CN112010492B - Physicochemical and biochemical treatment process for 1-aminoanthraquinone wastewater - Google Patents
Physicochemical and biochemical treatment process for 1-aminoanthraquinone wastewater Download PDFInfo
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Abstract
The invention discloses a physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater. Respectively and independently collecting and pretreating nitrating acid water, nitrating neutralization water and reducing mother liquor generated in the production process of 1-aminoanthraquinone, wherein the nitrating acid water pretreatment method comprises macroporous resin adsorption, lime neutralization and filter pressing dehydration, the nitrating neutralization water pretreatment method comprises flocculation precipitation and activated carbon filtration, and the reducing mother liquor pretreatment method comprises evaporation treatment; reducing washing water discharged from a workshop and pretreated nitrifying acid water, nitrifying neutralization water and reducing mother liquor evaporation condensate water are discharged to a wastewater collection tank together for storage, and plant ground washing water, domestic sewage and the like are discharged to a low-concentration wastewater tank for storage; pumping the high-concentration production wastewater in the collection tank and the low-concentration wastewater in the low-concentration wastewater tank into a regulating tank according to a proportion according to a blending requirement, homogenizing, and adding various nutrient elements required by biochemical treatment; the homogenized wastewater is sequentially treated by a coagulating sedimentation tank, a hydrolysis acidification tank, a multi-stage A/O tank, an intermediate sedimentation tank, a decolorization reaction tank and a flocculation sedimentation tank, and the treated effluent can reach the first-level standard of Integrated wastewater discharge Standard (GB 8978-1996).
Description
Technical Field
The invention relates to a wastewater treatment process, which directly relates to a 1-aminoanthraquinone production wastewater treatment process, in particular to the treatment of aminoanthraquinone wastewater which is high in salt, COD, nitrogen and difficult to degrade.
Technical Field
1-aminoanthraquinone is an important dye intermediate and is widely applied to the fields of anthraquinone dyes, medicines and the like. The 1-aminoanthraquinone production wastewater has the characteristics of high salt content, high COD (chemical oxygen demand), high nitrogen content and difficult biodegradation, and organic pollutants in the wastewater are difficult to effectively remove by the conventional technology and process.
Four kinds of waste water, namely nitration acid water, nitration neutralization water, reduction mother liquor and reduction washing water, are discharged in the production process of the 1-aminoanthraquinone. The nitrifying acid water is acidic, contains a large amount of nitrate, anthraquinone and nitroanthraquinone, has high total nitrogen content and is difficult to biodegrade; the chroma of the nitration neutralization water is 2000-5000 times; the salt content in the reduction mother liquor is up to 15-18%, the COD is up to 30000-35000 mg/L, and the chroma is up to 20000 times. If the wastewater is directly mixed for treatment, the biochemical system cannot normally operate, so various types of wastewater need to be subjected to targeted pretreatment to improve the biodegradability of the wastewater.
The wastewater nutrient substance has a single structure, the wastewater contains substances such as sulfate, nitrate, sulfide and sulfite, the activated sludge is easily inhibited, and the problems of rapid reduction of pH and biomass of a biochemical system and the like frequently occur in a conventional biological treatment system, so that the normal operation of the system is seriously influenced.
In view of the difficulty of wastewater treatment, a wastewater treatment technology which is reliable in technology, stable in operation and capable of treating effluent quality up to the standard is urgently needed to solve the environmental protection problem which restricts the development of the industry.
Disclosure of Invention
The invention aims to solve the technical problems and provides the 1-aminoanthraquinone production wastewater treatment process which is reliable in technology, stable in operation and capable of treating the effluent quality to reach the standard.
The technical scheme adopted by the invention is as follows: the method comprises the following steps: respectively and independently collecting and pretreating nitrating acid water, nitration neutralization water and reduction mother liquor generated in the production process of 1-aminoanthraquinone, wherein the nitrating acid water pretreatment method comprises macroporous resin adsorption and lime neutralization, filter pressing and dehydration, the nitration neutralization water pretreatment method comprises flocculation precipitation and activated carbon filtration, and the reduction mother liquor pretreatment method comprises evaporation treatment; step two: reducing washing water discharged from a workshop and pretreated nitrifying acid water, nitrifying neutralization water and reducing mother liquor evaporation condensate water are discharged to a wastewater collection tank together for storage, and plant ground washing water and domestic sewage are discharged to a low-concentration wastewater tank for storage; step three: pumping the high-concentration production wastewater in the wastewater collection tank and the low-concentration wastewater in the low-concentration wastewater collection tank into a regulating tank according to a mixing requirement in proportion, homogenizing, and adding various nutrient elements required by biochemical treatment; step four: pumping the wastewater obtained in the last step to a coagulative precipitation tank by a water pump, adding alkali into a stirring area of the coagulative precipitation tank to adjust the pH value, and adding polyaluminium chloride (PAC) and Polyacrylamide (PAM) to react to remove partial colloidal substances and suspended substances in the wastewater; step five: pumping the wastewater obtained in the last step to a hydrolysis acidification pool by a water pump for treatment, and converting macromolecular substances in the wastewater into micromolecular biodegradable components; step six: sequentially treating the wastewater obtained in the last step through a multi-stage A/O pool, wherein the A pool is an anoxic pool, the O pool is an aerobic pool, a mixed solution in the O pool flows back to the A pool, denitrifying bacteria in the A pool perform denitrification in an anoxic environment and remove part of COD, and aerobic microorganisms in the O pool oxidize ammonia nitrogen in the wastewater into nitrate nitrogen and COD into carbon dioxide and water; step seven: discharging the wastewater obtained in the last step into a middle sedimentation tank for sludge-water separation, refluxing the settled sludge into a first-stage A tank by a reflux pump, and discharging the supernatant into a subsequent unit for treatment; step eight: the wastewater obtained in the last step flows to a decolorization reaction tank automatically, a decolorizer is added to remove the chromaticity of the wastewater, and an oxidant adding device is reserved as a security measure for further removing residual organic matters in the wastewater; step nine: adding PAC and PAM into the wastewater after decolorization and oxidation in a flocculation sedimentation tank for flocculation sedimentation, wherein the effluent reaches the first-level standard discharge of Integrated wastewater discharge Standard (GB 8978-1996); step ten: residual sludge produced by the system is collected by a sludge tank, then is dehydrated by a filter press, the dehydrated sludge is transported and disposed, and filtrate is discharged to an adjusting tank for repeated treatment.
As an improved scheme of the invention, the flow rate of macroporous resin adsorption of the nitrating acid water is controlled within the range of 1-2 BV/h, the COD removal rate of effluent is less than 75%, and the chroma removal rate is less than 80% as an adsorption endpoint, and the analysis is started.
According to an improved scheme of the invention, after the nitrating acid water is adsorbed by resin, calcium hydroxide powder is added for neutralization, calcium hydroxide and sulfate in the wastewater form calcium sulfate, and the pH value of the wastewater reaches 7-10 as a neutralization reaction end point.
As an improvement scheme of the invention, after the nitration acid water is neutralized, a PAM solution is added into the mixture of lime and wastewater for flocculation, then the mixture is pumped to a filter press for dehydration, filtrate automatically flows to a wastewater collection tank for temporary storage, and the dehydrated sludge is transported to the outside for disposal.
As an improved scheme of the invention, the nitrification neutralization water is firstly added with PAC and PAM for flocculation and precipitation treatment, the adding amount of PAC is 200-400 mg/L, and the adding amount of PAM is 5-15 mg/L; then filtering by an activated carbon column, wherein the filtering speed of the activated carbon column is 1-2 BV/h.
According to an improved scheme of the invention, the reduction mother liquor is evaporated by a negative pressure evaporator, the evaporation control temperature is 60-90 ℃, the evaporated condensate water is sent to a wastewater collection pool, and the waste salt obtained by evaporation is treated according to hazardous waste.
As an improved scheme of the invention, the wastewater of the wastewater collection tank and the low-concentration wastewater tank is pumped to the adjusting tank for water distribution by taking the standard that the total salt content of the adjusting tank is controlled to be 14000 +/-1000 mg/L, COD and the concentration is less than 3000 mg/L.
As an improved scheme of the invention, a carbon source and phosphorus nutrient elements are added in the adjusting tank according to the composition of each nutrient element in the wastewater, the pH is adjusted to 6-8 by pre-adding alkali according to the pH of the wastewater, and an aeration stirring device is arranged in the adjusting tank and used for stirring and balancing the wastewater, the nutrient elements and the medicament.
As an improved scheme of the invention, a suspended vinylon soft filler is arranged in a hydrolysis acidification tank and is used for increasing the total microbial quantity and the diversity of microbial populations, the height of a filler layer is 2.5-3.5 m, and the specific surface area of the filler is 3000-5000 m2/m3The diameter of the filler filament is 3-5 μm.
As an improved scheme of the invention, a submersible stirrer is arranged in the A tank of the multistage A/O tank, and the stirring intensity is 8-16W/m3And the diagonal is arranged in the tank and is used for fully stirring and uniformly mixing the wastewater and the sludge.
1 as an improved scheme of the invention, in a multi-stage A/O pool, the volume load of total COD is controlled to be 0.3-0.8 kgCOD/m3D, controlling the biomass of the activated sludge within the range of 3000-8000 mg/L, wherein each O pool is provided with a mixed liquid reflux pump which refluxes to the A pool, the reflux pump is provided with a flow regulating valve and a flowmeter, and the reflux ratio is 50-300%.
As an improved scheme of the invention, in a multi-stage A/O pool, each O pool is provided with a pH on-line detector and an alkali adding device for maintaining the pH of the system within a range of 7.0-8.0, the A pools except the first stage are provided with carbon source supplementing devices for supplementing carbon sources for denitrification, the A pool controls the dissolved oxygen within a range of 0.2-0.5 mg/L, and the O pools control the dissolved oxygen within a range of 2.0-5.0 mg/L.
As an improved scheme of the invention, the intermediate sedimentation tank is provided with a sludge reflux pump, and the sludge reflux ratio is 60-100%.
As an improvement scheme of the invention, a liquid quaternary amine type decolorizing agent is added into a decolorizing reaction tank, the dosage is 5-50 mg/L, and if the system is impacted abnormally, a sodium hypochlorite oxidant adding device is started as a security measure to ensure that the effluent water reaches the standard.
As an improved scheme of the invention, the PAC dosage in the coagulation sedimentation tank and the flocculation sedimentation tank is 50-300 mg/L, the PAM dosage is 5-10 mg/L, and the dosage point is provided with an air stripping stirring device to meet the hydraulic condition required by the coagulation reaction of the medicament and the wastewater.
The invention has the advantages that: the biodegradability of various types of wastewater with different water quality characteristics is improved by separately collecting and pretreating the wastewater, the quality of inlet water of a biochemical system is adjusted by homogenization, COD, total nitrogen, chromaticity and the like in the wastewater are effectively removed by a combined process, and the outlet water can reach the first-level standard of Integrated wastewater discharge Standard (GB 8978-1996).
Drawings
FIG. 1 is a flow chart of the process for treating wastewater from 1-aminoanthraquinone production according to the present invention.
FIG. 2 is a graph of COD data from biochemical unit runs.
FIG. 3 is a COD data chart of the operation of the decoloring and flocculating unit.
Figure 4 is a graph of total nitrogen data for system operation.
Detailed Description
The invention will be further explained with reference to the drawings.
As shown in FIG. 1, the sewage treatment process of the present invention is as follows:
respectively and independently collecting nitration acid water, nitration neutralization water and reduction mother liquor generated in the production process of 1-aminoanthraquinone in a collection tank, dehydrating and pretreating the nitration acid water by using a macroporous resin adsorption column, a lime neutralization tank and a filter press, pretreating the nitration neutralization water by using a flocculation precipitation tank and an active carbon filter column, and evaporating the reduction mother liquor by using an MVR evaporator; reducing washing water discharged from a workshop and pretreated nitrifying acid water, nitrification neutralization water and reducing mother liquor evaporation condensate water are discharged to a wastewater collection tank together for storage, and plant ground washing water, domestic sewage and the like are discharged to a low-concentration wastewater tank for storage.
The high-concentration production wastewater in the collection tank and the low-concentration wastewater in the low-concentration wastewater tank are pumped into an adjusting tank according to respective salt content and COD content in proportion for homogeneous water distribution, the total salt content after water distribution in the adjusting tank is 14000 +/-1000 mg/L, the COD is controlled to 2000-3000 mg/L, and various nutrient elements required by biochemical treatment are supplemented and added in the adjusting tank according to the proportion of the COD, the nitrogen and the phosphorus in the wastewater.
Lifting the prepared wastewater to a coagulation sedimentation tank by a water pump, adding acid and alkali in a stirring area of the coagulation tank to adjust the pH value, and adding polyaluminium chloride (PAC) and Polyacrylamide (PAM) to react to remove partial colloidal substances and suspended substances in the wastewater; pumping the wastewater into a hydrolysis acidification tank by a water pump for treatment, and converting macromolecular substances in the wastewater into micromolecular easily biodegradable components; the effluent of the hydrolysis tank is sequentially treated by a secondary A/O tank, wherein the A tank is an anoxic tank, the O tank is an aerobic tank, the mixed liquid in the O tank flows back to the A tank, denitrifying bacteria in the A tank carry out denitrification and denitrogenation in an anoxic environment and remove part of COD, and aerobic microorganisms in the O tank oxidize ammonia nitrogen in the wastewater into nitrate nitrogen and COD into carbon dioxide and water; the secondary A pool is provided with a carbon source supplementing device for supplementing a carbon source required by denitrification; the two-stage O tanks are provided with an alkali adding device and a pH detector and are used for controlling the pH to be in the range of 7.0-8.0; discharging the A/O effluent into an intermediate sedimentation tank for mud-water separation, refluxing the precipitated sludge into a first-stage A tank by a reflux pump, and discharging the supernatant into a subsequent unit for treatment; the effluent of the sedimentation tank automatically flows to a decolorization reaction tank, a decolorizing agent is added to remove the chroma of the wastewater, and an oxidant adding device is reserved as a security measure for further removing residual organic matters in the wastewater; and adding PAC and PAM into the wastewater subjected to decoloration and oxidation in a flocculation sedimentation tank for flocculation sedimentation, wherein the effluent reaches the primary standard of Integrated wastewater discharge Standard (GB 8978-1996).
Medicament: supplementing glucose and sodium dihydrogen phosphate as nutrient elements into the adjusting tank, and adding partial alkali to pre-adjust the pH value; adding PAC and PAM into a reaction zone of the coagulating sedimentation tank to remove COD and suspended matters in the wastewater, and adding alkali to adjust the pH value to be within the range of 7.5-8.0; the second-stage A pool is provided with a methanol adding device for supplementing a carbon source required by denitrification; the two-stage O tanks are provided with an alkali adding device and a pH detector and are used for controlling the pH value to be 7.0-8.0; adding a decolorizing agent into the decolorizing reaction tank to remove the chromaticity of the wastewater, and reserving an oxidant adding device as a security measure for further removing residual organic matters in the wastewater; PAC and PAM are added into a reaction zone of the flocculation sedimentation tank to remove suspended matters in the wastewater.
Sludge: carrying out outward transportation treatment on the sludge after neutralization and dehydration of the nitrifying acid water; waste salt produced by MVR evaporation of the reduction mother liquor is treated according to hazardous waste; and collecting residual sludge generated by the coagulating sedimentation tank, the hydrolysis acidification tank, the two-stage A/O tank and the flocculation sedimentation tank in the sludge tank, concentrating, pumping into a filter press machine room for filter pressing, returning the filter press liquid to the regulating tank, and transporting and disposing the dewatered sludge.
The experimental results are as follows:
after the system is debugged for 3 months, the system runs stably. The operation effect of the pretreatment unit after stable operation is shown in table 1:
TABLE 1 Effect of pretreatment Unit operation
After stable operation, the operation effect of the biochemical system is as follows:
the inlet water amount is 1000-1200 m3D, 14000 +/-1000 mg/L, COD of salt content of regulating reservoircr2000-3000 mg/L and 200-400 mg/L of total nitrogen, and continuously detecting the water quality parameters of the effluent water of the main process, as shown in figures 2, 3 and 4, the COD of the effluent water of the sewage treatment system is basically below 100mg/L, and the total nitrogen is below 30mg/L, so that the effluent water reaches the first-level standard discharge of Integrated wastewater discharge Standard (GB 8978-1996).
Claims (15)
1. A physicochemical and biochemical treatment process for 1-aminoanthraquinone production wastewater is characterized by comprising the following steps:
the method comprises the following steps: respectively and independently collecting and pretreating nitrating acid water, nitration neutralization water and reduction mother liquor generated in the production process of 1-aminoanthraquinone, wherein the nitrating acid water pretreatment method comprises macroporous resin adsorption and lime neutralization, filter pressing and dehydration, the nitration neutralization water pretreatment method comprises flocculation precipitation and activated carbon filtration, and the reduction mother liquor pretreatment method comprises evaporation treatment;
step two: reducing washing water discharged from a workshop and pretreated nitrifying acid water, nitrifying neutralization water and reducing mother liquor evaporation condensate water are discharged to a wastewater collection tank together for storage, and plant ground washing water and domestic sewage are discharged to a low-concentration wastewater tank for storage;
step three: pumping the high-concentration production wastewater in the wastewater collection tank and the low-concentration wastewater in the low-concentration wastewater tank into a regulating tank according to a proportion according to a blending requirement, homogenizing, and adding various nutrient elements required by biochemical treatment;
step four: pumping the wastewater obtained in the last step to a coagulative precipitation tank by a water pump, adding alkali into a stirring area of the coagulative precipitation tank to adjust the pH value, and adding polyaluminium chloride and polyacrylamide to react to remove part of colloidal substances and suspended substances in the wastewater;
step five: pumping the wastewater obtained in the last step to a hydrolysis acidification pool by a water pump for treatment, and converting macromolecular substances in the wastewater into micromolecular biodegradable components;
step six: sequentially treating the wastewater obtained in the last step by a multi-stage A/O pool, wherein the A pool is an anoxic pool, the O pool is an aerobic pool, a mixed solution in the O pool flows back to the A pool, denitrifying bacteria in the A pool perform denitrification in an anoxic environment and remove part of COD, and aerobic microorganisms in the O pool oxidize ammonia nitrogen in the wastewater into nitrate nitrogen and COD into carbon dioxide and water;
step seven: discharging the wastewater obtained in the last step into an intermediate sedimentation tank for mud-water separation, refluxing the precipitated sludge into a first-stage A tank by a reflux pump, and discharging the supernatant into a subsequent unit for treatment;
step eight: the wastewater obtained in the last step flows to a decolorization reaction tank automatically, a decolorizer is added to remove the chromaticity of the wastewater, and an oxidant adding device is reserved as a security measure for further removing residual organic matters in the wastewater;
step nine: adding polyaluminium chloride and polyacrylamide into the wastewater after the decolorization and the oxidation in a flocculation precipitation tank for flocculation precipitation, wherein the effluent reaches the primary standard discharge of Integrated wastewater discharge Standard GB 8978-1996;
step ten: residual sludge produced by the system is collected by a sludge tank, then is dehydrated by a filter press, the dehydrated sludge is transported and disposed, and filtrate is discharged to an adjusting tank for repeated treatment.
2. The process for materializing and biochemically treating 1-aminoanthraquinone production wastewater according to claim 1, wherein the flow rate of the macroporous resin adsorption of the nitrifying acid water is controlled within the range of 1-2 BV/h, the adsorption endpoint is determined as the COD removal rate of the effluent water is less than 60%, and the chroma removal rate is less than 70%, and the process begins to analyze.
3. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, which is characterized in that after the nitrating acid water is adsorbed by resin, calcium hydroxide powder is added for neutralization, calcium hydroxide and sulfate in the wastewater form calcium sulfate, and the neutralization reaction end point is taken as that the pH value of the wastewater reaches 7-10.
4. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, characterized in that after the neutralization treatment of the nitrating acid water, a polyacrylamide solution is added into the mixture of lime and wastewater for flocculation, then the mixture is pumped to a filter press for dehydration, the filtrate automatically flows to a wastewater collection tank for temporary storage, and the dehydrated sludge is transported outside for disposal.
5. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, which is characterized in that the nitrification neutralization water is firstly added with polyaluminium chloride and polyacrylamide for flocculation and precipitation treatment, wherein the adding amount of the polyaluminium chloride is 200-400 mg/L, and the adding amount of the polyacrylamide is 5-15 mg/L; then filtering by an activated carbon column, wherein the filtering speed of the activated carbon column is 1-2 BV/h.
6. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, characterized in that the reducing mother liquor is evaporated by a negative pressure evaporator, the evaporation temperature is controlled to be 60-90 ℃, the evaporated condensate water is sent to a wastewater collection tank, and the waste salt obtained by evaporation is disposed according to dangerous waste.
7. The physicochemical and biochemical treatment process of wastewater from 1-aminoanthraquinone production as claimed in claim 1, wherein the wastewater from wastewater collection tank and low concentration wastewater tank is pumped to the adjusting tank for water distribution, with the standard of controlling the total salt content in the adjusting tank to 14000 ± 1000mg/L, COD and the concentration to be less than 3000 mg/L.
8. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein a carbon source and phosphorus nutrient elements are added in the adjusting tank according to the composition of each nutrient element in the wastewater, the pH is adjusted to 6-8 by pre-adding alkali according to the pH of the wastewater, and an aeration stirring device is arranged in the adjusting tank and used for stirring and balancing the wastewater, the nutrient elements and the medicament.
9. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein suspended vinylon soft filler is arranged in the hydrolysis acidification tank for increasing the total microbial content and microbial population diversity, the height of the filler layer is 2.5-3.5 m, and the specific surface area of the filler is 3000-5000 m2 /m3The diameter of the filler filament is 3-5 μm.
10. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein a submersible stirrer is arranged in the A tank of the multistage A/O tank, and the stirring intensity is 8-16W/m3And the diagonal is arranged in the tank and is used for fully stirring and uniformly mixing the wastewater and the sludge.
11. The process for physicochemical and biochemical treatment of 1-aminoanthraquinone production wastewater according to claim 1, wherein the total COD volume load in the multistage A/O tank is controlled to be 0.3-0.8 kgCOD/m3D, controlling the biomass of the activated sludge within the range of 3000-8000 mg/L, wherein each O pool is provided with a mixed liquid reflux pump which refluxes to the A pool, the reflux pump is provided with a flow regulating valve and a flowmeter, and the reflux ratio is 50-300%.
12. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein in the multistage A/O pools, each O pool is provided with a pH on-line detector and an alkali adding device for maintaining the pH of the system within a range of 7.0-8.0, the A pools except the first stage are provided with carbon source supplementing devices for supplementing carbon sources for denitrification, the A pool controls the dissolved oxygen within a range of 0.2-0.5 mg/L, and the O pool controls the dissolved oxygen within a range of 2.0-5.0 mg/L.
13. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein the intermediate sedimentation tank is provided with a sludge reflux pump, and the sludge reflux ratio is 60-100%.
14. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein a liquid quaternary amine type decolorizing agent is added into the decolorizing reaction tank, the dosage is 5-50 mg/L, and if the system is impacted abnormally, a sodium hypochlorite oxidant adding device is started as a security measure to ensure that the effluent reaches the standard.
15. The physicochemical and biochemical treatment process of 1-aminoanthraquinone production wastewater as claimed in claim 1, wherein the dosage of the polyaluminium chloride in the coagulation sedimentation tank and the flocculation sedimentation tank is 50-300 mg/L, the dosage of the polyacrylamide is 5-10 mg/L, and a gas stripping stirring device is arranged at the dosage point to meet the hydraulic conditions required by the coagulation reaction of the medicament and the wastewater.
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