CN104437466B - A kind of CNT is combined the preparation method of pucherite green deep water treatment agent - Google Patents
A kind of CNT is combined the preparation method of pucherite green deep water treatment agent Download PDFInfo
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- CN104437466B CN104437466B CN201410838227.3A CN201410838227A CN104437466B CN 104437466 B CN104437466 B CN 104437466B CN 201410838227 A CN201410838227 A CN 201410838227A CN 104437466 B CN104437466 B CN 104437466B
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The present invention relates to a kind of CNT and be combined the preparation method of pucherite green deep water treatment agent, including: CNT successively carboxylated, amination modified, 2,4,6 trifluoro 5 chlorine pyrimidine modifications are prepared response type CNT by (1)；(2) bismuth salt, stabilizer, template and response type CNT are joined in phosphate buffer, stir 30～60min, form suspension；Metavanadate is dissolved in phosphate buffer, is then added in described suspension, form clear solution；(3) filtration drying obtains product.The present invention's is with low cost, and preparation method is simple, and the requirement to equipment is low, and operability is good；The water treatment agent of the present invention can remove water middle and high concentration organic pollution, it is adaptable to the advanced treating of various waste water, environmental protection non-secondary pollution, and have antibacterial, deodorizing, can adsorb the advantages such as other heavy metal ion.
Description
Technical field
The invention belongs to water treatment agent field, be combined the system of pucherite green deep water treatment agent particularly to a kind of CNT
Preparation Method.
Background technology
The water in the whole world the most about 10% is directly used by the mankind.Lion's share, 70% for agricultural, and remaining 20% is work
Industry is used.The blowdown of China is about the 20% of the whole world, and it has to the fresh water of global 5%.Therefore, solve pollution to ask
Topic puts on the agenda.In textile printing and dyeing, leather, paper industry process, employ pollution environment and right in a large number
The auxiliary agent that human body is harmful, these auxiliary agents mostly discharge with the form of liquid and pollute environment, and biological degradability is poor, and toxicity is big,
Free formaldehyde content is high, the content overproof of heavy metal ion.Wherein, printing and dyeing dressing becomes water pollution the most undisputedly
Rich and influential family.From starching start to desizing, wash, scouring and bleaching, mercerising, then dyeing and printing, may also need coating, by this flow process
Every procedure is directed to washing, and every every kg of material of procedure needs 20L water consumption.Result be during dressing every kilogram former
Cotton water consumption adds up up to 200L.When showing at shopper window after the in men's style shirt of a standard customizes, more than 2000L
Water production and processing it time used up (cloth: textile, 125g/m).
The currently used method processing waste water mainly has: physical partition method, biological degradation method, chemical decomposition method, but these
Method all has some limitations, and is unfavorable for sustainable development.Thus, people start to be devoted to exploitation efficiently, low energy consumption,
Applied widely and have the pollutant clearance technique of deep oxidation ability.In recent years, a lot of scholars are by TiO2Drop for photocatalysis
Solve organic pollutants, but due to its greater band gap (3.2eV), only have response in ultraviolet light range, and pucherite exists
Visible region has photocatalytic activity, can be with degradable organic pollutant, to reach the purpose that processing environment pollutes.
Summary of the invention
The technical problem to be solved is to provide a kind of CNT and is combined the system of pucherite green deep water treatment agent
Preparation Method, the method is simple to operate, with low cost, and the requirement to equipment is low；Water treatment agent is applicable to the degree of depth of various waste water
Process, environmental protection non-secondary pollution.
A kind of CNT of the present invention is combined the preparation method of pucherite green deep water treatment agent, including:
(1) by CNT at H2SO4And HNO3Room temperature ultrasonic reaction 30～60min in mixed liquor, washing is to neutrality, room temperature
Vacuum drying, obtains carboxylic carbon nano-tube；Then carboxylic carbon nano-tube is distributed in excess diethylenetriamine, adds
2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluorophosphoric acid ester, 40～50 DEG C of reactions 5～6h, ethanol washs, room
Temperature vacuum drying, obtains aminated carbon nano tube；Then by aminated carbon nano tube ultrasonic disperse to water and the mixed liquor of acetone
In, regulation pH value is 5～6, and ice-water bath dropping 2,4,6-tri-fluoro-5-chlorine pyrimidines, regulation pH value is 6～6.5,20～30 DEG C
Ultrasonic reaction 24～48h, ethanol washs, washing, and room temperature in vacuo is dried, and irradiation is (under 222nm quasi-molecule ultraviolet source
Irradiation 3min) obtain response type CNT；
(2) response type CNT in bismuth salt, stabilizer, template and above-mentioned steps (1) is joined in phosphate buffer,
Stirring 30～60min, forms suspension；Metavanadate is dissolved in phosphate buffer, is then added to described suspension
In, form clear solution；Wherein, bismuth salt is 1:5～1:20 with the mass ratio of CNT；
(3) pH value with alkaline solution regulation clear solution is 5～9, is heated to 80～100 DEG C of backflows 6～24h and filters,
Process 1h under 500w microwave, obtain CNT and be combined pucherite green deep water treatment agent.
CNT in described step (1) and H2SO4And HNO3The ratio of mixed liquor is 10～20g:4L；Wherein, H2SO4
And HNO3Volume ratio be 1:1～5:1.
Carboxylic carbon nano-tube in described step (1) and 2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluoro
The mass ratio of phosphoric acid is 5～8:0.1～0.6.
Aminated carbon nano tube in described step (1) is 4～4.5g:1L with the ratio of water and the mixed liquor of acetone；Wherein,
The volume ratio of water and acetone is 3:1～5:1.
Aminated carbon nano tube in described step (1) is 4～4.5:4～6 with the mass ratio of 2,4,6-tri-fluoro-5-chlorine pyrimidine.
Described step (1) uses sodium carbonate liquor regulation pH value.
Bismuth salt in described step (2) is the one in bismuth nitrate, waltherite, bismuth chloride, bismuth acetate；The concentration of bismuth salt
It is 0.01～0.15mol/L.
Metavanadate in described step (2) is the one in sodium metavanadate, potassium metavanadate or ammonium metavanadate；Alum salts partially
Concentration be 0.01～0.15mol/L.
Stabilizer in described step (2) be disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, sodium gluconate,
One in BTCA；Stabilizer concentration is 0.01～0.05mol/L.
The triblock polyether P123's that template is mass ratio 1:3 in described step (2) and triblock copolymer F127
Mixture；Template concentration is 0.05～0.1mol/.
Phosphate buffer in described step (2) is by concentration 0.025～0.05mol/L sodium dihydrogen phosphate and 0.05～0.1mol/L
Dibastic sodium phosphate forms.
Alkaline solution in described step (3) is the water-soluble of concentration 0.5mol/L～the NaOH of 1.5mol/L or potassium hydroxide
Liquid.
CNT, as a kind of porous mass, has special interlayer characteristic, can at its area load nanometer pucherite particulate,
It is prepared as loaded catalyst.This loaded photocatalyst can improve the dispersiveness of photochemical catalyst, is beneficial to reclaim and repeats profit
With.
Feature and the photocatalysis of nanometer pucherite such as the present invention utilizes the porous of CNT, high adsorption capacity and water easily separated
Activity combines, and is successfully loaded on CNT by nanometer pucherite, is prepared as being suspended in waste water and can
The visible-light photocatalysis material of the high catalytic activity to be separated from water smoothly, and it is applied to the advanced treating of waste water, can
To realize water middle and high concentration organic pollution oxidation removal rather than to transfer to elsewhere, it is the technique of an environment-friendly type
Technology.
Beneficial effect
(1) present invention is with low cost, and preparation method is simple, and the requirement to equipment is low, and operability is good；
(2) water treatment agent of the present invention can remove water middle and high concentration organic pollution, it is adaptable to the advanced treating of various waste water,
Environmental protection non-secondary pollution, and there is antibacterial, deodorizing, the advantages such as other heavy metal ion can be adsorbed；
(3) water treatment agent of the present invention can overcome the deficiency of existing bismuthino water treatment agent, and water treatment efficiency is good, can circulate and make
With.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
(1) it is the H of 1:1 by 10g CNT in 4L volume ratio2SO4And HNO4Room temperature ultrasonic reaction in mixed liquor
30min, washing to neutrality, room temperature in vacuo is dried 48h, is obtained 5g carboxylic carbon nano-tube；Then by above-mentioned 5g carboxylated
CNT is distributed in excess diethylenetriamine, adds 100mg 2-(7-azo BTA)-N, N, N', N'-tetramethylurea
Hexafluorophosphoric acid ester, 40 DEG C of reaction 5h, ethanol washs, and room temperature in vacuo dries 48h, obtains 4g aminated carbon nano tube；?
After by 4g aminated carbon nano tube ultrasonic disperse in the mixed liquor of the water that 1L volume ratio is 3:1 and acetone, use sodium carbonate
Solution regulation pH value is 5, the ice-water bath dropping fluoro-5-chlorine pyrimidine of 4g 2,4,6-tri-, is 6 by sodium carbonate liquor regulation pH value,
20 DEG C of ultrasonic reaction 24h, ethanol washs, washing, and room temperature in vacuo dries 48h, spoke under 222nm quasi-molecule ultraviolet source
Response type CNT is obtained according to 3min；
(2) by triblock polyether P123 that bismuth nitrate, disodium ethylene diamine tetraacetate, mass ratio are 1:3 and three blocks altogether
In the mixture of polymers F127 and above-mentioned steps (1), response type CNT joins concentration is 0.025mol/L biphosphate
In the buffer solution of sodium and 0.05mol/L dibastic sodium phosphate composition, stir 30min, form suspension；Sodium metavanadate is dissolved in phosphorus
In phthalate buffer, it is then added in described suspension, forms clear solution；Wherein the concentration of bismuth nitrate be 0.01mol/L,
The concentration of stabilizer is 0.01mol/L, the concentration of concentration 0.05mol/L of template and sodium metavanadate is 0.01mol/L.
(3) pH value with the sodium hydrate aqueous solution above-mentioned clear solution of regulation of concentration 0.5mol/L is 5, at heating 80 DEG C,
Backflow 6h, filters, obtains product；Processing 1h under 500w microwave, wherein bismuth nitrate with the mass ratio of CNT is
1:5。
Embodiment 2
(1) it is the H of 3:1 by 10g CNT in 4L volume ratio2SO4And HNO4Room temperature ultrasonic reaction in mixed liquor
45min, washing to neutrality, room temperature in vacuo is dried 54h, is obtained 6.5g carboxylic carbon nano-tube；Then by above-mentioned 5g carboxyl
Carbon nano tube is distributed in excess diethylenetriamine, adds 300mg 2-(7-azo BTA)-N, N, N', N'-tetramethyl
Urea hexafluorophosphoric acid ester, 45 DEG C of reaction 5h, ethanol washs, and room temperature in vacuo dries 48h, obtains 4.2g aminated carbon nano tube；
Finally by 4.2g aminated carbon nano tube ultrasonic disperse in the mixed liquor of the water that 1L volume ratio is 4:1 and acetone, use carbonic acid
Sodium solution regulation pH value is 5.5, the ice-water bath dropping fluoro-5-chlorine pyrimidine of 5g 2,4,6-tri-, by sodium carbonate liquor regulation pH value is
6.2,25 DEG C of ultrasonic reaction 36h, ethanol washs, washing, and room temperature in vacuo dries 48h, at 222nm Excimer UV light
Under source, irradiation 3min obtains response type CNT；
(2) by triblock polyether P123 and triblock copolymer F127 that bismuth acetate, sodium gluconate, mass ratio are 1:3
Mixture and above-mentioned steps (1) in response type CNT join concentration be 0.03mol/L sodium dihydrogen phosphate and
In the buffer solution of 0.06mol/L dibastic sodium phosphate composition, stir 30min, form suspension；Potassium metavanadate is dissolved in phosphate
In buffer solution, it is then added in described suspension, forms clear solution；Wherein the concentration of bismuth acetate is 0.06mol/L, steady
The concentration determining agent is 0.03mol/L, the concentration of concentration 0.07mol/L of template and partially alum acid potassium is 0.07mol/L.
(3) pH value with the sodium hydrate aqueous solution above-mentioned clear solution of regulation of concentration 0.5mol/L is 7, at heating 90 DEG C,
Backflow 16h, filters, obtains product；1h, wherein bismuth acetate and the mass ratio of CNT is processed under 500w microwave
For 1:10.
Embodiment 3
(1) it is the H of 5:1 by 10g CNT in 4L volume ratio2SO4And HNO4Room temperature ultrasonic reaction in mixed liquor
60min, washing to neutrality, room temperature in vacuo is dried 60h, is obtained 8g carboxylic carbon nano-tube；Then by above-mentioned 8g carboxylated
CNT is distributed in excess diethylenetriamine, adds 600mg 2-(7-azo BTA)-N, N, N', N'-tetramethylurea
Hexafluorophosphoric acid ester, 50 DEG C of reaction 5h, ethanol washs, and room temperature in vacuo dries 48h, obtains 4.5g aminated carbon nano tube；?
After by 4.5g aminated carbon nano tube ultrasonic disperse in the mixed liquor of the water that 1L volume ratio is 5:1 and acetone, use sodium carbonate
Solution regulation pH value is 6, the ice-water bath dropping fluoro-5-chlorine pyrimidine of 6g 2,4,6-tri-, is 6.5 by sodium carbonate liquor regulation pH value,
30 DEG C of ultrasonic reaction 48h, ethanol washs, washing, and room temperature in vacuo dries 48h, spoke under 222nm quasi-molecule ultraviolet source
Response type CNT is obtained according to 3min；
(2) by triblock polyether P123 that bismuth chloride, disodium ethylene diamine tetraacetate, mass ratio are 1:3 and three blocks altogether
In the mixture of polymers F127 and above-mentioned steps (1), response type CNT joins concentration is 0.05mol/L biphosphate
In the buffer solution of sodium and 0.1mol/L dibastic sodium phosphate composition, stir 30min, form suspension；Sodium metavanadate is dissolved in phosphoric acid
In salt buffer, it is then added in described suspension, forms clear solution；Wherein the concentration of bismuth chloride be 0.15mol/L,
The concentration of stabilizer is 0.05mol/L, the concentration of concentration 0.1mol/L of template and sodium metavanadate is 0.15mol/L.
(3) pH value with the potassium hydroxide aqueous solution above-mentioned clear solution of regulation of concentration 0.6mol/L is 9, heats 100 DEG C
Under, reflux 24h, filters, obtains product；1h, wherein bismuth chloride and the matter of CNT is processed under 500w microwave
Amount ratio is 1:15.
The dyeing waste water of the printing and dyeing mill sampled with the same time, for processing object, is separately added into the enforcement of variable concentrations in waste water
The water treatment agent of example 1～3 gained, after 6 hours solar radiations, the water treatment agent percent of decolourization such as following table to dyeing waste water
Shown in:
| Percent of decolourization | COD clearance | |
| Embodiment 1 | 99.0% | 91.0% |
| Embodiment 2 | 99.3% | 91.3% |
| Embodiment 3 | 99.4% | 92.4% |
Claims (10)
1. CNT is combined a preparation method for pucherite green deep water treatment agent, including:
(1) by CNT at H2SO4And HNO3Room temperature ultrasonic reaction 30～60min in mixed liquor, washing is to neutrality, room temperature
Vacuum drying, obtains carboxylic carbon nano-tube；Then carboxylic carbon nano-tube is distributed in excess diethylenetriamine, adds
2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluorophosphoric acid ester, 40～50 DEG C of reactions 5～6h, ethanol washs, room
Temperature vacuum drying, obtains aminated carbon nano tube；Then by aminated carbon nano tube ultrasonic disperse to water and the mixed liquor of acetone
In, regulation pH value is 5～6, and ice-water bath dropping 2,4,6-tri-fluoro-5-chlorine pyrimidines, regulation pH value is 6～6.5,20～30 DEG C
Ultrasonic reaction 24～48h, ethanol washs, washing, and room temperature in vacuo is dried, and irradiation obtains response type CNT；
(2) response type CNT in bismuth salt, stabilizer, template and above-mentioned steps (1) is joined in phosphate buffer,
Stirring 30～60min, forms suspension；Metavanadate is dissolved in phosphate buffer, is then added to described suspension
In, form clear solution；Wherein, bismuth salt is 1:5～1:20 with the mass ratio of CNT；
(3) pH value with alkaline solution regulation clear solution is 5～9, is heated to reflux and filters, and microwave treatment obtains carbon nanometer
The compound pucherite green deep water treatment agent of pipe.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the CNT in described step (1) and H2SO4And HNO3The ratio of mixed liquor is 10～20g:4L；Wherein,
H2SO4And HNO3Volume ratio be 1:1～5:1.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the carboxylic carbon nano-tube in described step (1) and 2-(7-azo BTA)-N, N, N', N'-tetramethylurea six
The mass ratio of fluorophosphoric acid ester is 5～8:0.1～0.6.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the aminated carbon nano tube in described step (1) is 4～4.5g:1L with the ratio of water and the mixed liquor of acetone；Wherein,
The volume ratio of water and acetone is 3:1～5:1.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the aminated carbon nano tube in described step (1) is 4～4.5:4～6 with the mass ratio of 2,4,6-tri-fluoro-5-chlorine pyrimidine.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: described step (1) uses sodium carbonate liquor regulation pH value.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
Be: the stabilizer in described step (2) be disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, sodium gluconate,
One in BTCA；In clear solution, stabilizer concentration is 0.01～0.05mol/L.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the triblock polyether P123 that template is mass ratio 1:3 in described step (2) and triblock copolymer F127
Mixture；In clear solution, template agent concentration is 0.05～0.1mol/L.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, its feature
It is: the phosphate buffer in described step (2) is by concentration 0.025～0.05mol/L sodium dihydrogen phosphate and 0.05～0.1mol/L
Disodium hydrogen phosphate forms.
A kind of CNT the most according to claim 1 is combined the preparation method of pucherite green deep water treatment agent, and it is special
Levy and be: the alkaline solution in described step (3) is concentration 0.5mol/L～the NaOH of 1.5mol/L or potassium hydroxide
The aqueous solution.
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| CN106732805A (en) * | 2016-12-02 | 2017-05-31 | 东华大学 | A kind of fiber/CNT/BiVO4 three-dimensional recyclable efficient catalytic material and its preparation and application |
| CN106902890B (en) * | 2017-04-14 | 2020-05-08 | 吉林师范大学 | Cu-BTC/bismuth vanadate/SWCNTs ternary heterostructure photocatalyst and preparation method and application thereof |
| CN109231184A (en) * | 2018-11-13 | 2019-01-18 | 广州百思创科技有限公司 | A kind of multi-functional conductive carbon nanotube and its preparation method and application |
| CN110052263A (en) * | 2019-04-30 | 2019-07-26 | 广东工业大学 | A kind of photocatalytic nanometer fibrous material and its preparation method and application |
| CN115738598B (en) * | 2022-11-17 | 2023-09-08 | 江苏乾云环保工程有限公司 | Method for treating organic waste gas generated in shoemaking and gluing |
| CN115709059B (en) * | 2022-12-26 | 2024-03-08 | 开封大学 | Mulberry bismuth vanadate-carbon nano tube composite photocatalyst and preparation method and application thereof |
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| CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
| CN101010137A (en) * | 2004-05-13 | 2007-08-01 | 株式会社北海道Tlo | Fine carbon dispersion |
| CN102500356A (en) * | 2011-11-11 | 2012-06-20 | 东华大学 | Preparation method for carbon nanotube-nano-bismuth vanadate composite photocatalyst |
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| CN101010137A (en) * | 2004-05-13 | 2007-08-01 | 株式会社北海道Tlo | Fine carbon dispersion |
| CN1683074A (en) * | 2005-03-11 | 2005-10-19 | 南京大学 | Process for preparing visible light responding photo catalytic film layer |
| CN102500356A (en) * | 2011-11-11 | 2012-06-20 | 东华大学 | Preparation method for carbon nanotube-nano-bismuth vanadate composite photocatalyst |
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