CN108906108B - A Microwave Synthesis Process of N-SrTiO3/Activated Carbon Treated Materials and Its Application - Google Patents
A Microwave Synthesis Process of N-SrTiO3/Activated Carbon Treated Materials and Its Application Download PDFInfo
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Abstract
本发明涉及一种N‑SrTiO3/活性炭处理材料的微波法合成工艺及其应用，该工艺以活性炭为载体，N‑SrTiO3光催化剂为活性组分，采用微波法在活性炭上负载一定量的光催化剂以制备N‑SrTiO3/活性炭复合物，新型材料用于电镀废水中重金属及COD的处理具有高效、原料廉价易得、易分离、可重复利用、不会产生二次污染等优点。本发明利用高比表面积的活性炭作为光催化剂的载体，微波法合成高比表面积的N‑SrTiO3/活性炭处理材料，同时微波法可大大缩短反应时间，提高材料催化性能；此外，活性炭上负载掺杂N改性后的SrTiO3，两者具有协同效应，重金属及COD的处理效果好，N‑SrTiO3/活性炭处理材料的稳定性高；本发明工艺制备过程简单易控，具有很好的经济效益。The invention relates to a microwave method synthesis process of N-SrTiO 3 /activated carbon treatment material and its application. The process uses activated carbon as a carrier, an N-SrTiO 3 photocatalyst as an active component, and uses a microwave method to load a certain amount of activated carbon on the activated carbon. The photocatalyst is used to prepare N-SrTiO 3 /activated carbon composites. The new material is used for the treatment of heavy metals and COD in electroplating wastewater, which has the advantages of high efficiency, cheap and easily available raw materials, easy separation, reusability, and no secondary pollution. In the invention, the activated carbon with high specific surface area is used as the carrier of the photocatalyst, and the N-SrTiO 3 /activated carbon treatment material with high specific surface area is synthesized by the microwave method. Meanwhile, the microwave method can greatly shorten the reaction time and improve the catalytic performance of the material; The SrTiO 3 modified by hetero-N has a synergistic effect, the treatment effect of heavy metals and COD is good, and the stability of the N-SrTiO 3 /activated carbon treatment material is high; the preparation process of the invention is simple and easy to control, and has good economical efficiency. benefit.
Description
Technical Field
The invention belongs to the technical field of wastewater treatment, relates to preparation of a novel composite material for wastewater treatment, and particularly relates to N-SrTiO3Microwave synthesis process of active carbon treated material and its application.
Background
The active carbon is an excellent adsorbent with a highly developed pore structure and stable physicochemical properties. It is made up by using carbon-rich organic material, such as charcoal, high-quality coal and fruit shell, and making them pass through the processes of catalytic activation at high temp. and under a certain pressure. The inside of the active carbon is provided with a plurality of tiny pores which are communicated in a staggered way, and the pore diameter is 1 multiplied by 10-10μm～ 1×10-6μ m, which makes the specific surface area of the activated carbon as high as 1000m2Above/g, the developed pore structure is the main reason that the activated carbon has strong adsorption performance. In recent years, activated carbon, which is a high-tech, environmentally friendly engineering material, has been gradually applied to the purification of water and air, and the treatment of organic pollutants, and in general, activated carbon is mainly used for the final advanced treatment process. The method for removing heavy metal ions and COD in industrial wastewater by using the activated carbon adsorption technology is increasingly widely applied at home and abroad, and the process has the advantages of simple equipment, small occupied area, no secondary pollution and the like.
In addition, the photocatalysis technology is a novel advanced catalytic oxidation technology, and can oxidize and degrade various organic matters such as benzene series, chlorine-containing compounds, synthetic dyes, surfactants, pesticides and the like in water and reduce heavy metal ions such as lead, chromium, platinum, gold and the like in the water. Has the advantages of simple operation, low cost, high degradation rate, mild reaction conditions, no secondary pollution and the like, and is a novel green energy-saving water pollutionAnd (4) processing technology. Modification of photocatalyst SrTiO by N doping3The method can effectively improve the catalytic activity of the photocatalyst.
The active carbon is used as a catalyst carrier, and other catalysts such as metal oxide and the like are loaded on the surface of the active carbon, the catalyst efficiency of the catalysts such as the active carbon, the metal oxide and the like can be improved. The activated carbon is used as an electron acceptor, electrons generated by the photocatalyst are transferred to pollutants, so that the effect of degradation is achieved, and the synergistic effect of the activated carbon and the photocatalyst in wastewater treatment can effectively adsorb heavy metal and COD (chemical oxygen demand) and can also achieve the effect of strengthening catalytic degradation to treat wastewater.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides N-SrTiO3The microwave synthesis process has the advantages of simple operation, low cost, high degradation rate, mild reaction condition, no secondary pollution and the like, and can greatly shorten the reaction time and improve the catalytic performance of the material by adopting the microwave synthesis method.
N-SrTiO3The microwave synthesis process of the active carbon treatment material comprises the following steps:
(1) dissolving tetrabutyl titanate in isopropanol, and marking as a solution a; dissolving strontium nitrate in distilled water, and marking as a solution b; dropwise adding the solution b into the solution a under stirring, adding a mineralizer and an N source, and stirring and dissolving to obtain a mixed solution;
(2) weighing a certain proportion of active carbon according to the loading amount of the photocatalyst, uniformly dispersing the active carbon in the mixed solution, stirring and reacting in a microwave reactor, washing and drying after the reaction to obtain the N-SrTiO3Activated carbon treatment material.
The process of the invention uses active carbon as a carrier and N-SrTiO3The photocatalyst is an active component, and a certain amount of photocatalyst is loaded on the active carbon by adopting a microwave method to prepare the N-SrTiO3The invention adopts a microwave reactor, which not only can greatly shorten the reaction time, but also can improve the catalytic performance of the material.
Preferably, in the step (1), the molar ratio of tetrabutyl titanate to strontium nitrate is 1: 0.9 to 1.2.
Preferably, in the step (1), the mineralizer is a potassium hydroxide aqueous solution, the N source is hexamethylenetetramine, and the stirring time is 0.5-2 h.
Preferably, in the step (2), the activated carbon is soaked in 1M nitric acid for 0.5-1 h, and the specific surface area is 1200-1500M2/g。
Preferably, the loading amount of the photocatalyst in the step (2) is 1-10 wt%.
Preferably, the microwave reaction temperature in the step (2) is 100-180 ℃, and the reaction time is 5-20 min.
Preferably, the photocatalyst SrTiO in the step (2)3Is a material modified by N doping, and the specific surface area of the N-SrTiO 3/active carbon processing material is 1000-1500 m2/g。
The invention also provides the N-SrTiO prepared by the process3Application of activated carbon treatment material in wastewater treatment.
Preferably, the application comprises the following steps: taking a certain amount of electroplating wastewater from an electroplating plant, adding a certain mass of N-SrTiO3Active carbon treatment material, analysis and detection adding N-SrTiO3The concentrations of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material; wherein the N-SrTiO3The volume ratio of the mass of the active carbon treatment material to the electroplating wastewater is 1-5 g: 1L of the compound.
Preferably, the N-SrTiO compound3Use of an activated carbon treatment material comprising the steps of:
(1) dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; dropwise adding the solution b into the solution a under stirring, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g hexamethylene tetramine as a doped N source, and stirring and dissolving to obtain a mixed solution;
(2) weighing active carbon according to the loading amount of the photocatalyst of 5wt%, uniformly dispersing the active carbon in the mixed solution, and stirring the active carbon in a microwave reactor at 100 DEG CStirring and reacting for 20min, washing the product with ethanol, and drying in a forced air drying oven at 60 deg.C for 24 hr to obtain N-SrTiO3An activated carbon treatment material;
(3) 3g of N-SrTiO is added into electroplating wastewater of a 1L electroplating plant3Active carbon treatment material, analysis and detection adding N-SrTiO3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material.
The invention utilizes the active carbon with high specific surface area as the carrier of the photocatalyst and synthesizes the N-SrTiO with high specific surface area by a microwave method3The material is treated by the active carbon, so that the synthesis period is greatly shortened, and the catalytic performance of the material is improved; in addition, the active carbon is loaded with modified SrTiO doped with N3The two have synergistic effect, the treatment effect of heavy metal and COD is good, and N-SrTiO3The stability of the active carbon treatment material is high.
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of the invention.
Example 1
N-SrTiO3Preparation of activated carbon treatment material: dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; and (3) under the condition of violent stirring, dropwise adding the solution b into the solution a, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g of hexamethylenetetramine as a doped N source, and stirring and dissolving to obtain a mixed solution. Weighing the activated carbon according to the proportion that the loading capacity of the photocatalyst is 10 wt%, uniformly dispersing the activated carbon in the mixed solution, violently stirring and reacting for 20min at 100 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain the N-SrTiO3Activated carbon treatment material.
And (3) treating wastewater: 1g of treating agent is added into 1L of electroplating wastewater of a certain electroplating plant in Linan City, and N-SrTiO is added for analysis and detection3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material. The results show that the removal rate of chromium ions reaches 93.5 percent, the removal rate of cadmium ions reaches 91.1 percent and the removal rate of CODThe removal rate reaches 83.4 percent.
Example 2
N-SrTiO3Preparation of activated carbon treatment material: dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; and (3) under the condition of violent stirring, dropwise adding the solution b into the solution a, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g of hexamethylenetetramine as a doped N source, and stirring and dissolving to obtain a mixed solution. Weighing activated carbon according to the proportion that the loading capacity of the photocatalyst is 1 wt%, uniformly dispersing the activated carbon in the mixed solution, violently stirring and reacting for 5min at 180 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain the N-SrTiO3Activated carbon treatment material.
And (3) treating wastewater: 1g of treating agent is added into 1L of electroplating wastewater of a certain electroplating plant in Linan City, and N-SrTiO is added for analysis and detection3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material. The results show that the removal rate of chromium ions reaches 91.4%, the removal rate of cadmium ions reaches 90.2%, and the removal rate of COD reaches 85.3%.
Example 3
N-SrTiO3Preparation of activated carbon treatment material: dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; and (3) under the condition of violent stirring, dropwise adding the solution b into the solution a, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g of hexamethylenetetramine as a doped N source, and stirring and dissolving to obtain a mixed solution. Weighing active carbon according to the photocatalyst loading amount of 5wt%, uniformly dispersing in the mixed solution, violently stirring and reacting for 15min at 160 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain the N-SrTiO3Activated carbon treatment material.
And (3) treating wastewater: 1g of treating agent is added into 1L of electroplating wastewater of a certain electroplating plant in Linan City, and N-SrTiO is added for analysis and detection3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material.The results show that the removal rate of chromium ions reaches 96.3%, the removal rate of cadmium ions reaches 93.5%, and the removal rate of COD reaches 87.1%.
Example 4
N-SrTiO3Preparation of activated carbon treatment material: dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; and (3) under the condition of violent stirring, dropwise adding the solution b into the solution a, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g of hexamethylenetetramine as a doped N source, and stirring and dissolving to obtain a mixed solution. Weighing active carbon according to the photocatalyst loading amount of 5wt%, uniformly dispersing in the mixed solution, violently stirring and reacting for 15min at 160 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain the N-SrTiO3Activated carbon treatment material.
And (3) treating wastewater: adding 3g of N-SrTiO into 1L of electroplating wastewater of a certain electroplating plant in Linan City3Active carbon treatment material, analysis and detection adding N-SrTiO3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material. The results show that the removal rate of chromium ions reaches 99.8%, the removal rate of cadmium ions reaches 99.5%, and the removal rate of COD reaches 90.1%.
Example 5
N-SrTiO3Preparation of activated carbon treatment material: dissolving 3.40g of tetrabutyl titanate in 100ml of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100ml of distilled water, and marking as a solution b; and (3) under the condition of violent stirring, dropwise adding the solution b into the solution a, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g of hexamethylenetetramine as a doped N source, and stirring and dissolving to obtain a mixed solution. Weighing active carbon according to the photocatalyst loading amount of 5wt%, uniformly dispersing in the mixed solution, violently stirring and reacting for 15min at 160 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain the N-SrTiO3Activated carbon treatment material.
And (3) treating wastewater: adding 5g of N into electroplating wastewater of a certain electroplating plant in 1L of Linan City-SrTiO3Active carbon treatment material, analysis and detection adding N-SrTiO3Concentration of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material. The results show that the removal rate of chromium ions reaches 99.9%, the removal rate of cadmium ions reaches 99.7%, and the removal rate of COD reaches 90.3%.
Comparative example 1
N-SrTiO3Preparation of activated carbon treatment Material similar to the procedure of example 1, but using hydrothermal method to react in an air-blast drying oven at 160 deg.C for 180min with photocatalyst load of 5wt%, the rest steps being the same, N-SrTiO was obtained3Active carbon treating agent.
And (3) treating wastewater: adding 3g of treating agent into 1L of electroplating wastewater of a certain electroplating plant in Linan City, analyzing and detecting the added N-SrTiO3The concentrations of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment agent. The results showed that the removal rate of chromium ions was 83.1%, the removal rate of cadmium ions was 80.5%, and the removal rate of COD was 72.1%.
Comparative example 2
3g of activated carbon is added into 1L of electroplating wastewater of a certain electroplating plant in Linan City, and the concentrations of heavy metal ions and COD in the electroplating wastewater before and after the addition of the activated carbon treatment agent are analyzed and detected. The results show that the removal rate of chromium ions reaches 73.2%, the removal rate of cadmium ions reaches 71.3%, and the removal rate of COD reaches 53.3%.
Comparative example 3
N-SrTiO3The procedure of preparation example 1 was similar, except that no activated carbon was added, the reaction temperature was 160 deg.C, the reaction time was 15min, and the remaining steps were the same, to obtain N-SrTiO3And (3) sampling.
Adding 3g of N-SrTiO into 1L of electroplating wastewater of a certain electroplating plant in Linan City3Adding N-SrTiO for analysis and detection3The concentrations of heavy metal ions and COD in the electroplating wastewater before and after the treatment agent. The results show that the removal rate of chromium ions reaches 62.6%, the removal rate of cadmium ions reaches 54.5%, and the removal rate of COD reaches 62.5%.
The process conditions and results of examples 1 to 5 and comparative examples 1 to 3 are shown in Table 1:
TABLE 1
The treatment material is used for treating heavy metal and COD in electroplating wastewater, has the advantages of high efficiency, cheap and easily available raw materials, easy separation, reusability, no secondary pollution and the like, and can greatly shorten the reaction time and improve the catalytic performance of the material by a microwave method; the preparation process of the invention is simple and easy to control, and has good economic benefit.
Claims (1)
1. N-SrTiO3The application of the active carbon treatment material in adsorbing wastewater is characterized in that: the N-SrTiO3The activated carbon treatment material is prepared by the following steps:
(1) dissolving 3.40g of tetrabutyl titanate in 100mL of isopropanol, and marking as a solution a; dissolving 2.21g of strontium nitrate in 100mL of distilled water, and marking as a solution b; dropwise adding the solution b into the solution a under stirring, taking 0.1M potassium hydroxide aqueous solution as a mineralizer, adding 0.28g hexamethylene tetramine as a doped N source, and stirring and dissolving to obtain a mixed solution;
(2) weighing active carbon according to the photocatalyst loading amount of 5wt%, uniformly dispersing in the mixed solution, stirring and reacting for 15min at 160 ℃ in a microwave reactor, washing the product with ethanol after the reaction is finished, and drying for 24h at 60 ℃ in a forced air drying oven to obtain N-SrTiO3An activated carbon treatment material; wherein the photocatalyst is N-SrTiO3；
The N-SrTiO3When the active carbon treatment material is used for wastewater treatment: 3g of N-SrTiO is added into 1L of electroplating wastewater3Active carbon treatment material, analysis and detection adding N-SrTiO3The concentrations of heavy metal ions and COD in the electroplating wastewater before and after the active carbon treatment material; the results show that the removal rate of chromium ions reaches 99.8%, the removal rate of cadmium ions reaches 99.5%, and the removal rate of COD reaches 90.1%.
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