CN104475100A - Preparation method of carbon nano tube composite bismuth molybdate environmentally friendly and deep water treatment agent - Google Patents
Preparation method of carbon nano tube composite bismuth molybdate environmentally friendly and deep water treatment agent Download PDFInfo
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Abstract
The invention relates to a preparation method of a carbon nano tube composite bismuth molybdate environmentally friendly and deep water treatment agent. The preparation method comprises the following steps: (1), carboxylation and amination modification are performed on a carbon nano tube and 2,4,6-trifluoro-5-chloro-pyrimidine is modified to prepare a reaction type carbon nano tube; (2), bismuth salt, a stabilizer, a template agent and the reaction type carbon nano tube are added into a phosphate buffer solution, and stirring is performed for 30 to 60 min, so as to form turbid liquid; molybdate is dissolved into the phosphate buffer solution, and then the phosphate buffer solution is added into the turbid liquid, so as to form a transparent solution; (3), the product is obtained after filtering and drying. The preparation method provided by the invention has the advantages that the cost is low, the preparation method is simple, requirements for equipment are low, and the maneuverability is excellent; the water treatment agent can be used for removing high concentration organic pollutants in water, is suitable for deep treatment on various wastewater, environmental protection and zero secondary pollution are achieved, and the water treatment agent is antibacterial, deodorant and can absorb other heavy metal ions and the like.
Description
Technical field
The invention belongs to water treatment agent field, particularly a kind of preparation method of CNT compound bismuth molybdate green deep water treatment agent.
Background technology
The whole world only about 10% water be directly for the mankind used.Lion's share, 70% for agricultural, and remaining 20% is industrial.The blowdown of China is about 20% of the whole world, and it has to the fresh water of 5% of the whole world.Therefore, contaminated solution problem puts on the agenda.In textile printing and dyeing, leather, paper industry process, employ contaminated environment and harmful auxiliary agent in a large number, these auxiliary agents are the contaminated environment mainly with the form discharge of liquid greatly, biological degradability is poor, toxicity is large, and free formaldehyde content is high, the content overproof of heavy metal ion.Wherein, dressing of printing and dyeing becomes water pollutions rich and influential family especially undisputedly.From starching to destarch, wash, scouring and bleaching, mercerising, then dyeing and printing, also may need coating, all relate to washing by the every procedure of this flow process, and every every kg of material of procedure needs 20L water consumption.Result is that the water consumption of every kilogram of raw cotton in dressing process is added up nearly 200L.When showing at shopper window after the in men's style shirt customization of a standard, more than 2000L water production and processing it time used up (cloth: cotton textiles, 125g/m).
The method of the process waste water of current use mainly contains: physical partition method, biological degradation method, chemical decomposition method, but these methods all have some limitations, and are unfavorable for sustainable development.Thus, people start to be devoted to develop efficient, low energy consumption, applied widely and have the pollutant clearance technique of deep oxidation ability.In recent years, a lot of scholar is by TiO
2for Degradation of Organo-pollutants in Water with Photo-catalysis, but due to its greater band gap (3.2eV), only have response in ultraviolet light range, and bismuth molybdate has photocatalytic activity in visible region, can degradable organic pollutant, to reach the object that processing environment pollutes.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of CNT compound bismuth molybdate green deep water treatment agent, and the method is simple to operate, with low cost, low to the requirement of equipment; Water treatment agent is applicable to the advanced treating of various waste water, environmental protection non-secondary pollution.
The preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent of the present invention, comprising:
(1) by CNT at H
2sO
4and HNO
3room temperature ultrasonic reaction 30 ~ 60min in mixed liquor, washing is to neutral, and room temperature in vacuo is dried, and obtains carboxylic carbon nano-tube; Then carboxylic carbon nano-tube is distributed in excessive diethylenetriamine, adds 2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluorophosphoric acid ester, 40 ~ 50 DEG C of reaction 5 ~ 6h, ethanol washs, and room temperature in vacuo is dried, and obtains aminated carbon nano tube; Then by aminated carbon nano tube ultrasonic disperse in the mixed liquor of water and acetone, adjust ph is 5 ~ 6, ice-water bath drips 2,4,6-tri-fluoro-5-chlorine pyrimidine, adjust ph is 6 ~ 6.5,20 ~ 30 DEG C of ultrasonic reaction 24 ~ 48h, ethanol washs, washing, room temperature in vacuo is dried, and irradiation (under 222nm quasi-molecule ultraviolet source irradiation 3min) obtains response type CNT;
(2) response type CNT in bismuth salt, stabilizing agent, template and above-mentioned steps (1) is joined in phosphate buffer, stir 30 ~ 60min, form suspension; Molybdate is dissolved in phosphate buffer, then joins in described suspension, form clear solution; Wherein, the mass ratio of bismuth salt and CNT is 1:5 ~ 1:20;
(3) regulate the pH value of clear solution to be 5 ~ 9 with alkaline solution, be heated to 80 ~ 100 DEG C of backflow 6 ~ 24h and filter, under 300w microwave, processing 2h, obtain CNT compound bismuth molybdate green deep water treatment agent.
CNT in described step (1) and H
2sO
4and HNO
3the ratio of mixed liquor is 10 ~ 20g:4L; Wherein, H
2sO
4and HNO
3volume ratio be 1:1 ~ 5:1.
The mass ratio of the carboxylic carbon nano-tube in described step (1) and 2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluorophosphoric acid is 5 ~ 8:0.1 ~ 0.6.
The ratio of the aminated carbon nano tube in described step (1) and the mixed liquor of water and acetone is 4 ~ 4.5g:1L; Wherein, the volume ratio of water and acetone is 3:1 ~ 5:1.
The mass ratio of the aminated carbon nano tube in described step (1) and 2,4,6-tri-fluoro-5-chlorine pyrimidine is 4 ~ 4.5:4 ~ 6.
Sodium carbonate liquor adjust ph is adopted in described step (1).
Bismuth salt in described step (2) is the one in bismuth nitrate, waltherite, bismuth chloride, bismuth acetate; The concentration of bismuth salt is 0.01 ~ 0.15mol/L.
Molybdate in described step (2) is the one in sodium molybdate, potassium molybdate or ammonium molybdate; The concentration of molybdate is 0.01 ~ 0.15mol/L.
Stabilizing agent in described step (2) is the one in disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, gluconic acid sodium salt, BTCA; Stabilizer concentration is 0.01 ~ 0.05mol/L.
Template in described step (2) is the triblock polyether P123 of mass ratio 1:3 and the mixture of triblock copolymer F127; Template concentration is 0.05 ~ 0.1mol/.
Phosphate buffer in described step (2) is made up of concentration 0.025 ~ 0.05mol/L sodium dihydrogen phosphate and 0.05 ~ 0.1mol/L dibastic sodium phosphate.
Alkaline solution in described step (3) is the NaOH of concentration 0.5mol/L ~ 1.5mol/L or the aqueous solution of potassium hydroxide.
CNT, as a kind of porous mass, has special interlayer characteristic, at its area load nano bismuth molybdate particulate, can be prepared into loaded catalyst.This loaded photocatalyst can improve the dispersiveness of photochemical catalyst, is beneficial to and recycles and reuses.
The present invention utilizes the porous of CNT, high adsorption capacity, combines with the photocatalytic activity of the feature such as water is easily separated and nano bismuth molybdate, nano bismuth molybdate is successfully loaded on CNT, be prepared into the visible-light photocatalysis material of the high catalytic activity that can be suspended in waste water and can be separated with water smoothly, and be applied to the advanced treating of waste water, can realize water middle and high concentration organic pollution oxidation removal, instead of transfer to other places, be the technology of an environment-friendly type.
And due to the aboundresources, cheap of CNT, the load type photocatalytic material therefore prepared by the present invention also has advantage with low cost, there is antibacterial, deodorizing simultaneously, the advantages such as other heavy metal ion can be adsorbed.
beneficial effect
(1) the present invention is with low cost, and preparation method is simple, and low to the requirement of equipment, operability is good;
(2) water treatment agent of the present invention can remove water middle and high concentration organic pollution, is applicable to the advanced treating of various waste water, environmental protection non-secondary pollution, and has antibacterial, deodorizing, can adsorb the advantages such as other heavy metal ion;
(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 recycle.
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
(1) be the H of 1:1 by 10g CNT in 4L volume ratio
2sO
4and HNO
4room temperature ultrasonic reaction 30min in mixed liquor, washing is to neutral, and room temperature in vacuo dries 48h, obtains 5g carboxylic carbon nano-tube; Then above-mentioned 5g carboxylic carbon nano-tube is distributed in excessive 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; Finally by 4g aminated carbon nano tube ultrasonic disperse in 1L volume ratio is the water of 3:1 and the mixed liquor of acetone, be 5 by sodium carbonate liquor adjust ph, ice-water bath drips the fluoro-5-chlorine pyrimidine of 4g 2,4,6-tri-, be 6 by sodium carbonate liquor adjust ph, 20 DEG C of ultrasonic reaction 24h, ethanol washs, washing, room temperature in vacuo dries 48h, and under 222nm quasi-molecule ultraviolet source, irradiation 3min obtains response type CNT;
(2) be that in the triblock polyether P123 of 1:3 and the mixture of triblock copolymer F127 and above-mentioned steps (1), response type CNT joins concentration by bismuth nitrate, disodium ethylene diamine tetraacetate, mass ratio be in the buffer solution of 0.025mol/L sodium dihydrogen phosphate and 0.05mol/L dibastic sodium phosphate composition, stir 30min, form suspension; Sodium molybdate is dissolved in phosphate buffer, then joins in described suspension, form clear solution; Wherein the concentration of bismuth nitrate is 0.01mol/L, the concentration of stabilizing agent is 0.01mol/L, the concentration 0.05mol/L of template and the concentration of sodium molybdate are 0.01mol/L.
(3) regulate the pH value of above-mentioned clear solution to be 5 with the sodium hydrate aqueous solution of concentration 0.5mol/L, at heating 80 DEG C, backflow 6h, filters, obtains product; Under 300w microwave, process 2h, wherein the mass ratio of bismuth nitrate and CNT is 1:5.
Embodiment 2
(1) be the H of 3:1 by 10g CNT in 4L volume ratio
2sO
4and HNO
4room temperature ultrasonic reaction 45min in mixed liquor, washing is to neutral, and room temperature in vacuo dries 54h, obtains 6.5g carboxylic carbon nano-tube; Then above-mentioned 5g carboxylic carbon nano-tube is distributed in excessive diethylenetriamine, adds 300mg 2-(7-azo BTA)-N, N, N', N'-tetramethylurea 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 1L volume ratio is the water of 4:1 and the mixed liquor of acetone, be 5.5 by sodium carbonate liquor adjust ph, ice-water bath drips the fluoro-5-chlorine pyrimidine of 5g 2,4,6-tri-, be 6.2 by sodium carbonate liquor adjust ph, 25 DEG C of ultrasonic reaction 36h, ethanol washs, washing, room temperature in vacuo dries 48h, and under 222nm quasi-molecule ultraviolet source, irradiation 3min obtains response type CNT;
(2) be that in the triblock polyether P123 of 1:3 and the mixture of triblock copolymer F127 and above-mentioned steps (1), response type CNT joins concentration by bismuth acetate, gluconic acid sodium salt, mass ratio be in the buffer solution of 0.03mol/L sodium dihydrogen phosphate and 0.06mol/L dibastic sodium phosphate composition, stir 30min, form suspension; Potassium molybdate is dissolved in phosphate buffer, then joins in described suspension, form clear solution; Wherein the concentration of bismuth acetate is 0.06mol/L, the concentration of stabilizing agent is 0.03mol/L, the concentration 0.07mol/L of template and the concentration of potassium molybdate are 0.07mol/L.
(3) regulate the pH value of above-mentioned clear solution to be 7 with the sodium hydrate aqueous solution of concentration 0.5mol/L, at heating 90 DEG C, backflow 16h, filters, obtains product; Under 300w microwave, process 2h, wherein the mass ratio of bismuth acetate and CNT is 1:10.
Embodiment 3
(1) be the H of 5:1 by 10g CNT in 4L volume ratio
2sO
4and HNO
4room temperature ultrasonic reaction 60min in mixed liquor, washing is to neutral, and room temperature in vacuo dries 60h, obtains 8g carboxylic carbon nano-tube; Then above-mentioned 8g carboxylic carbon nano-tube is distributed in excessive 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; Finally by 4.5g aminated carbon nano tube ultrasonic disperse in 1L volume ratio is the water of 5:1 and the mixed liquor of acetone, be 6 by sodium carbonate liquor adjust ph, ice-water bath drips the fluoro-5-chlorine pyrimidine of 6g 2,4,6-tri-, be 6.5 by sodium carbonate liquor adjust ph, 30 DEG C of ultrasonic reaction 48h, ethanol washs, washing, room temperature in vacuo dries 48h, and under 222nm quasi-molecule ultraviolet source, irradiation 3min obtains response type CNT;
(2) be that in the triblock polyether P123 of 1:3 and the mixture of triblock copolymer F127 and above-mentioned steps (1), response type CNT joins concentration by bismuth chloride, disodium ethylene diamine tetraacetate, mass ratio be in the buffer solution of 0.05mol/L sodium dihydrogen phosphate and 0.1mol/L dibastic sodium phosphate composition, stir 30min, form suspension; Sodium molybdate is dissolved in phosphate buffer, then joins in described suspension, form clear solution; Wherein the concentration of bismuth chloride is 0.15mol/L, the concentration of stabilizing agent is 0.05mol/L, the concentration 0.1mol/L of template and the concentration of sodium molybdate are 0.15mol/L.
(3) regulate the pH value of above-mentioned clear solution to be 9 with the potassium hydroxide aqueous solution of concentration 0.6mol/L, at heating 100 DEG C, backflow 24h, filters, obtains product; Under 300w microwave, process 2h, wherein the mass ratio of bismuth chloride and CNT is 1:15.
With the dyeing waste water of the printing and dyeing mill of same time sampling for handling object, add the water treatment agent of embodiment 1 ~ 3 gained of variable concentrations in waste water respectively, after 6 hours of daylight irradiate, the percent of decolourization of water treatment agent to dyeing waste water is as shown in the table:
| Percent of decolourization | COD clearance | |
| Embodiment 1 | 99.2％ | 91.1％ |
| Embodiment 2 | 99.3％ | 91.4％ |
| Embodiment 3 | 99.6％ | 92.7％ |
Claims (10)
1. a preparation method for CNT compound bismuth molybdate green deep water treatment agent, comprising:
(1) by CNT at H
2sO
4and HNO
3room temperature ultrasonic reaction 30 ~ 60min in mixed liquor, washing is to neutral, and room temperature in vacuo is dried, and obtains carboxylic carbon nano-tube; Then carboxylic carbon nano-tube is distributed in excessive diethylenetriamine, adds 2-(7-azo BTA)-N, N, N', N'-tetramethylurea hexafluorophosphoric acid ester, 40 ~ 50 DEG C of reaction 5 ~ 6h, ethanol washs, and room temperature in vacuo is dried, and obtains aminated carbon nano tube; Then by aminated carbon nano tube ultrasonic disperse in the mixed liquor of water and acetone, adjust ph is 5 ~ 6, ice-water bath drips 2,4,6-tri-fluoro-5-chlorine pyrimidine, adjust ph is 6 ~ 6.5,20 ~ 30 DEG C of ultrasonic reaction 24 ~ 48h, ethanol washs, washing, room temperature in vacuo is dried, and irradiation obtains response type CNT;
(2) response type CNT in bismuth salt, stabilizing agent, template and above-mentioned steps (1) is joined in phosphate buffer, stir 30 ~ 60min, form suspension; Molybdate is dissolved in phosphate buffer, then joins in described suspension, form clear solution; Wherein, the mass ratio of bismuth salt and CNT is 1:5 ~ 1:20;
(3) regulate the pH value of clear solution to be 5 ~ 9 with alkaline solution, add hot reflux and filter, microwave treatment, obtaining CNT compound bismuth molybdate green deep water treatment agent.
2. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the CNT in described step (1) and H
2sO
4and HNO
3the ratio of mixed liquor is 10 ~ 20g:4L; Wherein, H
2sO
4and HNO
3volume ratio be 1:1 ~ 5:1.
3. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, it is characterized in that: the carboxylic carbon nano-tube in described step (1) and 2-(7-azo BTA)-N, N, the mass ratio of N', N'-tetramethylurea hexafluorophosphoric acid is 5 ~ 8:0.1 ~ 0.6.
4. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the ratio of the aminated carbon nano tube in described step (1) and the mixed liquor of water and acetone is 4 ~ 4.5g:1L; Wherein, the volume ratio of water and acetone is 3:1 ~ 5:1.
5. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, it is characterized in that: the aminated carbon nano tube and 2 in described step (1), the mass ratio of 4,6-tri-fluoro-5-chlorine pyrimidine is 4 ~ 4.5:4 ~ 6.
6. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: adopt sodium carbonate liquor adjust ph in described step (1).
7. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the stabilizing agent in described step (2) is the one in disodium ethylene diamine tetraacetate, tetrasodium ethylenediamine tetraacetate, gluconic acid sodium salt, BTCA; Stabilizer concentration is 0.01 ~ 0.05mol/L.
8. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the template in described step (2) is the triblock polyether P123 of mass ratio 1:3 and the mixture of triblock copolymer F127; Template concentration is 0.05 ~ 0.1mol/L.
9. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the phosphate buffer in described step (2) is made up of concentration 0.025 ~ 0.05mol/L sodium dihydrogen phosphate and 0.05 ~ 0.1mol/L dibastic sodium phosphate.
10. the preparation method of a kind of CNT compound bismuth molybdate green deep water treatment agent according to claim 1, is characterized in that: the alkaline solution in described step (3) is the NaOH of concentration 0.5mol/L ~ 1.5mol/L or the aqueous solution of potassium hydroxide.
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Cited By (4)
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| CN106238104A (en) * | 2016-08-30 | 2016-12-21 | 樊之雄 | A kind of photocatalysis composite dye gives up material for water treatment and preparation method thereof |
| CN106423301A (en) * | 2016-12-02 | 2017-02-22 | 东华大学 | Fiber/carbon nanotube/Bi2MoO6 three-dimensional recyclable efficient catalytic material as well as preparation method and application of catalytic material |
| CN106423302A (en) * | 2016-12-02 | 2017-02-22 | 东华大学 | Fiber/carbon nanotube/BiPO4 three-dimensional recyclable efficient catalyzing material 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106238104A (en) * | 2016-08-30 | 2016-12-21 | 樊之雄 | A kind of photocatalysis composite dye gives up material for water treatment and preparation method thereof |
| CN106423301A (en) * | 2016-12-02 | 2017-02-22 | 东华大学 | Fiber/carbon nanotube/Bi2MoO6 three-dimensional recyclable efficient catalytic material as well as preparation method and application of catalytic material |
| CN106423302A (en) * | 2016-12-02 | 2017-02-22 | 东华大学 | Fiber/carbon nanotube/BiPO4 three-dimensional recyclable efficient catalyzing material 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 |
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