CN111715213A - CQDs/Mn (0H) prepared from coreopsis2And applications thereof - Google Patents
CQDs/Mn (0H) prepared from coreopsis2And applications thereof Download PDFInfo
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- CN111715213A CN111715213A CN201910212467.5A CN201910212467A CN111715213A CN 111715213 A CN111715213 A CN 111715213A CN 201910212467 A CN201910212467 A CN 201910212467A CN 111715213 A CN111715213 A CN 111715213A
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- cqds
- coreopsis
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- raw material
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- 239000011572 manganese Substances 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 19
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 241000723366 Coreopsis Species 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000012216 screening Methods 0.000 claims abstract description 9
- 239000010902 straw Substances 0.000 claims abstract description 9
- 239000002351 wastewater Substances 0.000 claims abstract description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 8
- 235000005912 Coreopsis cardaminifolia Nutrition 0.000 claims abstract description 6
- 241000132544 Coreopsis tinctoria Species 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 229910001437 manganese ion Inorganic materials 0.000 claims abstract description 5
- 230000001699 photocatalysis Effects 0.000 claims abstract description 4
- 238000007146 photocatalysis Methods 0.000 claims abstract description 3
- 150000002696 manganese Chemical class 0.000 claims description 6
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- 229940099596 manganese sulfate Drugs 0.000 claims description 3
- 235000007079 manganese sulphate Nutrition 0.000 claims description 3
- 239000011702 manganese sulphate Substances 0.000 claims description 3
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- 238000004043 dyeing Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 239000000975 dye Substances 0.000 description 8
- LPLLVINFLBSFRP-UHFFFAOYSA-N 2-methylamino-1-phenylpropan-1-one Chemical compound CNC(C)C(=O)C1=CC=CC=C1 LPLLVINFLBSFRP-UHFFFAOYSA-N 0.000 description 3
- 241000132539 Cosmos Species 0.000 description 3
- 235000005956 Cosmos caudatus Nutrition 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a CQDs/Mn (0H) prepared by taking coreopsis as a raw material2Belonging to the technical field of printing and dyeing wastewater treatment. The invention aims to solve the technical problem of environmental pollution of the existing method for preparing the carbon quantum dots. The method comprises the following steps: firstly, screening and crushing coreopsis tinctoria straws, screening to obtain a material A, sequentially adding water and hydrogen peroxide, and carrying out ultrasonic treatment; secondly, carrying out hydrothermal reaction, adding manganese ions, adding ammonia water or urea, stirring uniformly, and carrying out microwave treatment to obtain CQDs/Mn (0H)2. CQDs/Mn (0H) obtained by the above method2Is used for treating dye wastewater by photocatalysis. The preparation method has the advantages of simple preparation process, easily obtained raw materials, environmental protection and harmlessness; meeting the requirement of dye wastewater treatment. Has good treatment effect on dye polluted wastewater.
Description
Technical Field
The invention belongs to the technical field of printing and dyeing wastewater treatment; relating to a CQDs/Mn (0H)2The preparation method and the application thereof in the aspect of photocatalytic dye wastewater.
Background
The carbon quantum dots are fluorescent nano materials with carbon as a basic structural unit, and the size of the fluorescent nano materials is usually less than 10 nm; has low toxicity and good biocompatibility, and has wide development space in the fields of biological imaging, drug delivery, photoelectric devices and catalysis. The preparation method of the common carbon quantum dots is mostly finished in a system of strong oxidant, strong acid and strong base; the direct harm is that the preparation process is complex, a large amount of waste liquid is discharged into the natural environment in the preparation process, and certain pollution is brought to the atmosphere, water and soil. The exploration of the green and environment-friendly preparation process of the carbon quantum dots is important content of research in the field.
Most dyes are organic compounds, are various in types, and are widely applied to industries such as printing and dyeing, cosmetics, food, medicines and the like; a large amount of dye wastewater is discharged into the natural environment every year in China, so that serious pollution is caused to a water body; the research on the treatment process of dye wastewater is still important in the field of environmental engineering.
Disclosure of Invention
The invention aims to solve the technical problem of environmental pollution of the existing method for preparing the carbon quantum dots; and provides a CQDs/Mn (0H) prepared by taking coreopsis as a raw material2And applications thereof.
In order to solve the technical problem, the invention provides a method for preparing CQDs/Mn (0H) by taking coreopsis as a raw material2The method is completed by the following steps:
firstly, screening and crushing coreopsis tinctoria straws, screening to obtain a material A, sequentially adding water and hydrogen peroxide, and carrying out ultrasonic treatment;
step two, carrying out hydrothermal reaction, adding manganese ions, adding ammonia water or urea, uniformly stirring, and carrying out microwave treatment to obtain CQDs/Mn (0H)2。
Further, the mass ratio of the water to the material A in the step one is (10-30) mL to (0.1-0.5) g.
Further limiting, in the step one, the mass ratio of the volume of the hydrogen peroxide to the material A is (10-30) mL to (0.1-0.5) g.
Further limit, the ultrasonic treatment time in the step one is 5 minutes to 50 minutes, and the ultrasonic frequency is 25kHz to 40 kHz.
Further limiting, in the second step, the hydrothermal reaction is carried out for 1-10 h at 130-200 ℃.
And further limiting, the manganese ions in the second step are provided by manganese salt, wherein the manganese salt is one of manganese sulfate, manganese chloride and manganese nitrate, and the mass ratio of the manganese salt to the material A is (0.1-5): 0.1-0.5.
Further limiting, the mass ratio of the volume of the ammonia water to the material A in the step two is (10-50) mL to (0.1-0.5) g.
Further limiting, the mass ratio of the urea to the material A in the step two is (1-10) to (0.1-0.5).
And further limiting, in the step two, the microwave power is 50-700 watts, and the microwave treatment is carried out for 10-60 minutes.
CQDs/Mn (0H) obtained by the above method2Is used for treating dye wastewater by photocatalysis.
Compared with the prior art, the preparation method has the advantages of simple preparation process, easily obtained raw materials, environmental protection and harmlessness; meeting the requirement of dye wastewater treatment. Has good treatment effect on dye polluted wastewater.
Detailed Description
Example 1: this example illustrates the preparation of CQDs/Mn (0H) from coreopsis2The method is completed by the following steps:
firstly, screening and crushing coreopsis tinctoria straws, sieving the crushed cosmos tinctoria straws with a 40-mesh sieve to obtain a material A, taking 0.2g of the material A, sequentially adding 20 ml of water and 10 ml of hydrogen peroxide, and carrying out ultrasonic treatment for 20 minutes under the condition that the ultrasonic frequency is 40 kHz;
step two, carrying out hydrothermal reaction at 130 ℃ for 3H, adding 1g of manganese sulfate, adding 10 ml of ammonia water, stirring uniformly, and carrying out microwave treatment at 700 watts for 10 minutes to obtain CQDs/Mn (0H)2。
The following test methods were used to verify the effects of the present invention, and the test results are shown in table 1.
TABLE 1 Water distribution removal effect of visible light catalytic degradation of methylene blue
As can be seen from Table 1, the present inventionCQDs/Mn (0H) prepared by the method2Has certain treatment effect on the dye polluted wastewater.
Example 2: this example illustrates the preparation of CQDs/Mn (0H) from coreopsis2The method is completed by the following steps:
firstly, screening and crushing coreopsis tinctoria straws, sieving the crushed cosmos tinctoria straws with a 60-mesh sieve to obtain a material A, taking 0.1g of the material A, sequentially adding 30 ml of water and 30 ml of hydrogen peroxide, and carrying out ultrasonic treatment for 30 minutes under the condition that the ultrasonic frequency is 25 kHz;
step two, carrying out hydrothermal reaction at 200 ℃ for 1H, adding 1g of manganese chloride, then adding 20 ml of ammonia water, stirring uniformly, and carrying out microwave treatment at 50 watts for 60 minutes to obtain CQDs/Mn (0H)2。
Example 3: this example illustrates the preparation of CQDs/Mn (0H) from coreopsis2The method is completed by the following steps:
firstly, screening and crushing coreopsis tinctoria straws, sieving the crushed cosmos tinctoria straws with a 40-mesh sieve to obtain a material A, taking 0.5g of the material A, sequentially adding 10 ml of water and 10 ml of hydrogen peroxide, and carrying out ultrasonic treatment for 20 minutes under the condition that the ultrasonic frequency is 25 kHz;
step two, carrying out hydrothermal reaction at 200 ℃ for 2H, adding 1g of manganese nitrate, then adding 10 ml of ammonia water, stirring uniformly, and carrying out microwave treatment at 100 watts for 50 minutes to obtain CQDs/Mn (0H)2。
Claims (10)
1. CQDs/Mn (0H) prepared from coreopsis2Characterized in that said CQDs/Mn (0H)2The preparation method is completed by the following steps:
firstly, screening and crushing coreopsis tinctoria straws, screening to obtain a material A, sequentially adding water and hydrogen peroxide, and carrying out ultrasonic treatment;
step two, carrying out hydrothermal reaction, adding manganese ions, adding ammonia water or urea, uniformly stirring, and carrying out microwave treatment to obtain CQDs/Mn (0H)2。
2. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2OfThe method is characterized in that the mass ratio of the volume of the water to the material A in the step one is (10-30) mL to (0.1-0.5) g.
3. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the mass ratio of the volume of the hydrogen peroxide to the material A in the step one is (10-30) mL to (0.1-0.5) g.
4. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the ultrasonic treatment time in the step one is 5-50 minutes, and the ultrasonic frequency is 25-40 kHz.
5. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that in the second step, the hydrothermal reaction is carried out for 1 to 10 hours at the temperature of between 130 and 200 ℃.
6. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the manganese ions in the step two are provided by manganese salt, wherein the manganese salt is one of manganese sulfate, manganese chloride and manganese nitrate, and the mass ratio of the manganese salt to the material A is (0.1-5) to (0.1-0.5).
7. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the mass ratio of the volume of the ammonia water to the material A in the step two is (10-50) mL to (0.1-0.5) g.
8. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the mass ratio of the urea to the material A in the step two is (1-10) to (0.1-0.5).
9. CQDs/Mn (0H) is prepared by taking coreopsis as a raw material2The method is characterized in that the microwave power in the step two is 50-700 watts, and the microwave treatment is carried out for 5-60 minutes.
10. CQDs/Mn (0H) obtained by the method of claim 12Is used for treating dye wastewater by photocatalysis.
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Application publication date: 20200929 |