CN113562833A - Method for efficiently and continuously treating culture pollutants by using microreactor - Google Patents
Method for efficiently and continuously treating culture pollutants by using microreactor Download PDFInfo
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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Abstract
本申请公开了一种利用微反应器连续高效处理水污染物的方法。该方法包括将待处理液体和氧化性气体共同通入装填有固相物质的微反应器，发生化学反应，得到净化液体；其中，所述待处理液体含有养殖污染物；所述氧化性气体中含有臭氧。该方法利用微反应器来降解养殖污染物，通过提高气液传质速率，可以显著提高臭氧降解养殖污染物的效率。The present application discloses a method for continuously and efficiently treating water pollutants by utilizing a microreactor. The method includes passing the liquid to be treated and the oxidizing gas together into a microreactor filled with solid-phase substances, and a chemical reaction occurs to obtain a purified liquid; wherein, the liquid to be treated contains aquaculture pollutants; the oxidizing gas contains Contains ozone. The method utilizes a microreactor to degrade aquaculture pollutants, and can significantly improve the efficiency of ozone degradation of aquaculture pollutants by increasing the gas-liquid mass transfer rate.
Description
Technical Field
The application relates to a method for continuously and efficiently treating water pollutants by utilizing a microreactor, belonging to the technical field of environmental purification.
Background
In recent years, with the rapid development of the breeding industry in China, the product quality is increasingly affected by harmful factors (persistent organic pollutants, endocrine disruptors and the like) and input products (pesticides, veterinary drugs, bactericides, antibiotics, fertilizer regulators, water regulators and the like) in the breeding environment. These recalcitrant pollutants are toxic, carcinogenic, teratogenic and mutagenic, and not only are they harmful to the environment and animals and plants, but also present potential hazards to humans. At present, the technologies for treating aquaculture wastewater mainly comprise physical treatment technologies (such as filtration technology, adsorption technology and extraction technology), chemical treatment technologies (electrochemical oxidation technology, ozone technology and Fenton oxidation technology) and biological treatment technologies (such as an activated sludge method and a biofilm method). Among degradation methods of difficultly degradable pollutants, the ozone oxidation degradation method is widely applied because of less harmful decomposition intermediate products and strong ozone oxidation capacity (oxidation potential 2.08 v).
Ozone is a green, pollution-free, effective oxidant. Ozone oxidation degradation of refractory pollutants generally involves two mechanisms: direct ozone oxidation and indirect ozone oxidation. At lower pH values, ozone reacts selectively in molecular form with compounds having specific functional groups, such as aromatic compounds (direct ozone oxidation). On the other hand, under alkaline and catalytic conditions, ozone can decompose into hydroxyl radicals (. OH) having a higher oxidation potential than ozone molecules (indirect ozone oxidation). Especially in the presence of a catalyst, the utilization rate and the reaction rate of the ozone are greatly improved.
However, ozone (or hydroxyl radicals) reacts with contaminants quickly and the rate of dissolution of the liquid by the ozone greatly limits the rate of reaction. In addition, ozone is easily decomposed (ozone decomposition rate constant: 7.32X 10)-4s-1The temperature is 20 ℃, the initial pH value is 7, the ozone concentration in water is 8mg/L), and if the reaction time is longer, the ozone utilization efficiency is reduced. Therefore, the efficiency of oxidative degradation of pollutants by ozone alone is not high in the prior art.
Disclosure of Invention
According to one aspect of the application, a method for treating aquaculture pollutants is provided, the method utilizes a micro-reactor to strengthen gas-liquid mass transfer to rapidly degrade refractory pollutants in aquaculture, and can remarkably improve the utilization rate of ozone and improve the efficiency of pollutant degradation.
A method for continuously and efficiently treating water pollutants by utilizing a microreactor comprises the steps of introducing liquid to be treated and oxidizing gas into the microreactor filled with solid-phase substances together, and carrying out chemical reaction to obtain purified liquid; wherein the liquid to be treated contains contaminants; the oxidizing gas contains ozone.
Specifically, liquid to be treated is contacted with a solid-phase substance in an oxidizing gas environment and reacts to obtain purified liquid; wherein the liquid to be treated contains contaminants; the oxidizing gas contains ozone.
In the application, the liquid to be treated containing pollutants is a liquid phase, the oxidizing gas containing ozone is a gas phase, and the liquid is cooperated with a solid phase substance to realize degradation of the pollutants difficult to degrade in the culture under the action of a microreactor.
Optionally, the micro-channels in the microreactors in the present application have a radial dimension of 5 to 800 μm.
After the solid-phase substance is accumulated in the microreactor, a certain porosity can be formed, so that the liquid phase and the gas phase can flow conveniently.
Preferably, the porosity after the solid-phase substance is deposited is 30 to 40%.
Optionally, the solid phase material comprises at least one of inert particles, active particles;
wherein the inert particles are solid particles without catalytically active centers;
the active particles are solid particles having catalytically active centers.
Preferably, the particle size of the solid phase substance is 100-1500 μm.
Optionally, the inert particles comprise at least one of ceramic particles, plastic particles, metal particles.
Specifically, for example, the ceramic particles include any one of zirconia ceramic particles, silicon nitride ceramic particles, and aluminum nitride ceramic particles.
For example, the plastic particles include any one of polyethylene plastic particles, polypropylene plastic particles, and polyvinyl chloride plastic particles.
For example, the metal particles include any one of carbon steel metal particles and stainless steel metal particles.
Optionally, the active particles comprise at least one of molecular sieves, activated carbon, metal oxides.
Specifically, for example, the molecular sieve includes any of natural zeolite, synthetic zeolite.
The metal oxide includes, for example, any of alumina, silica, ferroferric oxide, copper-manganese-supported alumina, and manganese-oxide-supported alumina.
Optionally, the contaminants include aquaculture contaminants.
Specifically, the culture pollutants in the present application refer to pollutants that are generated in the culture production process and have adverse effects on the environment, animals and plants, and even human beings. The micro-reactor degradation method has good effect.
Optionally, the organic contaminant comprises any one of a phenolic compound, a nitrogen-containing aromatic compound.
Optionally, the phenolic compound comprises any one of phenol, nonylphenol, bisphenol a, diethylstilbestrol.
Optionally, the nitrogen-containing aromatic compound is selected from any one of a bactericide aromatic compound and an antibiotic aromatic compound.
Optionally, the germicide aromatic compound comprises any one of malachite green, sulfadiazine, sulfathiazole and amitraz.
Optionally, the antibiotic aromatic compound comprises any one of norfloxacin, enrofloxacin, ciprofloxacin, chloramphenicol, amoxicillin.
Optionally, the oxidizing gas further comprises oxygen.
Specifically, the oxidizing gas in the present application may be a mixed gas of ozone and oxygen, or may be a mixed gas of ozone and an inert gas.
Optionally, the conditions of the reaction include:
the concentration of the pollutants in the liquid to be treated is 50-1000 mg/L;
the concentration of the ozone in the oxidizing gas is 25-130 mg/L;
the pH value of the liquid to be treated is 4-11.
Specifically, the upper limit of the concentration of the contaminant in the liquid to be treated is independently selected from the group consisting of 60mg/L, 200mg/L, 400mg/L, 500mg/L, 600mg/L, 800mg/L, 1000 mg/L; the lower limit of the concentration of the contaminant in the liquid to be treated is independently selected from the group consisting of 50mg/L, 200mg/L, 400mg/L, 500mg/L, 600mg/L, 800mg/L, 950 mg/L.
Preferably, the concentration of the pollutants in the liquid to be treated is 60-600 mg/L.
Further preferably, the concentration of the pollutants in the liquid to be treated is 60-500 mg/L.
Specifically, the upper limit of the concentration of ozone in the oxidizing gas is independently selected from 41mg/L, 60mg/L, 84mg/L, 102mg/L, 128 mg/L; the lower limit of the concentration of ozone in the oxidizing gas is independently selected from the group consisting of 25mg/L, 41mg/L, 60mg/L, 84mg/L, and 102 mg/L.
Preferably, the concentration of ozone in the oxidizing gas is 84mg/L to 128 mg/L.
Further preferably, the concentration of ozone in the oxidizing gas is 100mg/L to 128 mg/L.
Specifically, the pH of the liquid to be treated is the initial pH of the liquid to be treated.
The liquid to be treated may be acidic, or neutral, or basic.
Preferably, the liquid to be treated is alkaline.
Optionally, the value range of the pH of the liquid to be treated is 4 or more and less than 7.
Optionally, the value range of the pH of the liquid to be treated is 7 or more and less than 8.
Optionally, the value range of the pH of the liquid to be treated is more than or equal to 8 and less than 11.
Preferably, the value range of the pH of the liquid to be treated is 9-11.
Preferably, the conditions of the reaction include:
the concentration of the pollutants in the liquid to be treated is 60-600 mg/L;
the concentration of the ozone in the oxidizing gas is 80-130 mg/L;
the pH value of the liquid to be treated is 8-11.
Optionally, the volume space velocity of the liquid to be treated is 11-56 h-1；
The volume space velocity of the oxidizing gas is 560-2804 h-1。
Optionally, the method comprises: respectively and continuously introducing the oxidizing gas and the liquid to be treated into the microreactor, and reacting to obtain purified liquid;
wherein the microreactor contains the solid-phase substance.
The method aims to provide a method for degrading difficultly-degraded culture pollutants by using a microreactor, and the optimal operating conditions for degrading phenol by using a microreactor system are as follows: the liquid volume space velocity is 11-12 h-1The gas volume space velocity is 1400-1410 h-1Initial pH of 10.5 to 11.5, initial O3The concentration is 100-128 mg/L. For inert particles, the method can realize the effects that the removal rate of organic matters is more than 99 percent and the removal rate of COD is more than 40 percent; for active particles, the method can realize the effects that the removal rate of organic matters is more than 99 percent and the removal rate of COD is more than 70 percent.
The beneficial effects that this application can produce include:
1) the application discloses a method for continuously ozonizing and degrading refractory culture pollutants in a microreactor.
2) The micro-reactor system is adopted to treat the pollutants difficult to degrade, and has the advantages of easy control of the reaction process, high efficiency, clean environment and high safety. The results show that the micro-reactor is a promising approach for treating the pollutants difficult to degrade.
Drawings
Fig. 1 is a schematic structural view of a pollutant treating device.
Reference numerals:
1 an ozone generator; 2, a microreactor; 3 an outlet phase separation tank.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The device for treating the culture pollutants is shown in figure 1, and comprises an ozone generator 1, a micro-reactor 2 filled with solid-phase substances and an outlet phase-splitting tank 3;
firstly, an ozone generator 1 generates ozone, the ozone is introduced into a microreactor 2 containing solid particle fillers, meanwhile, liquid to be treated containing pollutants is introduced into the microreactor 2 to generate ozonization reaction, a gas-liquid mixture after the reaction enters a gas-liquid phase separation tank 3 to carry out gas-liquid separation, the unreacted ozone is destroyed by a destruction device to generate oxygen, and the solution is purified liquid after treatment.
In this example, a solution to be treated containing phenol (water is used as a solvent) and an oxidizing gas containing ozone are introduced into a microreactor, and contact reaction is carried out with a solid filler in the microreactor, so as to obtain a purified liquid.
The particle size of the zirconia ceramic bead in the embodiment of the application is 500-580 μm;
Gamma-Al in the examples of the present application2O3The particle size of the particles is 500-580 μm.
EXAMPLE 1 Effect of liquid volumetric space velocity
The experimental conditions are as follows: initial phenol concentration 500mg/L, initial COD 1450mg/L, initial ozone concentration 100mg/L, pH7, microreactor packing: zirconia ceramic beads. Liquid volume space velocity of 11.2, 22.4, 33.6, 44.8 and 56.1h-1The corresponding residence times are 195, 97.2, 64.8, 48.6, 39 s. Volumetric space velocity of oxidizing gas 1402h-1。
Test results, as shown in Table 1Residence time with liquid volume space velocity (11.2-56.1 h)-1) The increase of the amount of the phenol is continuously reduced, and the removal rate of the phenol and the COD is also continuously reduced. The liquid volume space velocity is 11.2h-1In the process, the phenol removal rate and the COD removal rate reach the maximum values, and are respectively 99.85 percent and 56.57 percent.
TABLE 1 influence of different liquid volume space velocities on phenol and COD removal rates
Example 2 Effect of initial pH
The experimental conditions are as follows: the initial phenol concentration is 500mg/L, the initial COD is 1450mg/L, the initial ozone concentration is 100mg/L, and the liquid volume space velocity is 28h-1Volumetric space velocity of oxidizing gas 1402h-1And filling a micro-reactor: zirconia ceramic beads.
Table 2 shows that the removal rate of phenol and COD increases with the initial pH (pH 4-11). At an initial pH of 11, the phenol and COD removal rates reached maximum values of 99.67% and 54.09%, respectively.
TABLE 2 Effect of different initial pH on phenol and COD removal rates
EXAMPLE 3 Effect of initial ozone concentration
The experimental conditions are as follows: the initial phenol concentration is 500mg/L, the initial COD is 1450mg/L, and the liquid volume space velocity is 28h-1Volumetric space velocity of oxidizing gas 1402h-1pH7, microreactor packing: zirconia ceramic beads.
The results in Table 3 show that the removal rate of phenol and COD increases with increasing initial ozone concentration (25-128 mg/L). When the initial concentration of ozone reaches 128mg/L, the removal rates of phenol and COD reach the highest values, namely 94.68% and 38.63% respectively.
TABLE 3 Effect of different initial ozone concentrations on phenol and COD removal rates
Example 4 Effect of initial phenol concentration
The experimental conditions are as follows: initial ozone concentration of 100mg/L and liquid volume space velocity of 28h-1Volumetric space velocity of oxidizing gas 1402h-1pH7, microreactor packing: zirconia ceramic beads.
The results in Table 4 show that the removal rate of phenol and COD decreased with increasing initial phenol concentration (98-627 mg/L). When the initial phenol concentration was increased from 400 to 627mg/L, the COD removal rate hardly changed.
TABLE 4 Effect of different initial phenol concentrations on phenol and COD removal rates
Example 5 Effect of solid Filler particles
The experimental conditions are as follows: the initial phenol concentration is 500mg/L, the initial COD is 1450mg/L, the initial ozone concentration is 100mg/L, and the liquid volume space velocity is 28h-1Volumetric space velocity of oxidizing gas 1402h-1pH7, microreactor packing: zirconia ceramic beads or gamma-Al2O3And (4) a small ball. Residence time: 78 s.
The results are shown in table 5, which indicates that the removal rate of phenol and COD is higher for the alumina pellets as the filler than for the zirconia ceramic beads as the filler. And compared with the filler of zirconia ceramic beads, the removal rate of COD (chemical oxygen demand) of the filler of alumina pellets is improved by 10-30%.
TABLE 5 Effect of different solid Filler particles on phenol and COD removal
Example 6 ozonation treatment of typical aquaculture contaminants
The experimental conditions are as follows: the initial pollutant concentration is 500mg/L, the initial ozone concentration is 100mg/L, and the liquid volume space velocity is 11.2h-1Corresponding to a residence time of 195s, an initial contaminant pH of 7, an ozone volume space velocity of 1402h-1And filling a micro-reactor: zirconia ceramic beads, activated alumina pellets (gamma-Al)2O3)。
In this example, typical aquaculture contaminants that were treated included: phenol, bisphenol A, nonyl phenol, diethylstilbestrol, malachite green, sulfadiazine, sulfathiazole, norfloxacin, enrofloxacin, ciprofloxacin, chloramphenicol and amoxicillin.
To demonstrate the versatility of the entire microreactor-centric system, we treated typical aquaculture contaminants including phenolic compounds, bactericidal aromatic compounds, antibiotic aromatic compounds with the entire system. The results in Table 6 show that the COD removal rates of different organic pollutants are 10-30% higher when alumina pellets are used as the filler than when zirconia ceramic beads are used as the filler. Moreover, the removal rate of different organic pollutants almost reaches 100 percent.
TABLE 6 removal rates of several typical aquaculture pollutants and COD removal rates
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A method for continuously and efficiently treating water pollutants by utilizing a microreactor is characterized in that liquid to be treated and oxidizing gas are introduced into the microreactor filled with solid-phase substances together to perform chemical reaction to obtain purified liquid;
wherein the liquid to be treated contains contaminants;
the oxidizing gas contains ozone.
2. The method of claim 1, wherein the solid phase material comprises at least one of inert particles, active particles;
wherein the inert particles are solid particles without catalytically active centers;
the active particles are solid particles having catalytically active centers.
3. The method of claim 2, wherein the inert particles comprise at least one of ceramic particles, plastic particles, metal particles;
the active particles comprise at least one of molecular sieve, activated carbon and metal oxide.
4. The method according to claim 1, wherein the solid phase material has a particle size of 100 to 1500 μm.
5. The method of claim 1, wherein the contaminants comprise aquaculture contaminants.
6. The method of claim 5, wherein the farming contaminants comprise any of phenolic compounds, nitrogen-containing aromatic compounds;
preferably, the phenolic compound comprises any one of phenol, nonyl phenol, bisphenol a and diethylstilbestrol;
preferably, the aromatic compound containing nitrogen is selected from any one of aromatic compounds of bactericides and aromatic compounds of antibiotics;
further preferably, the bactericide aromatic compound includes any one of malachite green, sulfadiazine, sulfathiazole, and the like;
the antibiotic aromatic compound comprises any one of norfloxacin, enrofloxacin, ciprofloxacin, chloramphenicol, amoxicillin and the like.
7. The method according to claim 1, wherein the oxidizing gas further contains at least one of oxygen and an inert gas.
8. The method of claim 1, wherein the reaction conditions comprise:
the concentration of the pollutants in the liquid to be treated is 50-1000 mg/L;
the concentration of the ozone in the oxidizing gas is 25-130 mg/L;
the pH value of the liquid to be treated is 4-11.
9. The method of claim 1, wherein the reaction conditions comprise:
the concentration of the pollutants in the liquid to be treated is 60-600 mg/L;
the concentration of the ozone in the oxidizing gas is 80-130 mg/L;
the pH value of the liquid to be treated is 8-11.
10. The method according to claim 1, wherein the volume space velocity of the liquid to be treated is 11-56 h-1；
The volume space velocity of the oxidizing gas is 560-2804h-1。
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Cited By (1)
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| CN116655098A (en) * | 2023-08-01 | 2023-08-29 | 中建安装集团有限公司 | A kind of method of microbubble ozone catalytic oxidation degradation phenol |
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Application publication date: 20211029 |