CN102294226A - Preparation method of bamboo charcoal loaded Au-TiO2 composite material and its application - Google Patents
Preparation method of bamboo charcoal loaded Au-TiO2 composite material and its application Download PDFInfo
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- CN102294226A CN102294226A CN 201110198661 CN201110198661A CN102294226A CN 102294226 A CN102294226 A CN 102294226A CN 201110198661 CN201110198661 CN 201110198661 CN 201110198661 A CN201110198661 A CN 201110198661A CN 102294226 A CN102294226 A CN 102294226A
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Abstract
The invention relates to a preparation method of an Au-TiO2-bamboo charcoal composite material and its application, and aims to provide a solution to the problems of poor ability in removing ammonia nitrogen from a polluted water body at low temperature and unobvious effect in eliminating micro-pollution in present water treatment processes. The method first prepares Au-TiO2 nanometer powder by an isometric impregnation method, and then loads the Au-TiO2 nanometer powder on the bamboo charcoal. According to the invention, an Au-TiO2 nano-material with a large specific surface area and strong adsorption and oxidation performances is loaded into the pores of the bamboo charcoal, thus the bamboo charcoal simultaneously has the functions of ammonia nitrogen adsorption as well as photocatalytic oxidation of ammonia nitrogen. Therefore, the bamboo charcoal loaded Au-TiO2 composite material can remove ammonia nitrogen from low temperature water at efficiency of 60-90%, and heavy metals and persistent organic pollutants can be partly removed. Besides, the preparation method of the invention has a simple preparation process.
Description
Technical field
The present invention relates to a kind of Au-TiO
2The preparation method of the composite of-bamboo charcoal and application.
Background technology
In recent years, along with rapid development of economy, most of surface water of China and underground water have been subjected to pollution in various degree, and ammonia nitrogen is one of main pollutant.Handle or deal with improperly if contaminated source water does not add, cause the ammonia-nitrogen content in the water outlet of waterworks higher, can cause the breeding growth of nitrococcus and nitrifier in the pipe network, thereby make the content overproof of nitrate and nitrite in the pipe network.The excessive meeting of nitrate makes the baby suffer from methemoglobinemia, nitrate nitrogen (NO in drinking water
3-will make red blood cell can not be with oxygen and cause baby's death by suffocation when N) content is higher than 10mg/L; In addition, nitrate and nitrite be converted into can produce " cancer, mutagenesis, teratogenesis " behind the nitrosamine three cause material.
The method that ammonia nitrogen in the drinking water is handled mainly contains: Activated Zeolite Adsorption, electric absorption method, aeration ammonia elimination process, break point chlorination ammonia elimination process, biological treatment and membrane filter method etc.Yet, at northern area because the water temperature in winter is very low, more than traditional method and be not suitable for removing ammonia nitrogen in the water at low temperature.
Summary of the invention
The objective of the invention is to the invention provides a kind of loaded on bamboo charcoal Au-TiO in order to solve in the existing water treatment technology to the unconspicuous problem of the relatively poor and little pollution removal effect of the removal ability of ammonia nitrogen in the low temperature polluted water body
2The preparation method of composite and application thereof.
Loaded on bamboo charcoal Au-TiO of the present invention
2The preparation method of composite realizes by following steps:
One, Au-TiO
2The preparation of nano material: with TiO
2It is that 8～9 concentration is the HAuCl of 8～15g/L that nanometer powder evenly is dispersed to the pH value
4In the solution, leave standstill 1～3h then, soak 1～3h after adding ammoniacal liquor again, filter then, again the sediment on the filter paper is washed to filtrate and be neutral, Au-TiO
2Precast body is again with Au-TiO
2Precast body is calcined 3～6h down at 400 ℃～600 ℃ again behind 100 ℃～115 ℃ down dry 12～16h, obtain Au-TiO
2Nano material, wherein, control TiO
2Nanometer powder quality and HAuCl
4The ratio of liquor capacity is 1g: 8～15mL, the addition of ammoniacal liquor and HAuCl
4The volume ratio of solution is 1: 1;
Two, loaded on bamboo charcoal Au-TiO
2The preparation of composite: a, the Au-TiO that step 1 is prepared
2Nano material evenly is dispersed in the ethanolic solution, gets the Au-TiO that homogeneous phase distributes
2Nano material dispersion liquid, wherein Au-TiO
2The ratio of nano material quality and volumes of aqueous ethanol is 1g: 20～50mL; B, the Au-TiO that obtains to step a
2Add the bamboo charcoal powder in the nano material dispersion liquid, stir 12～18h then, get mixed liquor, wherein Au-TiO in bamboo charcoal powder and the step 1
2The mass ratio of nano material is 1: 1～10, and described bamboo charcoal powder is that the final temperature by dry distillation charring is that to be broken to fineness be that 200 orders～250 orders obtain for 300 ℃～400 ℃ low-temperature carbonization bamboo charcoal powder; C, the mixed liquor that step b is obtained filter, and the sediment on the filter paper are washed to filtrate to be neutral again, and the sediment after will washing is again calcined 3～6h down at 400～450 ℃, and cooling obtains loaded on bamboo charcoal Au-TiO again
2Composite.
The present invention is with the loaded on bamboo charcoal Au-TiO for preparing
2Composite is crossed 200 purpose sieves, places the interior airtight preservation of vacuum drying chamber to get final product.
Loaded on bamboo charcoal Au-TiO of the present invention
2The loaded on bamboo charcoal Au-TiO that the preparation method of composite prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body.
Under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that the present invention is prepared
2Composite adds to polluted water, and stirring reaction 10～60min gets final product, and wherein the temperature of polluted water is 2 ℃～5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the polluted water is 5～15mg/L.
The loaded on bamboo charcoal Au-TiO that the present invention prepares
2In the application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, stir speed (S.S.) is 100～200 rev/mins (rpm).
The Au-TiO that step 1 of the present invention utilizes equi-volume impregnating to obtain
2Au loads on TiO in the nano material
2The nanometer powder surface belongs to compound nano material, has bigger specific area and stronger absorption and oxidation susceptibility.
The loaded on bamboo charcoal Au-TiO that the present invention prepares
2Au-TiO in the composite
2Nanometer powder is loaded on the bamboo charcoal, bamboo wood is as a kind of porous media material, the bamboo charcoal that forms after the destructive distillation pyrolysis has greater porosity, its hole comprises macrovoid, mesopore, micropore. bamboo charcoal has abundant porosity distribution and high-specific surface area, the surface functional group of other elements such as oxygen-containing functional group such as the carboxyl that there is carboxyl in its surface, exist with the lactone form, phenolic hydroxyl group and a small amount of sulfur-bearing, hydrogen, chlorine.Composite back Au-TiO
2Nanometer powder enters in the hole of bamboo charcoal, makes bamboo charcoal not only bring into play the physics usefulness of absorption ammonia nitrogen, has had the ability of photochemical catalytic oxidation ammonia nitrogen simultaneously, has improved Au-TiO
2To the removal efficient of ammonia nitrogen in the polluted water body, simultaneously persistence organic pollutant in the polluted water body is had certain suction-operated under the composite low temperature, obtained effect preferably.
Loaded on bamboo charcoal Si-TiO of the present invention
2Composite material and preparation method thereof is simple, but suitability for industrialized production.The loaded on bamboo charcoal Au-TiO that the present invention prepares
2The efficient that composite is removed ammonia nitrogen in 2 ℃～5 ℃ low temperature polluted waters reaches 60～90%, and heavy metal and persistence organic pollutant can access part and remove.Have than application prospects in water treatment field.
Description of drawings
Fig. 1 is the curve map that remains ammonia nitrogen concentration in the specific embodiment 24 in the water outlet behind the contaminated drinking water different time of processing, and wherein " ■-" is loaded on bamboo charcoal Au-TiO
2Composite, " ●-" is the bamboo charcoal powder; Fig. 2 is loaded on bamboo charcoal Au-TiO in the specific embodiment 25
2Residue ammonia nitrogen concentration curve map in the water outlet after the contaminated drinking water of composite processing different temperatures; Fig. 3 is loaded on bamboo charcoal Au-TiO in the specific embodiment 26
2Composite is handled residue ammonia nitrogen concentration curve map in the water outlet after the contaminated drinking water of different ammonia nitrogen concentrations; Fig. 4 is different Au-TiO
2Load Au-TiO with the bamboo charcoal mass ratio
2Composite is handled the curve map of residue ammonia nitrogen concentration in the water outlet after the contaminated drinking water, wherein " 1 " is the specific embodiment 23, " 2 " are the specific embodiment 27, " 3 " are the specific embodiment 28, " 4 " are the specific embodiment 29, and " 5 " are the specific embodiment 30.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: present embodiment is loaded on bamboo charcoal Au-TiO
2The preparation method of composite, it is realized by following steps:
One, Au-TiO
2The preparation of nano material: with TiO
2It is that 8～9 concentration is the HAuCl of 8～15g/L that nanometer powder evenly is dispersed to the pH value
4In the solution, leave standstill 1～3h then, soak 1～3h after adding ammoniacal liquor again, filter then, again the sediment on the filter paper is washed to filtrate and be neutral, Au-TiO
2Precast body is again with Au-TiO
2Precast body is calcined 3～6h down at 400 ℃～600 ℃ again behind 100 ℃～115 ℃ down dry 12～16h, obtain Au-TiO
2Nano material, wherein, control TiO
2Nanometer powder quality and HAuCl
4The ratio of liquor capacity is 1g: 8～15mL, the addition of ammoniacal liquor and HAuCl
4The volume ratio of solution is 1: 1;
Two, loaded on bamboo charcoal Au-TiO
2The preparation of composite: a, the Au-TiO that step 1 is prepared
2Nano material evenly is dispersed in the ethanolic solution, gets the Au-TiO that homogeneous phase distributes
2Nano material dispersion liquid, wherein Au-TiO
2The ratio of nano material quality and volumes of aqueous ethanol is 1g: 20～50mL; B, the Au-TiO that obtains to step a
2Add the bamboo charcoal powder in the nano material dispersion liquid, stir 12～18h then, get mixed liquor, wherein Au-TiO in bamboo charcoal powder and the step 1
2The mass ratio of nano material is 1: 1～10, and described bamboo charcoal powder is that the final temperature by dry distillation charring is that to be broken to fineness be that 200 orders～250 orders obtain for 300 ℃～400 ℃ low-temperature carbonization bamboo charcoal powder; C, the mixed liquor that step b is obtained filter, and the sediment on the filter paper are washed to filtrate to be neutral again, and the sediment after will washing is again calcined 3～6h down at 400～450 ℃, and cooling obtains loaded on bamboo charcoal Au-TiO again
2Composite.
The loaded on bamboo charcoal Au-TiO that the present invention prepares
2Au-TiO in the composite
2Nanometer powder is loaded on the bamboo charcoal, composite back Au-TiO
2Nanometer powder enters in the hole of bamboo charcoal, makes bamboo charcoal not only bring into play the physics usefulness of absorption ammonia nitrogen, has had the ability of photochemical catalytic oxidation ammonia nitrogen simultaneously, has improved Au-TiO
2To the removal efficient of ammonia nitrogen in the polluted water body, simultaneously persistence organic pollutant in the polluted water body is had certain suction-operated under the composite low temperature, obtained effect preferably.
The loaded on bamboo charcoal Au-TiO that the present invention prepares
2The efficient that composite is removed ammonia nitrogen reaches 60～90%, and heavy metal and persistence organic pollutant can access part and remove.Have than application prospects in water treatment field.
The specific embodiment two: what present embodiment and the specific embodiment one were different is with TiO in the step 1
2It is that 8～9 concentration is the HAuCl of 10g/L that nanometer powder evenly is dispersed to the pH value
4In the solution.Other step and parameter are identical with the specific embodiment one.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is to soak 2h after adding ammoniacal liquor again in the step 1.Other step and parameter are identical with the specific embodiment one or two.
The specific embodiment four: what present embodiment and the specific embodiment one, two or three were different is with Au-TiO in the step 1
2Precast body is behind dry 14h under 110 ℃.Other step and parameter are identical with the specific embodiment one, two or three.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to four is to calcine 5h down at 450 ℃ again in the step 1.Other step and parameter are identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different with one of specific embodiment one to five is that ethanolic solution is that mass percentage concentration is 2%～4% ethanol water in a step of step 2.Other step and parameter are identical with one of specific embodiment one to five.
The preparation percentage concentration of ethanol water preferably 2.2%～3.8% in the present embodiment, and best is 3%.
The specific embodiment seven: present embodiment is different with one of specific embodiment one to six is the Au-TiO that in a step of step 2 step 1 is prepared
2The even dispersing mode that nano material evenly is dispersed in the ethanolic solution is: the Au-TiO that step 1 is prepared
2Nano material adds in the ethanolic solution, at room temperature stirs 5h～8h with 150 rev/mins～180 rev/mins rotating speed then.Other step and parameter are identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different with one of specific embodiment one to seven is the Au-TiO that obtains to step a in the b step of step 2
2Add the bamboo charcoal powder in the nano material dispersion liquid, stir 15h then, get mixed liquor.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment nine: present embodiment is different with one of specific embodiment one to eight is Au-TiO in bamboo charcoal powder and the step 1 in the b step of step 2
2The mass ratio of nano material is 1: 2～7.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment ten: present embodiment is different with one of specific embodiment one to eight is Au-TiO in bamboo charcoal powder and the step 1 in the b step of step 2
2The mass ratio of nano material is 1: 5.Other step and parameter are identical with one of specific embodiment one to seven.
The specific embodiment 11: present embodiment is different with one of specific embodiment one to ten is that bamboo charcoal powder described in the b step of step 2 is that final temperature by dry distillation charring is that to be broken to fineness be that 220 orders obtain for 350 ℃ low-temperature carbonization bamboo charcoal powder.Other step and parameter are identical with one of specific embodiment one to ten.
The specific embodiment 12: present embodiment is different with one of specific embodiment one to 11 is that sediment after will washing in the c step of step 2 is at 410～440 ℃ of calcining 3.5～5h down.Other step and parameter are identical with one of specific embodiment one to 11.
The specific embodiment 13: present embodiment is different with one of specific embodiment one to 11 is that sediment after will washing in the c step of step 2 is at 420 ℃ of calcining 4h down.Other step and parameter are identical with one of specific embodiment one to 11.
The specific embodiment 14: present embodiment is the loaded on bamboo charcoal Au-TiO that the specific embodiment one prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body.
The specific embodiment 15: present embodiment is the specific embodiment 14 described loaded on bamboo charcoal Au-TiO
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that the specific embodiment one is prepared
2Composite adds to polluted water, and stirring reaction 10～60min gets final product, and wherein the temperature of polluted water is 2 ℃～5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the polluted water is 5～15mg/L.
After handling in the present embodiment, again with loaded on bamboo charcoal Au-TiO
2Composite filters out and gets final product.
The specific embodiment 16: present embodiment and the specific embodiment 15 are different is that the concentration that control adds the CNT-bamboo charcoal composite to the contaminated water source water is 8～12mg/L.Other step and parameter are identical with the specific embodiment 15.
The specific embodiment 17: present embodiment and the specific embodiment 15 are different is that the concentration that control adds the CNT-bamboo charcoal composite to the contaminated water source water is 10mg/L.Other step and parameter are identical with the specific embodiment 15.
The specific embodiment 18: what present embodiment and the specific embodiment 15,16 or 17 were different is that stir speed (S.S.) is 100～200 rev/mins (rpm).Other step and parameter are identical with the specific embodiment 15,16 or 17.
The specific embodiment 19: what present embodiment and the specific embodiment 15,16 or 17 were different is that stir speed (S.S.) is 120～180 rev/mins (rpm).Other step and parameter are identical with the specific embodiment 15,16 or 17.
The specific embodiment 20: what present embodiment and the specific embodiment 15,16 or 17 were different is that stir speed (S.S.) is 150 rev/mins (rpm).Other step and parameter are identical with the specific embodiment 15,16 or 17.
The specific embodiment 21: that present embodiment is different with one of specific embodiment 15 to 20 is stirring reaction 30～55min.Other step and parameter are identical with one of specific embodiment 15 to 20.
The specific embodiment 22: that present embodiment is different with one of specific embodiment 15 to 20 is stirring reaction 50min.Other step and parameter are identical with one of specific embodiment 15 to 20.
The specific embodiment 23: present embodiment is for being loaded on bamboo charcoal Au-TiO
2The preparation method of composite, it is realized by following steps:
One, Au-TiO
2The preparation of nano material: with 1gTiO
2It is that 8～9 concentration is the HAuCl of 10g/L that nanometer powder evenly is dispersed to 10mL pH value
4In the solution, leave standstill 2h then, soak 2h after adding ammoniacal liquor again, filter then, again the sediment on the filter paper is washed to filtrate and be neutral, Au-TiO
2Precast body is again with Au-TiO
2Precast body is calcined 6h down at 400 ℃ again behind dry 16h under 100 ℃, obtain Au-TiO
2Nano material, wherein, the addition of ammoniacal liquor and HAuCl
4The volume ratio of solution is 1: 1;
Two, loaded on bamboo charcoal Au-TiO
2The preparation of composite: a, the Au-TiO that the 1g step 1 is prepared
2Nano material adds in 2% (quality) ethanol water of 50mL, at room temperature with 160 rev/mins rotating speed stirring 6h, gets the Au-TiO that homogeneous phase distributes then
2The nano material dispersion liquid; B, the Au-TiO that obtains to step a
2Add 5g bamboo charcoal powder in the nano material dispersion liquid, stir 16h then, mixed liquor, wherein said bamboo charcoal powder is that the final temperature by dry distillation charring is that to be broken to fineness be that 200 orders obtain for 350 ℃ low-temperature carbonization bamboo charcoal powder; C, the mixed liquor that step b is obtained filter, and the sediment on the filter paper are washed to filtrate to be neutral again, and the sediment after will washing is again calcined 4h down at 40 ℃, and cooling obtains loaded on bamboo charcoal Au-TiO again
2Composite.
The loaded on bamboo charcoal Au-TiO that this enforcement is prepared into
2Au-TiO in the composite
2With the mass ratio of bamboo charcoal be 1: 5.
The TiO that present embodiment adopts
2Nanometer powder is the commercially available prod.
The specific embodiment 24: present embodiment is the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 is prepared
2Composite adds to contaminated drinking water, be under 150 rev/mins the condition in stir speed (S.S.), react 10min, 20min, 30min, 40min, 50min and 60min respectively, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.After disposing with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.
Loaded on bamboo charcoal Au-TiO in the present embodiment
2Composite handles that the residue ammonia nitrogen concentration is shown in " ■-" among Fig. 1 in the water outlet behind the contaminated drinking water different time, and as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is about 0.5mg/L, and ammonia nitrogen removal frank reaches about 90%; The residue ammonia nitrogen concentration is that ammonia nitrogen removal frank also reaches about 60% about 2mg/L in the water outlet of reaction 10min.Heavy metal and persistence organic pollutant obtain part and remove.
As a comparison, carry out following contrast experiment 1: under the lucifuge condition, with the final temperature of dry distillation charring is that to be broken to fineness be that the bamboo charcoal powder that 200 orders obtain adds to contaminated drinking water for 350 ℃ low-temperature carbonization bamboo charcoal powder, be under 150 rev/mins the condition in stir speed (S.S.), react 10min, 20min, 30min, 40min, 50min and 60min respectively, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.In the water outlet behind the contaminated drinking water treatment different time of bamboo charcoal powder foot couple among residue ammonia nitrogen concentration such as Fig. 1 " ●-" shown in, as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is about 4.0mg/L, ammonia nitrogen removal frank only is about 10%; The residue ammonia nitrogen concentration is about 0.2mg/L in the water outlet of reaction 10min, and ammonia nitrogen is not almost had removal effect.
As seen from Figure 1, load Au-TiO
2Bamboo charcoal behind the nanometer powder, the ammonia nitrogen removal effect is far superior to not loaded modified bamboo charcoal in the low temperature polluted water.
The specific embodiment 25: present embodiment is the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 is prepared
2Composite adds respectively to the contaminated drinking water of 1 ℃, 2 ℃, 3 ℃, 4 ℃ and 5 ℃, is under 150 rev/mins the condition in stir speed (S.S.), and reaction 60min must handle the water outlet after the contaminated drinking water of different temperatures.Wherein to add the concentration of the CNT-bamboo charcoal composite to the contaminated drinking water be 10mg/L in control.Contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.
After handling with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.
Loaded on bamboo charcoal Au-TiO in the present embodiment
2The residue ammonia nitrogen concentration as shown in Figure 2 in the water outlet after the contaminated drinking water of composite processing different temperatures, as seen, under 5 ℃ contaminated drinking water, composite reaches about 90% ammonia-N removal rate, and heavy metal and persistence organic pollutant obtain part and remove; And under 1 ℃, composite only is about 60% to ammonia-N removal rate, since composite to the absorption of ammonia nitrogen mainly based on chemisorbed, and temperature is the principal element of control molecular dynamics, Here it is along with the decline of system temperature, the main cause that composite reduces ammonia-N removal rate.
The specific embodiment 26: present embodiment is the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that the specific embodiment 23 is prepared
2Composite adds respectively to 5 ℃ ammonia nitrogen concentration and is respectively in the contaminated drinking water of 1mg/L, 2mg/L, 3mg/L, 4mg/L and 5mg/L, be under 150 rev/mins the condition in stir speed (S.S.), reaction 60min must handle the water outlet after the contaminated drinking water of different ammonia nitrogen concentrations.Wherein to add the concentration of the CNT-bamboo charcoal composite to the contaminated drinking water be 10mg/L in control.Contaminated drinking water is the water distribution of simulation ammonia nitrogen.After handling with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.
Loaded on bamboo charcoal Au-TiO in the present embodiment
2Composite is handled in the water outlet after the contaminated drinking water of different ammonia nitrogen concentrations the residue ammonia nitrogen concentration as shown in Figure 3, from Fig. 3 as seen, initial ammonia nitrogen concentration also is the important factor in order of composite to the ammonia nitrogen removal effect, reduction along with the ammonia nitrogen initial concentration, composite is also significantly descending to the removal effect of ammonia nitrogen, when initial ammonia nitrogen concentration was 1mg/L, composite only was about 50% to ammonia-N removal rate.
The specific embodiment 27: present embodiment and the specific embodiment 23 are different is the Au-TiO that obtains to step a in the b step of step 2
2Add 6g bamboo charcoal powder in the nano material dispersion liquid.Other step and parameter are identical with the specific embodiment 23.
The loaded on bamboo charcoal Au-TiO that this enforcement is prepared into
2Au-TiO in the composite
2With the mass ratio of bamboo charcoal be 1: 6.
The loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Composite adds to contaminated drinking water, be under 150 rev/mins the condition in stir speed (S.S.), reaction 60min, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.After disposing with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.Loaded on bamboo charcoal Au-TiO
2Composite is handled residue ammonia nitrogen concentration in the water outlet behind the contaminated drinking water different time shown in " 2 " among Fig. 4 corresponding point, and as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is that ammonia nitrogen removal frank reaches about 90% about 0.55mg/L.
The specific embodiment 28: present embodiment and the specific embodiment 23 are different is the Au-TiO that obtains to step a in the b step of step 2
2Add 7g bamboo charcoal powder in the nano material dispersion liquid.Other step and parameter are identical with the specific embodiment 23.
The loaded on bamboo charcoal Au-TiO that this enforcement is prepared into
2Au-TiO in the composite
2With the mass ratio of bamboo charcoal be 1: 7.
The loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Composite adds to contaminated drinking water, be under 150 rev/mins the condition in stir speed (S.S.), reaction 60min, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.After disposing with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.Loaded on bamboo charcoal Au-TiO
2Composite is handled residue ammonia nitrogen concentration in the water outlet behind the contaminated drinking water different time shown in " 3 " among Fig. 4 corresponding point, and as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is that ammonia nitrogen removal frank reaches about 86% about 0.72mg/L.
The specific embodiment 29: present embodiment and the specific embodiment 23 are different is the Au-TiO that obtains to step a in the b step of step 2
2Add 7.5g bamboo charcoal powder in the nano material dispersion liquid.Other step and parameter are identical with the specific embodiment 23.
The loaded on bamboo charcoal Au-TiO that this enforcement is prepared into
2Au-TiO in the composite
2With the mass ratio of bamboo charcoal be 1: 7.5.
The loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Composite adds to contaminated drinking water, be under 150 rev/mins the condition in stir speed (S.S.), reaction 60min, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.After disposing with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.Loaded on bamboo charcoal Au-TiO
2Composite is handled residue ammonia nitrogen concentration in the water outlet behind the contaminated drinking water different time shown in " 4 " among Fig. 4 corresponding point, and as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is that ammonia nitrogen removal frank reaches about 80% about 1.0mg/L.
The specific embodiment 30: present embodiment and the specific embodiment 23 are different is the Au-TiO that obtains to step a in the b step of step 2
2Add 10g bamboo charcoal powder in the nano material dispersion liquid.Other step and parameter are identical with the specific embodiment 23.
The loaded on bamboo charcoal Au-TiO that this enforcement is prepared into
2Au-TiO in the composite
2With the mass ratio of bamboo charcoal be 1: 10.
The loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, specific as follows: under the lucifuge condition, the loaded on bamboo charcoal Au-TiO that present embodiment is prepared
2Composite adds to contaminated drinking water, be under 150 rev/mins the condition in stir speed (S.S.), reaction 60min, obtain the water outlet under the stirring reaction different time, wherein the temperature of polluted water is 5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the contaminated drinking water is 10mg/L.Wherein, contaminated drinking water is that ammonia nitrogen concentration is the simulation ammonia nitrogen water distribution of 5mg/L.After disposing with loaded on bamboo charcoal Au-TiO
2The composite filtered and recycled gets final product.Loaded on bamboo charcoal Au-TiO
2Composite is handled residue ammonia nitrogen concentration in the water outlet behind the contaminated drinking water different time shown in " 5 " among Fig. 4 corresponding point, and as seen, remaining ammonia nitrogen concentration in the water outlet of reaction 60min is that ammonia nitrogen removal frank reaches about 75% about 1.25mg/L.
" 1 " corresponding point is the loaded on bamboo charcoal Au-TiO of the specific embodiment 23 preparations among Fig. 4
2In the application of composite material by adopting such as the specific embodiment 24 records, the reaction time is the ammonia nitrogen removal effect data under the 60min, and the residue ammonia nitrogen concentration is that ammonia nitrogen removal frank reaches about 90% about 0.5mg/L in the water outlet of reaction 60min.
As seen from Figure 4, as load Au-TiO
2With the mass ratio of bamboo charcoal 1: 6 o'clock, its composite is under the 5mg/L to initial ammonia nitrogen concentration in the polluted water, the removal efficient of ammonia nitrogen has reached about 90%, when the quality that increases support materials and bamboo charcoal again compares, composite remains unchanged substantially to ammonia-N removal rate, and both mass ratioes are when 1: 10 left and right sides, and composite still can reach about 70% the removal efficient of ammonia nitrogen.
Claims (10)
1. loaded on bamboo charcoal Au-TiO
2The preparation method of composite is characterized in that loaded on bamboo charcoal Au-TiO
2The preparation method of composite realizes by following steps:
One, Au-TiO
2The preparation of nano material: with TiO
2It is that 8～9 concentration is the HAuCl of 8～15g/L that nanometer powder evenly is dispersed to the pH value
4In the solution, leave standstill 1～3h then, soak 1～3h after adding ammoniacal liquor again, filter then, again the sediment on the filter paper is washed to filtrate and be neutral, Au-TiO
2Precast body is again with Au-TiO
2Precast body is calcined 3～6h down at 400 ℃～600 ℃ again behind 100 ℃～115 ℃ down dry 12～16h, obtain Au-TiO
2Nano material, wherein, control TiO
2Nanometer powder quality and HAuCl
4The ratio of liquor capacity is 1g: 8～15mL, the addition of ammoniacal liquor and HAuCl
4The volume ratio of solution is 1: 1;
Two, loaded on bamboo charcoal Au-TiO
2The preparation of composite: a, the Au-TiO that step 1 is prepared
2Nano material evenly is dispersed in the ethanolic solution, gets the Au-TiO that homogeneous phase distributes
2Nano material dispersion liquid, wherein Au-TiO
2The ratio of nano material quality and volumes of aqueous ethanol is 1g: 20～50mL; B, the Au-TiO that obtains to step a
2Add the bamboo charcoal powder in the nano material dispersion liquid, stir 12～18h then, get mixed liquor, wherein Au-TiO in bamboo charcoal powder and the step 1
2The mass ratio of nano material is 1: 1～10, and described bamboo charcoal powder is that the final temperature by dry distillation charring is that to be broken to fineness be that 200 orders～250 orders obtain for 300 ℃～400 ℃ low-temperature carbonization bamboo charcoal powder; C, the mixed liquor that step b is obtained filter, and the sediment on the filter paper are washed to filtrate to be neutral again, and the sediment after will washing is again calcined 3～6h down at 400～450 ℃, and cooling obtains loaded on bamboo charcoal Au-TiO again
2Composite.
2. loaded on bamboo charcoal Au-TiO according to claim 1
2The preparation method of composite is characterized in that in the step 1 TiO
2It is that 8～9 concentration is the HAuCl of 10g/L that nanometer powder evenly is dispersed to the pH value
4In the solution.
3. loaded on bamboo charcoal Au-TiO according to claim 1 and 2
2The preparation method of composite is characterized in that in the step 1 Au-TiO
2Precast body is behind dry 14h under 110 ℃.
4. loaded on bamboo charcoal Au-TiO according to claim 1 and 2
2The preparation method of composite is characterized in that calcining 5h down at 450 ℃ again in the step 1.
5. loaded on bamboo charcoal Au-TiO according to claim 1 and 2
2The preparation method of composite is characterized in that in the b step of step 2 Au-TiO in the bamboo charcoal powder and step 1
2The mass ratio of nano material is 1: 2～7.
6. loaded on bamboo charcoal Au-TiO according to claim 1 and 2
2The preparation method of composite is characterized in that in the b step of step 2 Au-TiO in the bamboo charcoal powder and step 1
2The mass ratio of nano material is 1: 5.
7. loaded on bamboo charcoal Au-TiO according to claim 1 and 2
2The preparation method of composite, the sediment after it is characterized in that will washing in the c step of step 2 is at 410～440 ℃ of calcining 3.5～5h down.
8. loaded on bamboo charcoal Au-TiO as claimed in claim 1
2The loaded on bamboo charcoal Au-TiO that the preparation method of composite prepares
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body.
9. loaded on bamboo charcoal Au-TiO according to claim 8
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body is characterized in that loaded on bamboo charcoal Au-TiO
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body is specific as follows: under the lucifuge condition, and the loaded on bamboo charcoal Au-TiO that the specific embodiment one is prepared
2Composite adds to polluted water, and stirring reaction 10～60min gets final product, and wherein the temperature of polluted water is 2 ℃～5 ℃, and the concentration that control adds the CNT-bamboo charcoal composite to the polluted water is 5～15mg/L.
10. loaded on bamboo charcoal Au-TiO according to claim 9
2Application in the method for composite ammonia nitrogen in removing the low temperature polluted water body, it is characterized in that controlling the concentration that adds the CNT-bamboo charcoal composite to the contaminated water source water is 10mg/L.
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| CN105585100A (en) * | 2015-12-16 | 2016-05-18 | 无锡吉进环保科技有限公司 | Visible light photo-catalyzed oxidization water treatment reactor |
| CN105585100B (en) * | 2015-12-16 | 2018-07-17 | 广东睿洁环保工程有限公司 | A kind of visible light light urges oxidation water processing reactor |
| CN105771882A (en) * | 2016-04-20 | 2016-07-20 | 湖北大学 | Bentonite particles, bentonite particle adsorption column and method for removing ammonia nitrogen |
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