CN103752846A - Micro-channel continuous and rapid nano copper preparing method - Google Patents
Micro-channel continuous and rapid nano copper preparing method Download PDFInfo
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- CN103752846A CN103752846A CN201410019986.7A CN201410019986A CN103752846A CN 103752846 A CN103752846 A CN 103752846A CN 201410019986 A CN201410019986 A CN 201410019986A CN 103752846 A CN103752846 A CN 103752846A
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- copper
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- microchannel
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 42
- 239000010949 copper Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000000243 solution Substances 0.000 claims abstract description 34
- 239000011259 mixed solution Substances 0.000 claims abstract description 25
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 23
- 239000004094 surface-active agent Substances 0.000 claims abstract description 19
- 239000012153 distilled water Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000005086 pumping Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims description 14
- 238000005119 centrifugation Methods 0.000 claims description 13
- 238000002360 preparation method Methods 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 6
- 230000001105 regulatory effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 4
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- -1 softex kw Polymers 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 8
- 238000001035 drying Methods 0.000 abstract description 7
- 238000006722 reduction reaction Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 239000002086 nanomaterial Substances 0.000 abstract description 3
- 150000001879 copper Chemical class 0.000 abstract 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000012530 fluid Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
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Abstract
The invention relates to a micro-channel continuous and rapid nano copper preparing method, and belongs to the technical field of synthesis of nano materials by the micro fluid and micro reactor technology. The method includes firstly, dissolving bivalent copper salt in distilled water, adjusting the PH value, adding surface active agent and evenly mixing to configure and obtain copper salt mixed solution; dissolving reducing agent in distilled water to configure and obtain reducing solution; pumping the obtained copper salt mixed solution and reducing solution to micro channels to perform micro mix, cleaning, centrifugally separating and drying the mixed solution in vacuum at low temperature, and obtaining black nano copper. According to the method, the wet reduction method is combined, micro reduction reaction is performed through the micro channels in a mixed manner, and accordingly the nano copper can be prepared continuously and rapidly; the method is simple in process, the diameter of nano copper particles are distributed evenly, and dispersibility is fine.
Description
Technical field
The present invention relates to a kind of microchannel and prepare fast continuously the method for Nanometer Copper, belong to microfluid and microreactor technology nano materials technical field.
Background technology
The specific area of copper nanoparticle is large, surface-active is high, in metallurgical and petrochemical industry, is good catalyst.Aspect lubrication and friction, copper nanoparticle has shown excellent performance as a kind of soft metal nano particle, can be used as advanced lubrication oil additive.In addition, copper nanoparticle is the same with its block materials has very high thermal conductivity and electrical conductivity, can be used for manufacturing electrocondution slurry, and is applied to encapsulation, connection in microelectronics industry, and the miniaturization of microelectronic component is played an important role.At present, the preparation method of copper nanoparticle mainly contains solid phase method, vapor phase method, liquid phase chemical reduction method and microemulsion method etc., because Nanometer Copper is very easily oxidized, and the problems such as existence and stability and dispersiveness are poor, therefore, preparation dispersed and have good stability, study hotspot that pattern and the controlled copper nano material of size have become field of nanometer material technology.
The homogeneous phase that micro-reaction is carried out in fact exactly under minute yardstick or heterogeneous mixing, thereby reaction and mass-transfer performance are improved, the conversion ratio of reaction, selective and mass transfer rate are improved significantly, and realize mode that minute yardstick mixes and mainly contain microchannel and mix with film dispersion and mix.
Summary of the invention
The problem and the deficiency that for above-mentioned prior art, exist, the invention provides a kind of method that microchannel is prepared Nanometer Copper continuously fast.The present invention proposes the method in conjunction with wet reducing, by microchannel, is mixed and is carried out micro-reduction reaction, thereby realize, prepares fast continuously Nanometer Copper, and the method technique is simple, and Nanometer Copper particle diameter is evenly distributed, good dispersion, and the present invention is achieved through the following technical solutions.
Microchannel is prepared a method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first cupric salt is dissolved in distilled water, adds ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 300 ~ 1000r/min condition to mix 0.25 ~ 1h, configuration obtains mantoquita mixed solution;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper.
Cupric salt in described step (1) is copper sulphate, copper nitrate or copper chloride.
Surfactant in described step (1) is one or more the arbitrary proportion mixtures in polyvinylpyrrolidone, softex kw, polyvinyl alcohol, polyacrylamide, and wherein mantoquita is 1:(0 ~ 20 with the mol ratio of the surfactant adding).
Reducing agent in described step (2) is sodium borohydride or potassium borohydride, and wherein mantoquita is 1:(5 ~ 15 with the mol ratio of the reducing agent adding).
In described step (3), microchannel is of a size of (20 ~ 40) × (100 ~ 300) μ m, and controlling and pumping into solution flow rate is 10 ~ 35ml/min.
In above-mentioned steps (3), the rotating speed of centrifugation is 1000 ~ 5000r/min.
Above-mentioned vacuum dehydrating at lower temperature temperature is 40 ~ 60 ℃, drying time 20 ~ 40h.
The invention has the beneficial effects as follows: the present invention proposes the method in conjunction with wet reducing, by microchannel, mixed and carried out micro-reduction reaction, thereby realize, prepare fast continuously Nanometer Copper, the method technique is simple, and Nanometer Copper particle diameter is evenly distributed, good dispersion.
Accompanying drawing explanation
Fig. 1 is the microchannel mixing schematic diagram that the present invention prepares Nanometer Copper;
Fig. 2 is that solution flow rate of the present invention is the nano copper particle transmission electron microscope picture of preparing under 15ml/min condition;
Fig. 3 is that solution flow rate of the present invention is the nano copper particle energy spectrogram of preparing under 15ml/min condition;
Fig. 4 is that solution flow rate of the present invention is the nano copper particle transmission electron microscope picture of preparing under 25ml/min condition.
The specific embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1
As shown in Figure 1, this microchannel is prepared the method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first 10g cupric salt is dissolved in distilled water, add ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 600r/min condition to mix 0.5h, configuration obtains mantoquita mixed solution, wherein cupric salt is copper sulphate, surfactant is polyvinylpyrrolidone, and mantoquita is 1:2 with the mol ratio of the surfactant adding;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution, wherein reducing agent is sodium borohydride, and mantoquita is 1:5 with the mol ratio of the reducing agent adding;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper, black nano copper particle transmission electron microscope picture and energy spectrogram are as shown in Figures 2 and 3, wherein microchannel is of a size of 40 × 200 μ m, it is 15ml/min that control pumps into solution flow rate, the rotating speed of centrifugation is 3000r/min, vacuum dehydrating at lower temperature temperature is 40 ℃, drying time 30h.
Embodiment 2
As shown in Figure 1, this microchannel is prepared the method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first 10g cupric salt is dissolved in distilled water, add ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 800r/min condition to mix 0.5h, configuration obtains mantoquita mixed solution, wherein cupric salt is copper sulphate, surfactant is the mixed solution of polyvinylpyrrolidone and softex kw, and mantoquita is 1:4 with the mol ratio of the surfactant adding;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution, wherein reducing agent is sodium borohydride, and mantoquita is 1:8 with the mol ratio of the reducing agent adding;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper, this nano copper particle transmission electron microscope picture as shown in Figure 4, wherein microchannel is of a size of 40 × 200 μ m, and controlling and pumping into solution flow rate is 25ml/min; The rotating speed of centrifugation is 3000r/min; Vacuum dehydrating at lower temperature temperature is 40 ℃, drying time 30h.
Embodiment 3
As shown in Figure 1, this microchannel is prepared the method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first 10g cupric salt is dissolved in distilled water, add ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 1000r/min condition to mix 1h, configuration obtains mantoquita mixed solution, wherein cupric salt is copper nitrate, surfactant is polyvinyl alcohol, and mantoquita is 1:8 with the mol ratio of the surfactant adding;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution, wherein reducing agent is potassium borohydride, and mantoquita is 1:15 with the mol ratio of the reducing agent adding;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper, wherein microchannel is of a size of 20 × 100 μ m, and controlling and pumping into solution flow rate is 35ml/min; The rotating speed of centrifugation is 5000r/min; Vacuum dehydrating at lower temperature temperature is 60 ℃, drying time 40h.
Embodiment 4
As shown in Figure 1, this microchannel is prepared the method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first 10g cupric salt is dissolved in distilled water, add ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 300r/min condition to mix 0..25h, configuration obtains mantoquita mixed solution, wherein cupric salt is copper chloride, surfactant is the mixture of polyvinyl alcohol and polyacrylamide, and mantoquita is 1:20 with the mol ratio of the surfactant adding;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution, wherein reducing agent is potassium borohydride, and mantoquita is 1:5 with the mol ratio of the reducing agent adding;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper, wherein microchannel is of a size of 40 × 300 μ m, and controlling and pumping into solution flow rate is 10ml/min; The rotating speed of centrifugation is 1000r/min; Vacuum dehydrating at lower temperature temperature is 40 ℃, drying time 20h.
Embodiment 5
As shown in Figure 1, this microchannel is prepared the method for Nanometer Copper continuously fast, and its concrete steps are as follows:
(1) first 10g cupric salt is dissolved in distilled water, interpolation ammoniacal liquor regulates PH to 12 to mix rear configuration solution and obtains mantoquita mixed solution, and wherein cupric salt is copper chloride;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution, wherein reducing agent is sodium borohydride, and mantoquita is 1:10 with the mol ratio of the reducing agent adding;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper, wherein microchannel is of a size of 30 × 200 μ m, and controlling and pumping into solution flow rate is 25ml/min; The rotating speed of centrifugation is 3000r/min; Vacuum dehydrating at lower temperature temperature is 50 ℃, drying time 30h.
Claims (5)
1. microchannel is prepared a method for Nanometer Copper continuously fast, it is characterized in that concrete steps are as follows:
(1) first cupric salt is dissolved in distilled water, adds ammoniacal liquor solution is regulated to PH to 12, then after stir speed (S.S.) is to add surfactant under 300 ~ 1000r/min condition to mix 0.25 ~ 1h, configuration obtains mantoquita mixed solution;
(2) reducing agent is dissolved in to distilled water preparation and obtains reducing solution;
(3) reducing solution that mantoquita mixed solution step (1) being obtained and step (2) obtain pumps in microchannel and carries out minute yardstick mixing, to mixed solution clean, centrifugation, vacuum dehydrating at lower temperature processing, obtain black nano copper.
2. microchannel according to claim 1 is prepared the method for Nanometer Copper continuously fast, it is characterized in that: the cupric salt in described step (1) is copper sulphate, copper nitrate or copper chloride.
3. microchannel according to claim 1 is prepared the method for Nanometer Copper continuously fast, it is characterized in that: the surfactant in described step (1) is one or more the arbitrary proportion mixtures in polyvinylpyrrolidone, softex kw, polyvinyl alcohol, polyacrylamide, wherein mantoquita is 1:(0 ~ 20 with the mol ratio of the surfactant adding).
4. microchannel according to claim 1 is prepared the method for Nanometer Copper continuously fast, it is characterized in that: the reducing agent in described step (2) is sodium borohydride or potassium borohydride, and wherein mantoquita is 1:(5 ~ 15 with the mol ratio of the reducing agent adding).
5. microchannel according to claim 1 is prepared the method for Nanometer Copper continuously fast, it is characterized in that: in described step (3), microchannel is of a size of (20 ~ 40) × (100 ~ 300) μ m, and controlling and pumping into solution flow rate is 10 ~ 35ml/min.
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Cited By (11)
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|---|---|---|---|---|
| CN105598464A (en) * | 2016-01-06 | 2016-05-25 | 哈尔滨工业大学（威海） | In-situ preparation method of copper nanowires in microchannel |
| CN105727959A (en) * | 2014-12-11 | 2016-07-06 | 中国石油化工股份有限公司 | Method for preparing methanol synthesis catalyst by using microchannel reactor |
| CN107673394A (en) * | 2017-09-30 | 2018-02-09 | 南京工业大学 | A kind of method for preparing micron order triangular pyramidal cuprous bromide using ultrasonic wave added microchannel reaction unit |
| CN108057898A (en) * | 2016-11-08 | 2018-05-22 | 高勇谦 | A kind of continuous and automatic synthetic method of highly controllable metal nanometer line |
| CN108247077A (en) * | 2018-01-25 | 2018-07-06 | 深圳市中金岭南科技有限公司 | A kind of method that micro- reaction prepares copper powder |
| CN108486364A (en) * | 2018-05-31 | 2018-09-04 | 昆明理工大学 | A kind of microfluid extraction of 3D printing expands reactor and its application |
| CN108941599A (en) * | 2018-07-03 | 2018-12-07 | 珠海市彩龙科技有限公司 | A kind of continuous preparation method of Nanometer Copper |
| CN109332722A (en) * | 2018-11-28 | 2019-02-15 | 龚秀清 | A kind of method of microchannel synthesis copper nano-wire |
| CN112355320A (en) * | 2019-07-25 | 2021-02-12 | 上海沪正实业有限公司 | Nano copper powder and application thereof in preparation of antibacterial and haze-preventing mask |
| CN112913857A (en) * | 2021-01-21 | 2021-06-08 | 周红岩 | Nano-copper antibacterial material, antibacterial coating, and preparation method and application thereof |
| CN113976903A (en) * | 2021-10-18 | 2022-01-28 | 昆明理工大学 | Method for preparing micron-sized flaky silver powder through continuous reduction |
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| CN105727959A (en) * | 2014-12-11 | 2016-07-06 | 中国石油化工股份有限公司 | Method for preparing methanol synthesis catalyst by using microchannel reactor |
| CN105727959B (en) * | 2014-12-11 | 2018-08-07 | 中国石油化工股份有限公司 | A method of preparing methanol synthesis catalyst using micro passage reaction |
| CN105598464B (en) * | 2016-01-06 | 2017-10-24 | 哈尔滨工业大学（威海） | The in-situ preparation method of copper nano-wire in a kind of microchannel |
| CN105598464A (en) * | 2016-01-06 | 2016-05-25 | 哈尔滨工业大学（威海） | In-situ preparation method of copper nanowires in microchannel |
| CN108057898A (en) * | 2016-11-08 | 2018-05-22 | 高勇谦 | A kind of continuous and automatic synthetic method of highly controllable metal nanometer line |
| CN107673394B (en) * | 2017-09-30 | 2019-07-02 | 南京工业大学 | A method of micron order triangular pyramidal cuprous bromide is prepared using ultrasonic wave added microchannel reaction unit |
| CN107673394A (en) * | 2017-09-30 | 2018-02-09 | 南京工业大学 | A kind of method for preparing micron order triangular pyramidal cuprous bromide using ultrasonic wave added microchannel reaction unit |
| CN108247077A (en) * | 2018-01-25 | 2018-07-06 | 深圳市中金岭南科技有限公司 | A kind of method that micro- reaction prepares copper powder |
| CN108486364A (en) * | 2018-05-31 | 2018-09-04 | 昆明理工大学 | A kind of microfluid extraction of 3D printing expands reactor and its application |
| CN108941599A (en) * | 2018-07-03 | 2018-12-07 | 珠海市彩龙科技有限公司 | A kind of continuous preparation method of Nanometer Copper |
| CN108941599B (en) * | 2018-07-03 | 2021-06-08 | 珠海市彩龙科技有限公司 | Continuous preparation method of nano-copper |
| CN109332722A (en) * | 2018-11-28 | 2019-02-15 | 龚秀清 | A kind of method of microchannel synthesis copper nano-wire |
| CN112355320A (en) * | 2019-07-25 | 2021-02-12 | 上海沪正实业有限公司 | Nano copper powder and application thereof in preparation of antibacterial and haze-preventing mask |
| CN112913857A (en) * | 2021-01-21 | 2021-06-08 | 周红岩 | Nano-copper antibacterial material, antibacterial coating, and preparation method and application thereof |
| CN113976903A (en) * | 2021-10-18 | 2022-01-28 | 昆明理工大学 | Method for preparing micron-sized flaky silver powder through continuous reduction |
| CN113976903B (en) * | 2021-10-18 | 2023-04-07 | 昆明理工大学 | Method for preparing micron-sized flaky silver powder through continuous reduction |
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