the slightly soluble calcium compound is dissociated in water to form a solution with low calcium ion concentration, the speed of dripping the waste liquid and the solution of the soluble calcium compound into the suspension of the slightly soluble calcium compound is controlled, the reaction system is ensured to have lower calcium ion and fluorine ion concentrations, fluorine ions react with calcium ions to generate insoluble calcium fluoride microcrystals, the calcium fluoride microcrystals are gradually increased in the reaction system along with the addition of the waste liquid, the first generated microcrystals can become seed crystals, and finally calcium fluoride crystals with larger granularity and easy filtration are formed. The suspension of the slightly soluble calcium compound plays a role of buffering in the reaction process, and when the concentration of calcium ions in the solution is increased, the suspension is converted to the direction of generating the slightly soluble calcium compound due to the homoionic effect; when the concentration of calcium ions in the solution is reduced, the slightly soluble calcium compound dissociates calcium ions to maintain the concentration of calcium ions in the reaction system and keep the concentration of calcium ions in the reaction under conditions suitable for the formation of larger crystals of calcium fluoride.
Preferably, the sparingly-soluble calcium compound in the suspension of the sparingly-soluble calcium compound is CaO, Ca (OH) 2 And CaSO 4 More preferably CaO and Ca (OH) 2 、CaSO 4 CaO and Ca (OH) 2 CaO and CaSO 4 Mixture of (2), Ca (OH) 2 And CaSO 4 CaO, Ca (OH) 2 And CaSO 4 A mixture of (a).
Preferably, the adding amount of the slightly soluble calcium compound in the slightly soluble calcium compound suspension is 0.5 to 5.5 times, more preferably 1.5 to 4.5 times, and most preferably 2.5 to 3.5 times of the mass of fluorine in the waste liquid; when the addition amount of the slightly-soluble calcium compound is too small, the growth of calcium fluoride crystals is not facilitated, and the filtration is difficult; when the sparingly-soluble calcium compound is added in an excessive amount, the cost of the treatment increases.
Preferably, the adding amount of the water in the suspension of the sparingly-soluble calcium compound is 10-15 times, more preferably 11-14 times, and most preferably 12-13 times of the mass of the fluorine in the waste liquid; when the addition amount of water is too small, the suspension of the slightly soluble calcium compound is too thick and difficult to stir; when the amount of water added is too large, the treatment cost increases.
Preferably, the mass concentration of the fluorine ions in the waste liquid is 60 to 250g/L, and the measurement is carried out by a method of ion selective electrode method for measuring water quality fluoride (GB 7484-87).
Preferably, the soluble calcium compound in the soluble calcium compound solution is Ca (ClO) 2 、CaCN 2 、CaCrO 4 、Ca(H 2 PO 4 ) 2 、Ca(HSO 3 ) 2 、Ca(NO 3 ) 2 、CaI 2 、CaBr 2 And CaCl 2 At least one of (1).
Preferably, the waste liquid and the soluble calcium compound solution are added while keeping the fluorine ions and the calcium ions in equimolar; when the amount of calcium ion substances in the soluble calcium compound solution is lower than that of fluorine ion substances in the waste liquid, the fluorine ion content in the filtrate after the reaction is high; when the amount of calcium ion species in the soluble calcium compound solution is higher than the amount of fluoride ion species in the waste liquid, the treatment cost increases.
Preferably, the adding time of the waste liquid and the soluble calcium compound solution is 15-60min, more preferably 20-40min, and most preferably 25-35 min; when the adding time is too short, calcium fluoride microcrystals generated by the reaction are increased, and the filtration is difficult; when the addition time is too long, the treatment cycle is prolonged, and the treatment efficiency is reduced.
Preferably, the reaction time after the waste liquid and the soluble calcium compound solution are added is 30-90min, more preferably 40-80min, and most preferably 50-70 min; when the reaction time is too short, the fluorine ions and the calcium ions do not fully react, and the concentration of the fluorine ions in the filtrate is high; when the reaction time is too long, the treatment cycle is prolonged, and the treatment efficiency is lowered.
Preferably, washing the filter residue with water until the mass fraction of chloride ions in the filter residue is lower than 0.5%, and then comprehensively utilizing the filter residue in a cement kiln; and evaporating and crystallizing the filtrate to obtain crystalline salt and condensate, wherein the crystalline salt can be comprehensively utilized as an ammonium nitrogen fertilizer, and the condensate can be used as a solvent of a slightly soluble calcium compound suspension and a soluble calcium compound solution and water for washing filter residues.
Preferably, the filtration separation method may be a method such as suction filtration, pressure filtration, or centrifugal separation, and more preferably, centrifugal separation.
Preferably, the device for evaporating and crystallizing can adopt a single-effect evaporator or a multi-effect evaporator, and further preferably adopts a single-effect evaporator.
The invention has the beneficial effects that:
the method provided by the invention is adopted to treat the high-concentration buffered hydrofluoric acid etching waste liquid, the fluoride ion concentration of the obtained filtrate meets the first-level standard in Integrated wastewater discharge Standard (GB8978-1996), no ammonia gas escapes in the treatment process, the treatment efficiency is high, and the treatment cost is low.
Detailed Description
The present invention is described in detail with reference to the following embodiments, but the following embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited to the following embodiments, and any person skilled in the art can make equivalent substitutions or changes according to the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention disclosed by the present invention.
Example 1
A harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid comprises the following steps:
step 1): adding 65ml of condensate and 22.5g of thermal power plant desulfurized gypsum (the mass percentage content of calcium sulfate is 92%) with the water content of 24% into a 250ml beaker, stirring and mixing to prepare a suspension, simultaneously adding 30ml of buffered hydrofluoric acid etching waste liquid with the molar concentration of 10mol/L and the pH value of 4 and 80ml of calcium chloride solution with the concentration of 3.75mol/L by using a separating funnel, keeping the equimolar addition of fluorine ions and calcium ions, wherein the adding time is 30min, and reacting for 60min after the addition;
step 2): adding lime into the product obtained in the step 1) to adjust the pH value to 6.5, and carrying out vacuum filtration for 3min to obtain filter residue and filtrate;
step 3): leaching the filter residue obtained in the step 2) by using condensate with 5 times of the mass of the filter residue for 5 times until the content of chloride ions in the filter residue is 0.43%;
step 4): comprehensively utilizing the filter residue obtained in the step 2) in a cement kiln;
step 5): the concentration of the fluorine ions in the filtrate obtained in the step 2) is 9mg/L, and the filtrate is evaporated and crystallized by using a laboratory distillation device to obtain crystallized salt and condensate;
step 6): the crystal salt obtained in the step 5) can be comprehensively utilized as an ammonium nitrogen fertilizer;
step 7): the condensate obtained in the step 5) is used as the solvent of the desulfurized gypsum suspension and the calcium chloride solution and the washing water of the filter residue.
Example 2
A harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid comprises the following steps:
step 1): adding 65ml of condensate and 22.5g of thermal power plant desulfurized gypsum (the mass percentage content of calcium sulfate is 92%) with the water content of 24% into a 250ml beaker, stirring and mixing to prepare a suspension, adding 30ml of buffered hydrofluoric acid etching waste liquid with the molar concentration of 10mol/L and the pH value of 4 and 80ml of calcium chloride solution with the concentration of 3.75mol/L by using a separating funnel, keeping the equimolar addition of fluorine ions and calcium ions, keeping the addition time of 25min, and reacting for 60min after the addition;
step 2): adding lime into the product obtained in the step 1) to adjust the pH value to 6.5, and carrying out vacuum filtration for 3min to obtain filter residue and filtrate;
step 3): leaching the filter residue obtained in the step 2) by using condensate with 5 times of the mass of the filter residue for 5 times until the content of chloride ions in the filter residue is 0.43%;
and step 4): carrying out cement kiln comprehensive utilization on the filter residue obtained in the step 2);
step 5): the concentration of the fluorine ions in the filtrate obtained in the step 2) is 7mg/L, and the filtrate is evaporated and crystallized by using a laboratory distillation device to obtain crystallized salt and condensate;
step 6): the crystal salt obtained in the step 5) can be comprehensively utilized as an ammonium nitrogen fertilizer;
step 7): the condensate obtained in the step 5) is used as the solvent of the desulfurized gypsum suspension and the calcium chloride solution and the washing water of the filter residue.
Example 3
A harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid comprises the following steps:
step 1): adding 65ml of condensate and 15g of thermal power plant desulfurized gypsum (the mass percentage content of calcium sulfate is 92%) with the water content of 24% into a 250ml beaker, stirring and mixing to prepare a suspension, adding 30ml of buffered hydrofluoric acid etching waste liquid with the molar concentration of 10mol/L and the pH value of 4 and 80ml of calcium chloride solution with the concentration of 3.75mol/L by using a separating funnel, keeping the equimolar addition of fluorine ions and calcium ions, keeping the addition time of 30min, and reacting for 60min after the addition;
step 2): adding lime into the product obtained in the step 1) to adjust the pH value to 6.5, and carrying out vacuum filtration for 3min to obtain filter residue and filtrate;
step 3): leaching the filter residue obtained in the step 2) by using condensate with 5 times of the mass of the filter residue for 5 times until the content of chloride ions in the filter residue is 0.43%;
and step 4): comprehensively utilizing the filter residue obtained in the step 2) in a cement kiln;
step 5): the concentration of the fluorine ions in the filtrate obtained in the step 2) is 8mg/L, and the filtrate is evaporated and crystallized by using a laboratory distillation device to obtain crystallized salt and condensate;
step 6): the crystal salt obtained in the step 5) can be comprehensively utilized as an ammonium nitrogen fertilizer;
step 7): the condensate obtained in the step 5) is used as the solvent of the desulfurized gypsum suspension and the calcium chloride solution and the washing water of the filter residue.
Example 4
A harmless treatment method of high-concentration buffered hydrofluoric acid etching waste liquid comprises the following steps:
step 1): adding 1 condensate and 225kg of thermal power plant desulfurization gypsum (the mass percentage content of calcium sulfate is 92%) with the water content of 24% into a 2000L enamel reaction kettle, stirring and mixing to prepare a suspension, adding 300L of 10mol/L fluorine ion molar concentration and pH 4 buffered hydrofluoric acid etching waste liquid and 800L of 3.75mol/L calcium chloride solution into the suspension by using a diaphragm pump, keeping the fluorine ions and the calcium ions added in an equimolar manner for 30min, and stirring for 60min after the addition;
step 2): adding lime into the product obtained in the step 1) to adjust the pH value to 6.5, and performing centrifugal filtration to obtain filter residue and filtrate;
step 3): leaching the filter residue obtained in the step 2) by using condensate with 5 times of the mass of the filter residue for 5 times until the content of chloride ions in the filter residue is 0.4%;
step 4): comprehensively utilizing the filter residue obtained in the step 2) in a cement kiln;
step 5): the concentration of the fluorine ions in the filtrate obtained in the step 2) is 7mg/L, and the filtrate is evaporated and crystallized by using a single-effect forced circulation evaporator to obtain crystallized salt and condensate;
step 6): the crystal salt obtained in the step 5) can be comprehensively utilized as an ammonium nitrogen fertilizer;
step 7): the condensate obtained in the step 5) is used as the solvent of the desulfurized gypsum suspension and the calcium chloride solution and the washing water of the filter residue.
Claims (8)
1. A harmless treatment method of high-concentration buffer hydrofluoric acid etching waste liquid is characterized in that: the method comprises the following steps: simultaneously adding the waste liquid and the soluble calcium compound solution into the slightly soluble calcium compound suspension, and filtering and separating the obtained product after reaction to obtain filter residue and filtrate;
the soluble calcium compound solution and the waste liquid keep the equimolar addition of calcium ions and fluorine ions in the simultaneous addition process.
2. The method of claim 1, wherein: the slightly soluble calcium compound in the slightly soluble calcium compound suspension is CaO, Ca (OH) 2 And CaSO 4 At least one of。
3. The method of claim 2, wherein: the adding amount of the slightly soluble calcium compound in the slightly soluble calcium compound suspension is 0.5-5.5 times of the mass of fluorine in the waste liquid.
4. The method of claim 3, wherein: the adding amount of water in the suspension of the slightly soluble calcium compound is 10 to 15 times of the mass of fluorine in the waste liquid.
5. The method of claim 4, wherein: the mass concentration of the fluorine ions in the waste liquid is 60-250 g/L.
6. The method of claim 4, wherein: the soluble calcium compound in the soluble calcium compound solution is Ca (ClO) 2 、CaCN 2 、CaCrO 4 、Ca(H 2 PO 4 ) 2 、Ca(HSO 3 ) 2 、Ca(NO 3 ) 2 、CaI 2 、CaBr 2 And CaCl 2 At least one of (1).
7. The method of claim 4, wherein: the reaction time after the waste liquid and the soluble calcium compound solution are added is 30-90 min.
8. The method of claim 1, wherein: washing the filter residue with water until the mass fraction of chloride ions in the filter residue is lower than 0.5%, and then performing comprehensive utilization by a cement kiln; and evaporating and crystallizing the filtrate to obtain crystalline salt and condensate, wherein the crystalline salt can be comprehensively utilized as an ammonium nitrogen fertilizer, and the condensate can be used as a solvent of a slightly soluble calcium compound suspension and a soluble calcium compound solution and washing water of filter residue.
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