CN103785856B - A kind of preparation method of copper nano particles load carbon ball composite - Google Patents
A kind of preparation method of copper nano particles load carbon ball composite Download PDFInfo
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- CN103785856B CN103785856B CN201410067105.9A CN201410067105A CN103785856B CN 103785856 B CN103785856 B CN 103785856B CN 201410067105 A CN201410067105 A CN 201410067105A CN 103785856 B CN103785856 B CN 103785856B
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Abstract
A kind of copper nano particles load carbon ball composite and preparation method thereof, belongs to composite powder preparing technical field.Copper nano-particle is carried on carbon ball surface, and copper nano-particle is without Coated with Organic Matter, and clean surface, carbon ball and copper nano-particle size adjustable, carbon ball size is between 100 nanometers are to 100 microns, and copper nano-particle size is between 1 nanometer to 30 nanometers.Preparation is with mantoquita, carbon source, deionized water for raw material, the molar ratio of mantoquita and carbon source is 0.01-100.Mixing material is put into hydrothermal reaction kettle, at 80-250 DEG C of temperature, is incubated 2-50 hour; Take out reactor, be cooled to room temperature, pour out precipitation, cleaning, carries out drying at drying box; Finally, powder is put into aluminium oxide and is burnt boat, carries out calcination processing, holding temperature 300-900 DEG C, temperature retention time 0.5-10 hour, naturally cool to room temperature, obtain product in protective atmosphere pipe type stove.The invention has the advantages that and avoid using organic surface active agent, the copper nano particles obtaining having clean surface is fast carried on the composite of carbon ball.
Description
Technical field
The invention belongs to composite powder preparing technical field, be specifically related to a kind of new copper nano particles load carbon ball composite and preparation method thereof.
Background technology
Copper rich reserves, cheap, the nanocrystalline and composite of copper base more and more causes concern and the attention of people.Copper nano particles is a kind of excellent catalyst and eelctro-catalyst, how to prepare desirable copper nano particles tool and is of great significance.Conventional nanometer grain preparation method has Vacuum Heat vapour deposition, electron-beam lithography, pulsed laser deposition, cushion assisting growth, chemical vapour deposition (CVD), condensation of gas and cluster ions bundle condensation technology, electrochemical deposition, sol-gal process, deposition-precipitation and infusion process.Although a lot of document shows, the active nanoparticles catalyst that these technology can be prepared reliably, size is controlled, still has a large amount of problem to need to solve, particularly develops monodisperse nanoparticle that wrap up without part, clean surface very necessary.Usually in liquid-phase reaction system technology of preparing, surfactant or end-capping reagent be added, prevent the reunion of nano particle, growing up of restriction nano particle.But these organic existence often can harm the direct application of nano particle.Such as, when nano particle is wrapped up by diblock copolymer, the surface of nano particle finally can form one deck carbon or carbide, if be not further processed nano particle like this, catalyst can be caused in use poisoning.And to carry out process to these particle surfaces be take time and effort very much, how a step obtains the nano particle particular importance of clean surface.
The in-situ reducing of hydrothermal carbonization and metal ion combines by the present invention, is obtained the carbon ball composite construction of copper nano particles load by hydro-thermal method one step, and the copper nano particles prepared has clean surface, and single dispersing is carried on carbon ball surface.This copper carbon composite is all attractive viewed from economy and environment angle, can be used as a kind of new catalyst.
Summary of the invention
The copper nano particles that the present invention seeks to prepare a kind of clean surface is carried on the composite of carbon ball, with renewable carbon source substitution tables surface-active agent, simplifies the production technology of copper nano particles.
A kind of copper nano particles load carbon ball material, the architectural feature of this material is:
A, material are made up of carbon ball and copper nano-particle.
In b, material, carrier is solid carbon ball, and copper nano-particle is carried on carbon ball surface.
In c, material, copper nano-particle without Coated with Organic Matter, clean surface.
In d, material, carbon ball and copper nano-particle size adjustable, carbon ball size is between 100 nanometers are to 100 microns, and copper nano-particle size is between 1 nanometer to 30 nanometers.
The present invention provides a kind of new method preparing above-mentioned composite powder material simultaneously, and its preparation method comprises the steps:
A, raw material comprise three kinds: mantoquita, carbon source, solvent.Mantoquita can choose copper sulphate, cuprous iodide, copper nitrate, copper chloride, copper acetate are raw material; Carbon source can adopt sucrose, shitosan, glucose, citric acid, maltose, ascorbic acid, soluble starch to be raw material; Solvent adopts deionized water;
B, configuration precursor liquid: mantoquita and carbon source are dissolved in deionized water respectively, then by two kinds of solution mixing, in mixed solution, the molar ratio of mantoquita and carbon source is 0.01-100;
C, mixing material is put into hydrothermal reaction kettle, at 80-250 DEG C of temperature, be incubated 2-50 hour;
D, taking-up reactor, after being cooled to room temperature, open container, pour out precipitation, washing, carries out drying in drying box;
E, last, dried powder is put into aluminium oxide and is burnt boat, carries out calcination processing, holding temperature 300-900 DEG C, temperature retention time 0.5-10 hour, naturally cool to room temperature, obtain product in protective atmosphere pipe type stove.
The method cost is low, environmentally friendly, and purity is higher, be easy to promote.Hydrothermal carbonization method is combined the carbon ball composite preparing copper nano particles load by the method first time with slaine in-situ reducing.
Accompanying drawing explanation
In Fig. 1, a and b is the different amplification transmission electron microscope photo of copper nano particles load carbon ball composite of the present invention.
Detailed description of the invention
Embodiment 1:
0.015 gram of copper chloride and 0.7 gram of shitosan are dissolved in 20 ml distilled waters separately, be stirred to and dissolve completely, then by above-mentioned two kinds of solution mixing, sonic oscillation 15 minutes under normal temperature, mixing material after vibration is put into 50 milliliters of teflon-lined stainless steel hydro-thermal tanks, after tightening lid, hydro-thermal tank is put into 175 DEG C of baking ovens, be incubated after 4 hours, hydro-thermal tank is taken out baking oven, be placed in air and be cooled to room temperature, then hydro-thermal jar is opened, pour out the mixture of the inside, centrifugal in the centrifuge of 4000 revs/min, be precipitated, then repeatedly clean with water and ethanol, within 12 hours, drying is carried out in the insulation of 60 DEG C, drying box, finally, powder is put into aluminium oxide and is burnt boat, carries out calcination processing, heating rate 10 DEG C of min in argon gas atmosphere pipe type stove
-1, holding temperature 300 DEG C, temperature retention time 10 hours, naturally cools to room temperature, obtains product.
Embodiment 2:
0.4 gram of cuprous iodide and 0.1 gram of citric acid are dissolved in 20 ml distilled waters separately, be stirred to and dissolve completely, then by above-mentioned two kinds of solution mixing, sonic oscillation 15 minutes under normal temperature, mixing material after vibration is put into 50 milliliters of teflon-lined stainless steel hydro-thermal tanks, after tightening lid, hydro-thermal tank is put into 120 DEG C of baking ovens, be incubated after 9 hours, hydro-thermal tank is taken out baking oven, be placed in air and be cooled to room temperature, then hydro-thermal jar is opened, pour out the mixture of the inside, centrifugal in the centrifuge of 4000 revs/min, be precipitated, then repeatedly clean with water and ethanol, within 12 hours, drying is carried out in the insulation of 60 DEG C, drying box, finally, powder is put into aluminium oxide and is burnt boat, carries out calcination processing, heating rate 10 DEG C of min in argon gas atmosphere pipe type stove
-1, holding temperature 500 DEG C, temperature retention time 19 hours, naturally cools to room temperature, obtains product.
Embodiment 3:
0.5 gram of copper sulphate and 0.7 gram of maltose are dissolved in 20 ml distilled waters separately, be stirred to and dissolve completely, then by above-mentioned two kinds of solution mixing, sonic oscillation 15 minutes under normal temperature, mixing material after vibration is put into 50 milliliters of teflon-lined stainless steel hydro-thermal tanks, after tightening lid, hydro-thermal tank is put into 220 DEG C of baking ovens, be incubated after 24 hours, hydro-thermal tank is taken out baking oven, be placed in air and be cooled to room temperature, then hydro-thermal jar is opened, pour out the mixture of the inside, centrifugal in the centrifuge of 4000 revs/min, be precipitated, then repeatedly clean with water and ethanol, within 12 hours, drying is carried out in the insulation of 60 DEG C, drying box, finally, powder is put into aluminium oxide and is burnt boat, carries out calcination processing, heating rate 10 DEG C of min in argon gas atmosphere pipe type stove
-1, holding temperature 550 DEG C, temperature retention time 2 hours, naturally cools to room temperature, obtains product.
Embodiment 4:
0.1 gram of copper acetate and 0.7 gram of glucose are dissolved in 20 ml distilled waters separately, be stirred to and dissolve completely, then by above-mentioned two kinds of solution mixing, sonic oscillation 15 minutes under normal temperature, mixing material after vibration is put into 50 milliliters of teflon-lined stainless steel hydro-thermal tanks, after tightening lid, hydro-thermal tank is put into 150 DEG C of baking ovens, be incubated after 34 hours, hydro-thermal tank is taken out baking oven, be placed in air and be cooled to room temperature, then hydro-thermal jar is opened, pour out the mixture of the inside, centrifugal in the centrifuge of 4000 revs/min, be precipitated, then repeatedly clean with water and ethanol, within 12 hours, drying is carried out in the insulation of 60 DEG C, drying box, finally, powder is put into aluminium oxide and is burnt boat, carries out calcination processing, heating rate 10 DEG C of min in argon gas atmosphere pipe type stove
-1, holding temperature 650 DEG C, temperature retention time 1 hour, naturally cools to room temperature, obtains product.
Claims (1)
1. a preparation method for copper nano particles load carbon ball composite, is characterized in that: material is made up of carbon ball and copper nano-particle;
In material, carrier is solid carbon ball, and copper nano-particle is carried on carbon ball surface; Copper nano-particle without Coated with Organic Matter, clean surface; Carbon ball and copper nano-particle size adjustable, carbon ball size is between 100 nanometers are to 100 microns, and copper nano-particle size is between 1 nanometer to 30 nanometers;
Concrete preparation process is as follows:
A, raw material comprise three kinds: mantoquita, carbon source, solvent; It is raw material that mantoquita chooses copper sulphate, cuprous iodide, copper nitrate, copper chloride or copper acetate; Carbon source adopts sucrose, shitosan, glucose, citric acid, maltose, ascorbic acid or soluble starch to be raw material; Solvent adopts deionized water;
B, configuration precursor liquid: mantoquita and carbon source are dissolved in deionized water respectively, then by two kinds of solution mixing, in mixed solution, the molar ratio of mantoquita and carbon source is 0.01-100;
C, mixing material is put into hydrothermal reaction kettle, at 80-250 DEG C of temperature, be incubated 2-50 hour;
D, taking-up reactor, after being cooled to room temperature, open container, pour out precipitation, washing, carries out drying in drying box;
E, last, dried powder is put into aluminium oxide and is burnt boat, carries out calcination processing, holding temperature 300-900 DEG C, temperature retention time 0.5-10 hour, naturally cool to room temperature, obtain product in protective atmosphere pipe type stove.
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| CN104882187A (en) * | 2015-03-23 | 2015-09-02 | 江西九鹏科技股份有限公司 | Polythiophene-based low-density composite conductive paste and preparation method thereof |
| CN106424751A (en) * | 2016-11-18 | 2017-02-22 | 南昌大学 | Preparation method of nano copper powder |
| CN106818869B (en) * | 2017-01-10 | 2019-06-21 | 南通大学 | A kind of preparation method of carbon-based nano carbon/carbon-copper composite material |
| CN108187666B (en) * | 2018-01-23 | 2020-11-17 | 杭州卢普生物科技有限公司 | Preparation of biomass derived palladium catalyst and application of biomass derived palladium catalyst in synthesis of antitumor drug ocitinib |
| CN108315771B (en) * | 2018-02-11 | 2019-09-13 | 中国工程物理研究院材料研究所 | A kind of electrochemical preparation method of sub-nanometer size copper particle elctro-catalyst |
| CN111530417B (en) * | 2020-04-24 | 2021-04-27 | 北京科技大学 | Preparation method of cuprous ion loaded mesoporous carbon powder |
| CN113181913A (en) * | 2021-04-08 | 2021-07-30 | 湖北文理学院 | Copper-carbon composite catalyst and preparation method thereof |
| CN113600191A (en) * | 2021-08-30 | 2021-11-05 | 浙江工业大学 | Copper (II) doped chitosan carbon material and preparation method and application thereof |
| CN114917907A (en) * | 2022-04-19 | 2022-08-19 | 大连理工大学 | Supported non-noble metal catalyst with high catalytic hydrogenation activity, preparation method and application thereof |
| CN114797857B (en) * | 2022-05-20 | 2023-11-24 | 广东工业大学 | Nanometer flower-like copper-based material, and preparation method and application thereof |
| CN115282948B (en) * | 2022-07-07 | 2023-12-15 | 江苏大学 | Preparation method and application of ionic liquid mediated oligomeric chitosan derived IL-Cu/Al@NC microsphere |
| CN115285972B (en) * | 2022-08-05 | 2023-07-04 | 湖南师范大学 | Porous carbon-loaded metal nano material and preparation method thereof |
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