CN112979082B - Recycling process of furan ammonium salt production wastewater - Google Patents
Recycling process of furan ammonium salt production wastewater Download PDFInfo
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Abstract
The invention belongs to the technical field of wastewater treatment, in particular to a process for recycling furaminium salt production wastewater, which solves the problems that the treatment of the furaminium salt production wastewater in the prior art lacks economic and effective treatment technology, the traditional distillation treatment is easy to generate flooding phenomenon, the requirement of byproduct salt does not reach the standard and the like, and comprises the following steps: calcining and grinding coal gangue, reacting with hydrochloric acid, and performing thermal decomposition and post-treatment to obtain a settling agent; adjusting the pH value of the wastewater, and adding a settling agent to obtain primary treatment water; after anaerobic reaction, filtering by using a biological membrane to obtain secondary treated water; adding a settling agent to obtain third-stage treated water; after the ozone oxidation reaction, adding an adsorbent for adsorption, standing, filtering and distilling to complete the recycling process of the furan ammonium salt production wastewater. The process has simple operation, the salt content of the effluent is as low as 2 percent, the COD value is obviously reduced, the effluent is clear and transparent, and no visible impurity or impurity is generated.
Description
Technical Field
The invention relates to the technical field of wastewater treatment, in particular to a process for recycling and reusing furan ammonium salt production wastewater.
Background
Cephalosporin antibiotics are the most widely anti-infective drugs in clinical application in recent years. Cefuroxime (including cefuroxime sodium and cefuroxime axetil) as a second generation cephalosporin is originally researched and developed by the Kudzuvine company in England, has the characteristics of broad-spectrum antibacterial activity and low toxic and side effects, has the resistance to gram-positive bacteria similar to that of the first generation cephalosporin, and has the sensitivity rate of over 95 percent; but the resistance to gram-negative bacteria is greatly enhanced, such as haemophilus influenzae, escherichia coli, salmonella, proteobacteria mirabilis, meningococcus and the like are sensitive, the medicine is basically nontoxic to kidney, and is mainly used for lower respiratory tract infection, osteoarticular infection and skin and soft tissue infection clinically, the ADME of cefuroxime in a human body is quick, the pharmacokinetics in vivo is a two-chamber open model, and no gender difference exists, when the cefuroxime and tazobactam are jointly used by taking 4; is a cephalosporin antibiotic which is well developed in recent years. (Z) -2-methoxyimino-2- (furan-2-yl) ammonium acetate is called furan ammonium salt for short, and is an important intermediate for producing cefuroxime.
A large amount of high-salinity high-chroma organic wastewater is generated in the production process of furan ammonium salt, the content of pollutants in the wastewater is generally high, the chroma is high, the components are complex, the environment is unbalanced in acid and alkali due to direct discharge, and a water body is polluted; the water quality mineralization is improved due to the fact that a large amount of inorganic salt is contained, direct discharge can cause more and more serious pollution to soil, surface water and underground water, and the ecological environment is endangered; the wastewater is directly distilled, and the fraction contains a large amount of low-boiling point refractory organic matters, so that the wastewater is difficult to biochemically treat. At the present stage, economic and effective treatment technology is still lacked for the wastewater, the wastewater is directly distilled in the traditional treatment process, the serious flooding phenomenon is generated in the distillation desalting process, the organic matter content of the obtained salt is high, and the requirement of byproduct salt cannot be met. Based on the statement, the invention provides a process for recycling furan ammonium salt production wastewater.
Disclosure of Invention
The invention aims to solve the problems that the treatment of the furaminium salt production wastewater in the prior art is lack of an economic and effective treatment technology, the traditional distillation treatment method is easy to cause a flooding phenomenon, the obtained salt content is high in organic matter content, the requirement of byproduct salt cannot be met, and the like, and provides a process for recycling the furaminium salt production wastewater.
A process for recycling furan ammonium salt production wastewater comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining, grinding, reacting with hydrochloric acid with the concentration of 22-32% for 2-3h, spraying the mixture in a mist form into a high-temperature atmosphere for thermal decomposition reaction, and carrying out post-treatment on the obtained reactant to obtain a settling agent;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.1-7, heating to 35-45 ℃, adding a sedimentation agent, stirring for 20-40min, standing, and filtering by a filter screen to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treated water into a sedimentation tank II, heating to 35-45 ℃, adding a sedimentation agent, stirring for 20-40min, standing, and filtering by a filter screen to obtain tertiary treated water;
and S5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent to adsorb after the reaction is finished, standing, filtering and distilling to finish the recycling process of the furan ammonium salt production wastewater.
Preferably, the calcination temperature in step S1 is 560 to 760 ℃.
Preferably, the mass ratio of the coal gangue to the hydrochloric acid in the step S1 is 1.5-2.5.
Preferably, the post-treatment step in step S1 specifically comprises the following operations: a. compounding silicic acid sol, glycidyl butyl ether and oleic acid polyethylene glycol ester to prepare a treatment fluid according to the mass ratio of 2-3; b. soaking the obtained reactant in the treatment solution, stirring at 68-75 deg.C and 350-450r/min for 8-15min, heating to 80-90 deg.C, stirring for 5-10min, drying, and pulverizing to obtain settling agent.
Preferably, the addition amount of the settling agent in the step S2 is 0.02-0.04% of the total amount of the furan ammonium salt production wastewater.
Preferably, the mesh number of the filter screen in the step S2 is 20-40 meshes, and the mesh number of the filter screen in the step S4 is 100-140 meshes.
Preferably, the adsorbent in the step S5 is prepared by compounding medical stone powder, bentonite and gallic acid according to the mass ratio of 1.
Preferably, the adding amount of the adsorbent in the step S5 is 0.008-0.012% of the total amount of the three-stage treated water.
The process for recycling and reusing the furan ammonium salt production wastewater provided by the invention has the following beneficial effects:
1. the invention utilizes two-stage sedimentation treatment in combination with anaerobic treatment, ozone oxidation, adsorbent adsorption, filtration and distillation means to carry out sedimentation, adsorption and separation on macromolecular organic matters such as furan ammonium salt, 2-acetylfuran and the like in the furan ammonium salt production wastewater, the salt content of the effluent treated by the procedures is as low as 2 percent, the COD value is obviously reduced, the effluent is clear and transparent, has no visible impurity and impurity, and can be used for daily production and life.
2. The invention adopts the solid waste coal gangue as the raw material, the raw material is simple and easy to obtain, the cost is low, the coal gangue is calcined and ground to react with hydrochloric acid, and then thermal decomposition and post treatment are carried out to obtain the settling agent, the obtained settling agent has good solubility and dispersibility and stable quality, can effectively adsorb suspended particles in the wastewater, realizes rapid settling, further accelerates the clarification of the wastewater and improves the filtering effect of the wastewater.
3. The adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid and is used for adsorption treatment of three-stage treated water; the adsorbent has the advantages of large specific surface area, strong activity, small using amount for water purification, strong decoloring capacity and simple separation and filtration; and the used adsorbent can be recycled by calcining, and is safe and environment-friendly.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 560 ℃, grinding, adding 22% hydrochloric acid according to a mass ratio of 1.5, reacting for 2 hours, spraying into a high-temperature atmosphere in a mist form to perform a thermal decomposition reaction, dipping the obtained reactant into a treatment solution, stirring at a temperature of 68 ℃ and a rotating speed of 350r/min for 8min, heating to 80 ℃, continuing stirring for 5min, drying, and crushing to obtain a settling agent, wherein the treatment solution is prepared by compounding silicic acid sol, glycidyl butyl ether and polyethylene glycol oleate according to a mass ratio of 2.1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.1, heating to 35 ℃, adding a sedimentation agent accounting for 0.02 percent of the total amount of the furan ammonium salt production wastewater, stirring for 20min, standing, and filtering by a filter screen with the mesh number of 20 to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treatment water into a sedimentation tank II, heating to 35 ℃, adding a sedimentation agent accounting for 0.01 percent of the total amount of the secondary treatment water, stirring for 20min, standing, and filtering through a filter screen with 80 meshes to obtain tertiary treatment water;
s5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.008% of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 110 meshes, and distilling to finish the recovery and reutilization process of the furan ammonium salt production wastewater, wherein the adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid with the mass ratio of 1.
Example two
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 660 ℃, grinding, adding 27% hydrochloric acid according to a mass ratio of 1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.5, heating to 40 ℃, adding a sedimentation agent accounting for 0.03 percent of the total amount of the furan ammonium salt production wastewater, stirring for 30min, standing, and filtering by a filter screen with 30 meshes to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treatment water into a sedimentation tank II, heating to 40 ℃, adding a sedimentation agent accounting for 0.012 percent of the total amount of the secondary treatment water, stirring for 30min, standing, and filtering by a filter screen with 90 meshes to obtain tertiary treatment water;
and S5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.01% of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 125 meshes, and distilling to finish the recovery and reutilization process of the furan ammonium salt production wastewater, wherein the adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid with the mass ratio of 1.
EXAMPLE III
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 760 ℃, grinding, adding 32% hydrochloric acid according to a mass ratio of 1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 7, heating to 45 ℃, adding a sedimentation agent accounting for 0.04 percent of the total amount of the furan ammonium salt production wastewater, stirring for 40min, standing, and filtering by a filter screen with 40 meshes to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treated water into a sedimentation tank II, heating to 45 ℃, adding a sedimentation agent accounting for 0.015% of the total amount of the secondary treated water, stirring for 40min, standing, and filtering by a filter screen with 100 meshes to obtain tertiary treated water;
and S5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.012 percent of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 140 meshes, and distilling to finish the recovery and reutilization process of the furan ammonium salt production wastewater, wherein the adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid with the mass ratio of 1.
Comparative example 1
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.5, heating to 40 ℃, adding a sedimentation agent accounting for 0.03 percent of the total amount of the furan ammonium salt production wastewater, stirring for 30min, standing, and filtering by a filter screen with 30 meshes to obtain primary treatment water, wherein the sedimentation agent is polyaluminium chloride;
s2, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s3, pumping the secondary treatment water into a sedimentation tank II, heating to 40 ℃, adding a sedimentation agent accounting for 0.012 percent of the total amount of the secondary treatment water, stirring for 30min, standing, and filtering by a filter screen with 90 meshes to obtain tertiary treatment water, wherein the sedimentation agent is polyaluminium chloride;
and S4, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.01% of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 125 meshes, and distilling to finish the recovery and reutilization process of the furan ammonium salt production wastewater, wherein the adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid with the mass ratio of 1.
Comparative example No. two
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 660 ℃, grinding, adding 27% hydrochloric acid according to a mass ratio of 1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.5, heating to 40 ℃, adding a sedimentation agent accounting for 0.03 percent of the total amount of the furan ammonium salt production wastewater, stirring for 30min, standing, and filtering by a filter screen with 30 meshes to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treatment water into a sedimentation tank II, heating to 40 ℃, adding a sedimentation agent accounting for 0.012 percent of the total amount of the secondary treatment water, stirring for 30min, standing, and filtering by a filter screen with 90 meshes to obtain tertiary treatment water;
s5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.01% of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 125, and distilling to finish the recycling process of the furan ammonium salt production wastewater, wherein the adsorbent is prepared by compounding medical stone powder, bentonite and gallic acid with the mass ratio of 1.
Comparative example No. three
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 660 ℃, grinding, adding 27% hydrochloric acid according to a mass ratio of 1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.5, heating to 40 ℃, adding a sedimentation agent accounting for 0.03 percent of the total amount of the furan ammonium salt production wastewater, stirring for 30min, standing, and filtering by a filter screen with 30 meshes to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treatment water into a sedimentation tank II, heating to 40 ℃, adding a sedimentation agent accounting for 0.012 percent of the total amount of the secondary treatment water, stirring for 30min, standing, and filtering by a filter screen with 90 meshes to obtain tertiary treatment water;
and S5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent accounting for 0.01% of the total amount of the three-stage treated water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 125, and distilling to finish the recycling process of the furan ammonium salt production wastewater, wherein the adsorbent is medical stone powder.
Comparative example No. four
The invention provides a process for recycling furan ammonium salt production wastewater, which comprises the following steps:
s1, taking solid waste coal gangue as a raw material, calcining at a high temperature of 660 ℃, grinding, adding 27% hydrochloric acid according to a mass ratio of 1;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.5, heating to 40 ℃, adding a sedimentation agent accounting for 0.03 percent of the total amount of the furan ammonium salt production wastewater, stirring for 30min, standing, and filtering by a filter screen with 30 meshes to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treatment water into a sedimentation tank II, heating to 40 ℃, adding a sedimentation agent accounting for 0.012 percent of the total amount of the secondary treatment water, stirring for 30min, standing, and filtering by a filter screen with 90 meshes to obtain tertiary treatment water;
and S5, carrying out ozone oxidation reaction on the tertiary treatment water, adding an adsorbent accounting for 0.01% of the total amount of the tertiary treatment water after the reaction is finished, adsorbing, standing, filtering by a filter screen with the mesh number of 125, and distilling to finish the recycling process of the furan ammonium salt production wastewater, wherein the adsorbent is bentonite.
The furaammonium salt production wastewater recovery and reuse process disclosed by the embodiment and the comparative example is utilized to purify the furaammonium salt production wastewater, wherein the COD concentration in the furaammonium salt production wastewater is 38000mg/L, the ammonia nitrogen concentration is 930mg/L, and the salt content is 22%.
The effluent quality after the recovery and reuse process of the furylammonium salt production wastewater of the first to third examples and the first to fourth comparative examples is respectively detected, and the following results are obtained:
table 1:
| detecting items | COD(mg/L) | Ammonia nitrogen (mg/L) | Salt content (%) |
| Example one | 3454 | 43.8 | 2 |
| Example two | 3312 | 39.2 | 1.8 |
| EXAMPLE III | 3519 | 46.5 | 2.3 |
| Comparative example 1 | 6630 | 109.5 | 8.7 |
| Comparative example No. two | 5715 | 87.7 | 5.3 |
| Comparative example No. three | 4865 | 64.1 | 3.6 |
| Comparative example No. four | 4560 | 61.9 | 3.9 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A process for recycling furan ammonium salt production wastewater is characterized by comprising the following steps:
s1, taking solid waste coal gangue as a raw material, calcining, grinding, reacting with hydrochloric acid with the concentration of 22-32% for 2-3h, spraying the mixture in a mist form into a high-temperature atmosphere for thermal decomposition reaction, and carrying out post-treatment on the obtained reactant to obtain a settling agent;
s2, pumping the furan ammonium salt production wastewater into a sedimentation tank I, adjusting the pH value to 6.1-7, heating to 35-45 ℃, adding a sedimentation agent, stirring for 20-40min, standing, and filtering by a filter screen to obtain primary treatment water;
s3, feeding the primary treated water and a nutrient source required by anaerobic treatment into an EGSB anaerobic reactor for anaerobic reaction, and filtering by using a biomembrane filtration method after the reaction is finished to obtain secondary treated water;
s4, pumping the secondary treated water into a sedimentation tank II, heating to 35-45 ℃, adding a sedimentation agent, stirring for 20-40min, standing, and filtering by a filter screen to obtain tertiary treated water;
s5, carrying out ozone oxidation reaction on the three-stage treated water, adding an adsorbent to adsorb after the reaction is finished, standing, filtering and distilling to finish the recycling process of the furan ammonium salt production wastewater;
the calcination temperature in the step S1 is 560-760 ℃;
the mass ratio of the coal gangue to the hydrochloric acid in the step S1 is 1.5-2.5;
the post-treatment process in step S1 specifically operates as follows: a. compounding silicic acid sol, glycidyl butyl ether and oleic acid polyethylene glycol ester according to the mass ratio of 2-3; b. soaking the obtained reactant in the treatment solution, stirring at 68-75 deg.C and 350-450r/min for 8-15min, heating to 80-90 deg.C, stirring for 5-10min, drying, and pulverizing to obtain settling agent;
the addition amount of the sedimentation agent in the step S2 is 0.02-0.04% of the total amount of the furan ammonium salt production wastewater, and the addition amount of the sedimentation agent in the step S4 is 0.01-0.015% of the total amount of the secondary treatment water.
2. The process for recycling furan ammonium salt production wastewater according to claim 1, wherein the mesh number of the filter screen in the step S2 is 20-40 meshes; in the step S4, the mesh number of the filter screen is 80-100 meshes; the mesh number of the filter screen in the step S5 is 110-140 meshes.
3. The process for recycling and reusing furan ammonium salt production wastewater according to claim 1, wherein the adsorbent in the step S5 is prepared by compounding medical stone powder, bentonite and gallic acid in a mass ratio of 1.
4. The process for recycling and reusing furaminium salt production wastewater as claimed in claim 1, wherein the addition amount of the adsorbent in the step S5 is 0.008-0.012% of the total amount of the tertiary treatment water.
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| CN110980860A (en) * | 2019-12-19 | 2020-04-10 | 广州欧邦联合建材有限公司 | Wastewater treatment agent and preparation method thereof |
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| US4298732A (en) * | 1978-01-17 | 1981-11-03 | Glaxo Group Limited | Crystallization process |
| CN101823721A (en) * | 2010-03-19 | 2010-09-08 | 合肥学院 | Method for producing poly silicate aluminium ferric flocculating agent by utilizing coal gangue |
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