CN111943230A - Recycling treatment method for industrial wastewater byproduct salt - Google Patents
Recycling treatment method for industrial wastewater byproduct salt Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
Abstract
A method for recycling industrial wastewater byproduct salt, belonging to the technical field of environmental protection. The method comprises the following steps: 1) washing salt; 2) dissolving salt; 3) nano-filtration membrane treatment; 4) advanced oxidation treatment; 5) flocculation; 6) settling; 7) performing secondary nanofiltration; 8) and (4) adsorbing. The method for recycling the industrial wastewater byproduct salt adopts the ozone catalytic oxidation technology for oxidation treatment, finally uses the adsorbent to adsorb the filtrate, has good effect of removing organic matters and inorganic matters in the byproduct salt, greatly improves the refining effect, uses the purified solid salt or the refined brine in other industries such as chlor-alkali production, caustic soda production and the like, realizes the recycling of waste, and has high economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a recycling treatment method for industrial wastewater byproduct salt.
Background
A large amount of high-salt organic wastewater is often generated in the chemical production process. Due to high salt content, organic matters in the wastewater cannot be effectively removed directly by means of biochemistry, oxidation and the like. The method mainly treats the high-salt organic wastewater through evaporation, and the evaporation condensate enters biochemical, oxidation and physical and chemical means for further treatment, but a large amount of byproduct salt (NaCl) is generated. Because the byproduct salt still contains a large amount of organic matters or inorganic matters, the byproduct salt cannot be used as industrial raw material salt and further cannot be used for eating or medical use, and most manufacturers accumulate the byproduct salt or treat the byproduct salt as dangerous waste. Not only causes the waste of a large amount of sodium chloride resources, but also seriously damages the ecological environment due to improper treatment. The chlor-alkali industry consumes a large amount of salt for chlor-alkali production every year, so that the refined salt prepared by refining the byproduct salt to remove organic matters and inorganic matters in the waste salt is used for chlor-alkali electrolysis process, and has great economic benefit and social significance. The invention patents of application numbers CN201410009835.3, CN201310184084.4, CN201611042295.4, CN201510089822.6 and the like respectively refer to a method for recycling or refining a byproduct salt, but all the invention patents have a high-temperature calcination step in a refining process, which not only has high treatment cost, but also has requirements on treatment places.
Patent No. CN201510441594.4, name: the invention discloses a refining process method of byproduct salt in a glyphosate production line, which comprises the following steps of regulating the pH value of the obtained nanofiltration membrane dilute solution to 2-12, adding an oxidant for oxidation, wherein the oxidant is sodium hypochlorite and H, the concentration of the oxidant is 100-5000 mg/L, the oxidation temperature is 5-60 ℃, and the oxidation time is 1-5 hours2O2One or more of chlorine dioxide, sodium ferrate and sodium persulfate, and has the following disadvantages: the oxidation efficiency is low, and the dosage is large; the oxidation capability is slightly weaker than that of the advanced oxidation technology, so that the treatment object is not wide and is only limited to organic matters in glyphosate byproduct salt; a new substance is introduced in the oxidation process, so that secondary pollution is easily caused, and the new substance needs to be removed in the subsequent treatment process; and step seven, performing solid-liquid separation on the obtained brine and the precipitated sludge to obtain filtrate, namely refined brine, wherein the filtrate has the defects that residual organic matters exist in the brine, and indexes such as effluent TOC and the like can not stably meet the requirements of the chlor-alkali refined brine.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a resource treatment method for industrial wastewater byproduct salt, which adopts an ozone catalytic oxidation technology to carry out oxidation treatment, and finally uses an adsorbent to adsorb filtrate, so that the effect of removing organic matters and inorganic matters in the byproduct salt is good, the refining effect is greatly improved, and the purified solid salt or the refined brine is used in other industries such as chlor-alkali production, caustic soda production and the like, so that the resource utilization of waste is realized, and the method has high economic and social benefits.
The method for recycling the industrial wastewater byproduct salt is characterized by comprising the following steps of selecting all or a plurality of steps aiming at different byproduct salt, and forming different treatment processes to reach the standard of refined brine:
1) salt washing: cleaning the solid waste salt to be treated by using a cleaning agent for 10-60 min, wherein the using amount of the cleaning agent is 0.1-10 times of the mass of the solid salt, the cleaning temperature is 5-60 ℃, and carrying out solid-liquid separation after cleaning;
2) salt dissolving: adding pure water into the washed solid salt to prepare a solution with the NaCl content of 200-310 g/L, and adjusting the pH value to 6-12 by using NaOH;
3) and (3) nanofiltration membrane treatment: separating and concentrating the salt water by a nanofiltration membrane, wherein the nanofiltration operation pressure is 2.0-3.5 MPa, the temperature is 15-35 ℃, and the nanofiltration recovery rate is 85-90%;
4) advanced oxidation treatment: adjusting the pH value of the obtained nanofiltration membrane dilute solution to 8-12 by using NaOH, carrying out oxidation treatment by using an ozone catalytic oxidation technology, wherein the ozone concentration is 50-1000 mg/L, the oxidation temperature is 5-60 ℃, the oxidation time is 1-5 hours, and the catalyst is one or a mixture of more than one of activated carbon, manganese dioxide, titanium dioxide, magnesium oxide and calcium oxide;
5) flocculation: adding a flocculating agent into the brine after the advanced oxidation, wherein the concentration of the flocculating agent is 10-1000 ppm, continuously stirring and reacting at a low speed, wherein the reaction temperature is 5-60 ℃, and the reaction time is 0.5-2 hours;
6) and (3) settling: adjusting the pH of the solution obtained in the step 5) to 7-8 by using HCl, standing and settling for 0.5-6 h;
7) and (3) secondary nanofiltration: filtering the supernatant after settling by ultrafiltration at an ultrafiltration pressure of 0.15-0.25MPa, and performing secondary nanofiltration on the ultrafiltration product water to further remove impurities in the brine, wherein the nanofiltration pressure is 2.0-3.5 MPa, the temperature is 15-35 ℃, and the nanofiltration recovery rate is 90-95%;
8) adsorption: and (3) carrying out adsorption treatment on the secondary nanofiltration produced water, wherein the adsorbent is one or a mixture of more than one of active carbon, macroporous adsorption resin and kieselguhr, and the filtration speed is 8-20 m/h, so as to finally obtain primary refined brine.
The method for recycling the industrial wastewater byproduct salt is characterized by comprising the following steps of 1): the cleaning agent is one or more aqueous solutions of NaCl, HCl, NaOH, acetone, methanol and ethanol; the cleaning time is 20-50 min, preferably 30-40 min, and more preferably 35-38 min; the dosage of the cleaning agent is 1-8 times, preferably 3-7 times and more preferably 4-6 times of the mass of the solid salt; the cleaning temperature is 10-55 ℃, preferably 20-45 ℃, and more preferably 30-40 ℃.
The method for recycling the industrial wastewater byproduct salt is characterized in that in the step 2): the concentration of the NaCl solution is 220-300 g/L, preferably 255-280 g/L; adjusting the pH value to 7-11, preferably 8-10.
The method for recycling the industrial wastewater byproduct salt is characterized in that in the step 3): the nanofiltration operation pressure is 2.2-3.0 MPa, preferably 2.5-2.8 MPa; the temperature is 20-30 deg.C, preferably 20-25 deg.C.
The method for recycling the industrial wastewater byproduct salt is characterized in that in the step 4): adjusting the pH of the nanofiltration membrane dilute solution to 9-11 by using NaOH, and preferably adjusting the pH to 9.5-10; the concentration of the ozone is 100-800 mg/L, preferably 200-500 mg/L, and more preferably 300-400 mg/L; the oxidation temperature is 10-50 ℃, preferably 20-40 ℃, and more preferably 30-35 ℃; the oxidation time is 2 to 4 hours, more preferably 2.5 to 3 hours.
The method for recycling the industrial wastewater byproduct salt is characterized in that in the step 6): adjusting the pH value to 7.2-7.6; the settling time is 1-5 h, preferably 2-4 h.
The method for recycling the industrial wastewater byproduct salt is characterized in that in the step 7): the ultrafiltration pressure is 0.18-0.23MPa, preferably 0.20-0.21 MPa; the temperature is 20-30 ℃, preferably 20-25 ℃; the filtration rate is 10-18 m/h, preferably 12-16 m/h.
The method for recycling the industrial wastewater byproduct salt adopts the ozone catalytic oxidation technology for oxidation treatment, finally uses the adsorbent to adsorb the filtrate, has good effect of removing organic matters and inorganic matters in the byproduct salt, greatly improves the refining effect, uses the purified solid salt or the refined brine in other industries such as chlor-alkali production, caustic soda production and the like, realizes the recycling of waste, and has high economic and social benefits.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are provided for illustration of the present invention and are not intended to limit the scope of the present invention.
Example 1
Taking 5kg of byproduct salt obtained in the 2,4-D production line, cleaning with a cleaning agent, controlling the mass ratio of the cleaning agent to the solid salt to be 1:1, the cleaning time to be 20min, and the cleaning times to be 1 time, and then carrying out solid-liquid separation to obtain the solid salt. The solid salt is prepared into a solution with NaCl content of 300g/L, and the total organic carbon TOC is measured to be 500mg/L, and the total nitrogen TN is measured to be 50 mg/L.
Adjusting the pH value of the prepared brine to 10 by using 1mol/L NaOH, performing nanofiltration membrane separation, controlling the membrane feeding pressure to be 3.0MPa and the temperature to be 15 +/-2 ℃, and stopping the nanofiltration membrane separation when the concentration multiple of the nanofiltration membrane is 8 times by mass. The total organic carbon TOC of the nanofiltration membrane dilute solution is 26.29mg/L, and the total nitrogen TN is 8.07 mg/L.
Regulating the pH value of the nanofiltration membrane dilute solution to 10.42 by using lmol/L NaOH, performing ozone catalytic oxidation, controlling the concentration of ozone to be 50mg/L, adding a flocculating agent after stirring and reacting for 2.5h at the temperature of 13.7 ℃ by using titanium dioxide as a catalyst, controlling the concentration of the flocculating agent to be 100mg/L, and continuing to stir and react for 0.5h at a slow speed. Then, the pH value is adjusted to 8 by using an lmol/L HCl solution, and the mixture is kept stand and settled for 5 hours. And filtering the supernatant after sedimentation by ultrafiltration at the pressure of 0.2MPa and the temperature of 14 +/-2 ℃, and performing adsorption treatment on the filtrate by using macroporous adsorption resin at the filtering speed of 15m/h, wherein the key indexes of the total organic carbon is 3.5mg/L and the total nitrogen TN is 2.26 mg/L.
Example 2
Taking 5kg of byproduct salt obtained in the production line of preparing glyphosate by a glycine method, cleaning with a cleaning agent, controlling the mass ratio of the dosage of the cleaning agent to the solid salt to be 0.5:1, the cleaning time to be 30min, and the cleaning times to be 1 time, and then carrying out solid-liquid separation to obtain the solid salt. The solid salt is prepared into a solution with the NaCl content of 295g/L, and the total organic carbon TOC is measured to be 400mg/L, the total nitrogen TN is measured to be 25mg/L, and the total nitrogen TP is measured to be 85 mg/L.
Adjusting the pH value of the prepared brine to 10 by using 1mol/L NaOH, performing nanofiltration membrane separation, controlling the membrane feeding pressure to be 2.0MPa and the temperature to be 15 +/-2 ℃, and stopping the nanofiltration membrane separation when the concentration multiple of the nanofiltration membrane is 7 times by mass. The total organic carbon TOC of the nanofiltration membrane dilute solution is 26.29mg/L, the total nitrogen TN is 8.07mg/L, and the total nitrogen TP is 2.74 mg/L.
Regulating the pH value of the nanofiltration membrane dilute solution to 10.42 by using lmol/L NaOH, performing ozone catalytic oxidation, controlling the concentration of ozone to be 50mg/L, adding a flocculating agent after stirring and reacting for 2.5h at the temperature of 13.7 ℃ by using titanium dioxide as a catalyst, controlling the concentration of the flocculating agent to be 100mg/L, and continuing to stir and react for 0.5h at a slow speed. Then, the pH value is adjusted to 7 by using an lmol/L HCl solution, and the mixture is kept stand and settled for 5 hours. And filtering the supernatant after sedimentation by ultrafiltration at the ultrafiltration pressure of 0.2MPa and the temperature of 15.7 +/-2 ℃, adsorbing the filtrate by using active carbon at the filtration speed of 8m/h, wherein the key indexes of the total organic carbon is 3.5mg/L, the total nitrogen TN is 2.26mg/L, and the TP is 0.003 mg/L.
The invention adopts ozone catalytic oxidation: the catalytic ozonation method is an advanced oxidation technology which utilizes a catalyst to convert ozone into active substances with strong oxidizing capability, such as hydroxyl radicals and the like, so as to quickly and thoroughly degrade organic matters in wastewater, and the organic matters can be directly mineralized to generate carbon dioxide and water. The method has the characteristics of high reaction rate, thorough degradation, no secondary pollution, no selectivity, wide application range and the like.
The homogeneous catalytic ozonization utilizes metal ions in the solution as catalyst to promote ozone to generate free radicals (such as. OH) while decomposing ozone, i.e. the metal ions in the solution promote ozone decomposition to generate. O2 -Electron from O2Transfer to another O3Formation of O3 -Then, OH is formed. The heterogeneous catalytic ozonization is an advanced oxidation technology which uses solid metal, metal oxide and metal or metal oxide loaded on a carrier as a catalyst to catalyze the decomposition of ozone into strong oxidizing substances such as hydroxyl radicals and the like so as to degrade organic matters. Partial oxidation energy of oxidizing agentThe force comparison is shown in table 1.
The step 7) of the invention adopts an adsorption process, and the adsorbent is one or a mixture of more than one of active carbon, macroporous adsorption resin and diatomite. The macroporous adsorption resin is also called full porous resin and polymer adsorbent, is a high molecular adsorbent which does not contain ion exchange groups and has a macroporous network structure, belongs to porous cross-linked polymer, and has the functions of separating and enriching organic matters. The resin is generally white, milky white or yellow particles, and some novel resins are yellow, brown yellow to reddish brown, and the particle size is usually 20-60 meshes. Has stable physicochemical properties, is insoluble in water, acid, alkali and hydrophilic organic solvent, is insoluble by heating, and can be used at a temperature below 150 ℃. Macroporous resins have good network structure and large specific surface area, are separation materials combining adsorption and molecular sieving separation principles, and the adsorption is a result of van der waals attraction or hydrogen bond generation. The resins with different polarities and different pore diameters have different selectivity on different compounds, so that the aim of separation and purification is fulfilled. The adsorption of the resin is a physical and chemical action, and the adsorbed substances are easy to elute from the resin, and the resin is easy to regenerate. Therefore, the macroporous adsorption resin has the advantages of good selectivity, high mechanical strength, convenient regeneration treatment and high adsorption speed, and is not influenced by the existence of inorganic salts, strong ions and low molecular compounds.
The following combinations of the corresponding test data demonstrate the beneficial effects of the present invention, see table 2.
Table 2 shows that: compared with the prior glyphosate byproduct salt refining process, on one hand, the prior process has higher TOC removal efficiency, and particularly has more obvious high-efficiency advantages when other industrial byproduct salts (such as 2,4-D byproduct salt and CHD byproduct salt) are treated; on the other hand, the TOC index of the brine treated by the prior art can meet the index of the chlor-alkali refined brine (TOC is less than 10 ppm).
While specific embodiments of the invention have been described above, it will be appreciated by those skilled in the art that these are by way of example only, and that the scope of the invention is defined by the appended claims. Various changes or modifications to these embodiments may be made by those skilled in the art without departing from the principle and spirit of the invention, and these changes or modifications are within the scope of the invention.
Claims (7)
1. A method for recycling industrial wastewater byproduct salt is characterized by comprising the following steps of selecting all or a plurality of steps aiming at different byproduct salt, and forming different treatment processes to reach the standard of refined brine:
1) salt washing: cleaning the solid waste salt to be treated by using a cleaning agent for 10-60 min, wherein the using amount of the cleaning agent is 0.1-10 times of the mass of the solid salt, the cleaning temperature is 5-60 ℃, and carrying out solid-liquid separation after cleaning;
2) salt dissolving: adding pure water into the washed solid salt to prepare a solution with the NaCl content of 200-310 g/L, and adjusting the pH value to 6-12 by using NaOH;
3) and (3) nanofiltration membrane treatment: separating and concentrating the salt solution through a nanofiltration membrane, wherein the nanofiltration operation pressure is 2.0-3.5 MPa, and the temperature is 15-35 ℃;
4) advanced oxidation treatment: adjusting the pH value of the obtained nanofiltration membrane dilute solution to 8-12 by using NaOH, carrying out oxidation treatment by using an ozone catalytic oxidation technology, wherein the ozone concentration is 50-1000 mg/L, the oxidation temperature is 5-60 ℃, the oxidation time is 1-5 hours, and the catalyst is one or a mixture of more than one of activated carbon, manganese dioxide, titanium dioxide, magnesium oxide and calcium oxide;
5) flocculation: adding a flocculating agent into the brine after the advanced oxidation, wherein the concentration of the flocculating agent is 10-1000 ppm, continuously stirring and reacting at a low speed, wherein the reaction temperature is 5-60 ℃, and the reaction time is 0.5-2 hours;
6) and (3) settling: adjusting the pH of the solution obtained in the step 5) to 7-8 by using HCl, standing and settling for 0.5-6 h;
7) and (3) secondary nanofiltration: filtering the supernatant after sedimentation by ultrafiltration at the ultrafiltration pressure of 0.15-0.25MPa, the nanofiltration operation pressure of 2.0-3.5 MPa and the temperature of 15-35 ℃;
8) adsorption: and (3) carrying out adsorption treatment on the secondary nanofiltration produced water, wherein the adsorbent is one or a mixture of more than one of active carbon, macroporous adsorption resin and kieselguhr, and the filtration speed is 8-20 m/h, so as to finally obtain primary refined brine.
2. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein the step 1) comprises: the cleaning agent is one or more aqueous solutions of NaCl, HCl, NaOH, acetone, methanol and ethanol; the cleaning time is 20-50 min, preferably 30-40 min, and more preferably 35-38 min; the dosage of the cleaning agent is 1-8 times, preferably 3-7 times and more preferably 4-6 times of the mass of the solid salt; the cleaning temperature is 10-55 ℃, preferably 20-45 ℃, and more preferably 30-40 ℃.
3. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein the step 2) comprises: the concentration of the NaCl solution is 220-300 g/L, preferably 255-280 g/L; adjusting the pH value to 7-11, preferably 8-10.
4. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein in the step 3): the nanofiltration operation pressure is 2.2-3.0 MPa, preferably 2.5-2.8 MPa; the temperature is 20-30 deg.C, preferably 20-25 deg.C.
5. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein the step 4) comprises: adjusting the pH of the nanofiltration membrane dilute solution to 9-11 by using NaOH, and preferably adjusting the pH to 9.5-10; the concentration of the ozone is 100-800 mg/L, preferably 200-500 mg/L, and more preferably 300-400 mg/L; the oxidation temperature is 10-50 ℃, preferably 20-40 ℃, and more preferably 30-35 ℃; the oxidation time is 2 to 4 hours, more preferably 2.5 to 3 hours.
6. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein in the step 6): adjusting the pH value to 7.2-7.6; the settling time is 1-5 h, preferably 2-4 h.
7. The method for recycling industrial wastewater byproduct salts according to claim 1, wherein in the step 7): the ultrafiltration pressure is 0.18-0.23MPa, preferably 0.20-0.21 MPa; the temperature is 20-30 ℃, preferably 20-25 ℃; the filtration rate is 10-18 m/h, preferably 12-16 m/h.
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| CN112960817A (en) * | 2021-03-02 | 2021-06-15 | 浙江海禹环保科技有限公司 | Comprehensive treatment method and system for hydrazine hydrate waste salt |
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| CN113754192A (en) * | 2021-09-14 | 2021-12-07 | 叶婷婷 | High-salinity wastewater refining process and equipment |
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| CN114940546A (en) * | 2022-04-29 | 2022-08-26 | 清创人和生态工程技术有限公司 | Treatment method for recycling hydrazine hydrate industrial wastewater to prepare caustic soda by electrolyzing salt solution |
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