CN105710383A - Method for preparing Cu powder by reducing CuO by adopting glycerinum - Google Patents
Method for preparing Cu powder by reducing CuO by adopting glycerinum Download PDFInfo
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- CN105710383A CN105710383A CN201610292183.8A CN201610292183A CN105710383A CN 105710383 A CN105710383 A CN 105710383A CN 201610292183 A CN201610292183 A CN 201610292183A CN 105710383 A CN105710383 A CN 105710383A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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Abstract
The invention discloses a method for preparing Cu powder by reducing CuO by adopting glycerinum. The method is characterized in that glycerinum which is a byproduct of biodiesel is used as a reducing agent; and under an alkaline condition of 250 DEG C, copper oxide is reduced to prepare pure copper powder. The method comprises the specific steps of A, adding CuO and alkali into a reactor, then adding a fixed amount of glycerinum solution, sealing the reactor, and keeping the pressure in the reactor at 3.9 MPa; B, putting the reactor into a high-temperature drying oven with the temperature of 200 to 250 DEG C for reaction for 1.5 to 4.0 hours; C, after the reaction is completed, cooling the reactor under a natural state to end the reaction; and D, opening the reactor, and collecting solid-phase products obtained in the reaction. The method is simple and feasible and is high in operability; in the whole preparation process, the environment cannot be polluted; the problem of environment pollution in the process of preparing copper by the conventional method is well solved; and furthermore, glycerinum can be also converted into a chemical engineering product such as organic acid with high additional value, and resource utilization of wastes is realized.
Description
Technical field
The present invention relates to technical field of chemistry, a kind of glycerol reduction CuO prepares the side of Cu powder
Method.
Background technology
Copper powder is a kind of important chemical materials, because it has the conduction of excellence, the spy such as corrosion-resistant, nonmagnetic
Point, is widely used in multiple fields such as metallurgy, chemical industry, medicine, biology, superconduction and environmental protection.System at present
The method of standby copper powder mainly has atomization, oxidation-reduction method and electrolysis etc..Wherein, electrolysis produces
Copper powder have that clean surface, formability be good, green strength high, at some higher-end businesses or special
Industry has the effect that can not be substituted.But, the existing preparation method of copper powder there is also some shortcomings, such as:
Electrolysis has the shortcomings such as big, the technological process length of electrolyte intractability after production cost height, impurity enriched；
Atomization prepares copper powder, and to there is formability poor, the shortcoming that apparent density is higher；Oxidation-reduction method prepares copper powder work
Skill is the harshest to the requirement of the equipment of production and operator, and production cost is high, and copper powder needs before application
Carry out extremely complex anti-oxidant treatment.
Summary of the invention
It is an object of the invention to the method that a kind of glycerol reduction CuO prepares Cu powder, the letter of the method production technology
Single, with low cost, whole operating process environmentally safe, it is possible to prepare that purity is high, particle diameter is little, point
Dissipate the copper powder that property is good.
The present invention solves technical problem and adopts the following technical scheme that
The method that a kind of glycerol reduction CuO prepares Cu powder, its feature is, with biological diesel oil byproduct
Glycerol is as reducing agent, and under the conditions of the alkalescence of 200-250 DEG C, reductive copper oxide prepares copper.
Further, the concretely comprising the following steps of described method:
CuO and alkali are added in reactor, is subsequently adding quantitative glycerite, seal reactor；
B, reactor is put in 200 DEG C of-250 DEG C of high temperature ovens reaction 1.5-4.0h, and keep reactor intrinsic pressure
Strong is 1.5-3.9MPa；
Reactor is cooled down with stopped reaction after terminating by C, reaction in its natural state；
D, open reactor, collect solid product after reaction.
Further, described glycerol: CuO mol ratio is 2-3mol:5-10mol.
Further, described glycerol: CuO mol ratio is 2mol:5mol.
Further, described alkali is selected from NaOH, KOH, Ca (OH)2In any one.
Further, described step B for putting into reaction 1.5h in 250 DEG C of high temperature ovens by reactor.
Further, the molar concentration of the reactant glycerol that described step A is sealed in reactor is 0.5mol/L,
Alkali molar concentration is 0.1mol/L.
Compared with the prior art, the present invention has the beneficial effect that:
1, the inventive method simple possible, workable, in whole preparation process, environment is not resulted in
Polluting, well solution transmission method controlling is for the problem of environmental pollution during copper, and glycerol can also
The chemical products such as the organic acid changing into high added value, are simultaneously achieved the recycling of garbage.
2, the copper powder purity that prepared by the inventive method is high, particle diameter is little, good dispersion.
Accompanying drawing explanation
Fig. 1 is the inventive method process chart.
Fig. 2 is the solid product XRD figure spectrum that the embodiment of the present invention 5 obtains.
Fig. 3 is the solid product XRD figure spectrum that the embodiment of the present invention 3 obtains
Fig. 4 is that the inventive method prepares copper powder size analysis chart.
Fig. 5 is commercially available copper powder (200 mesh) granularmetric analysis figure.
Detailed description of the invention
By specific embodiment, technical solution of the present invention is further explained explanation below in conjunction with accompanying drawing.
Embodiment
Using biological diesel oil byproduct glycerin as reducing agent, utilize Teflon reactor (manufacturer: Wu Xinan
Fang Jinggong company limited), under the alkaline water heat condition of 250 DEG C, reductive copper oxide prepares copper.Tool
Body step is as follows:
(1) inject in 100ml volumetric flask with prunus mume (sieb.) sieb.et zucc. Teller ten thousand/balance precise glycerol 9.210g,
Add distilled water and be settled to 100ml；Obtain the glycerite of molar concentration 1.0mol/L.
(2) King is joined with prunus mume (sieb.) sieb.et zucc. Teller a certain amount of CuO and NaOH of ten thousand/balance precise
In the Teflon inner bag of reactor, then with liquid-transfering gun, the 1.0mol/L glycerite prepared in advance is moved
Take and a certain amount of join in Teflon inner bag, inner bag is put in King shell of reactor, spring leaf on pad
And build the lid of reactor；With bench vice fixed plastics king's reactor, rapidly reactor is sealed；
(3) the King reactor of good seal is put in baking oven that (reactor is put into front oven temperature and risen to instead
Answer temperature) react, and start timing；During reaction, in keeping reactor, there is certain pressure.
(4) after reaction certain time, baking oven is opened, with clamp, King reactor is taken out, at natural shape
Cool down with stopped reaction under state.
(5) after King reactor cooled, open reactor, collect the solid product obtained with qualitative filter paper
Copper powder.
(6), after copper powder natural air drying collection obtained, load in sample bottle, carry out XRD to analysis room and divide
Analysis and laser particle size analysis.
Table 1 prepares the embodiment of copper powder for this employing said method
Glycerol in table 1, the molar concentration of alkali refer to the reaction density of glycerol in reactor, alkali.
As a example by embodiment 3 and 5, as Figure 2-3, can by gained solid phase sample is carried out XRD analysis
Knowing, embodiment 5 gained solid product only has copper simple substance, does not has other any metallicses, illustrates that copper powder is pure
Spend the highest.And embodiment 3 gained solid product is in addition to copper simple substance, possibly together with CuO, Cu2O, purity is relatively
Embodiment 5 is poor.
By gained copper powder and certain copper powder commercial are carried out particle diameter contrast, result see Fig. 4,5, the present embodiment 5
The various target particle size of gained copper powder and surface area index are superior to buy copper powder, illustrate to use glycerol oxygen reduction
Change the copper method for copper powder, it is possible to prepare high-quality copper powder.Additionally, the inventive method simple possible, can
Strong operability, in whole preparation process, does not results in pollution to environment, well solves transmission method controlling standby
Problem of environmental pollution during copper, and glycerol can also change into the chemical industry such as the organic acid of high added value
Product, is simultaneously achieved the recycling of garbage.
Claims (7)
1. the method that a glycerol reduction CuO prepares Cu powder, it is characterised in that with biodiesel byproduct
Thing glycerol is as reducing agent, and under the conditions of the alkalescence of 200 DEG C-250 DEG C, reductive copper oxide prepares copper.
The method that a kind of glycerol the most according to claim 1 reduction CuO prepares Cu powder, its feature exists
In, concretely comprising the following steps of described method:
A, CuO and alkali are added in reactor, be subsequently adding quantitative glycerite, seal reactor；
B, reactor is put in 200 DEG C of-250 DEG C of high temperature ovens reaction 1.5-4.0h；And keep reactor intrinsic pressure
Strong is 1.5-3.9MPa.
Reactor is cooled down with stopped reaction after terminating by C, reaction in its natural state；
D, open reactor, collect solid product after reaction.
The method that a kind of glycerol the most according to claim 2 reduction CuO prepares Cu powder, its feature exists
In, described glycerol: CuO mol ratio is 2-3mol:5-10mol.
The method that a kind of glycerol the most according to claim 3 reduction CuO prepares Cu powder, its feature exists
In, described glycerol: CuO mol ratio is 2mol:5mol.
5. the method preparing Cu powder according to a kind of glycerol reduction CuO described in Claims 2 or 3, it is special
Levying and be, described alkali is selected from NaOH, KOH, Ca (OH)2In any one.
6. the method preparing Cu powder according to a kind of glycerol reduction CuO described in Claims 2 or 3, it is special
Levying and be, described step B for putting into reaction 1.5h in 250 DEG C of high temperature ovens by reactor.
7. the method preparing Cu powder according to a kind of glycerol reduction CuO described in claim requirement 2 or 3,
It is characterized in that, the molar concentration of the reactant glycerol that described step A is sealed in reactor is 0.5mol/L,
Alkali molar concentration is 0.1mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610292183.8A CN105710383A (en) | 2016-04-30 | 2016-04-30 | Method for preparing Cu powder by reducing CuO by adopting glycerinum |
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| CN201610292183.8A CN105710383A (en) | 2016-04-30 | 2016-04-30 | Method for preparing Cu powder by reducing CuO by adopting glycerinum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110976901A (en) * | 2019-12-31 | 2020-04-10 | 湘潭大学 | Preparation method of nano copper powder |
Citations (8)
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|---|---|---|---|---|
| JPS6447801A (en) * | 1987-08-13 | 1989-02-22 | Daido Steel Co Ltd | Production of fine metal powder |
| CN1082468A (en) * | 1993-06-05 | 1994-02-23 | 范玉东 | Superfine cupper powder and technology of preparing thereof |
| US6436167B1 (en) * | 1996-05-13 | 2002-08-20 | The United States Of America As Represented By The Secretary Of The Navy | Synthesis of nanostructured composite particles using a polyol process |
| WO2006076611A3 (en) * | 2005-01-14 | 2007-03-01 | Cabot Corp | Production of metal nanoparticles |
| JP4120007B2 (en) * | 2003-01-21 | 2008-07-16 | ラサ工業株式会社 | Method for producing copper powder |
| CN101302148A (en) * | 2008-06-24 | 2008-11-12 | 同济大学 | Method for producing aminic acid by glycerin water thermal reduction of CO2 |
| CN103014216A (en) * | 2013-01-08 | 2013-04-03 | 中南大学 | Reduction method of iron compound in iron-containing material |
| CN105458295A (en) * | 2016-02-01 | 2016-04-06 | 中国科学院深圳先进技术研究院 | Multi-hole micrometer copper ball and preparation method thereof |
-
2016
- 2016-04-30 CN CN201610292183.8A patent/CN105710383A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6447801A (en) * | 1987-08-13 | 1989-02-22 | Daido Steel Co Ltd | Production of fine metal powder |
| CN1082468A (en) * | 1993-06-05 | 1994-02-23 | 范玉东 | Superfine cupper powder and technology of preparing thereof |
| US6436167B1 (en) * | 1996-05-13 | 2002-08-20 | The United States Of America As Represented By The Secretary Of The Navy | Synthesis of nanostructured composite particles using a polyol process |
| JP4120007B2 (en) * | 2003-01-21 | 2008-07-16 | ラサ工業株式会社 | Method for producing copper powder |
| WO2006076611A3 (en) * | 2005-01-14 | 2007-03-01 | Cabot Corp | Production of metal nanoparticles |
| CN101302148A (en) * | 2008-06-24 | 2008-11-12 | 同济大学 | Method for producing aminic acid by glycerin water thermal reduction of CO2 |
| CN103014216A (en) * | 2013-01-08 | 2013-04-03 | 中南大学 | Reduction method of iron compound in iron-containing material |
| CN105458295A (en) * | 2016-02-01 | 2016-04-06 | 中国科学院深圳先进技术研究院 | Multi-hole micrometer copper ball and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110976901A (en) * | 2019-12-31 | 2020-04-10 | 湘潭大学 | Preparation method of nano copper powder |
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