CN104308143A - Production method of ternary copper powder - Google Patents
Production method of ternary copper powder Download PDFInfo
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- CN104308143A CN104308143A CN201410514933.2A CN201410514933A CN104308143A CN 104308143 A CN104308143 A CN 104308143A CN 201410514933 A CN201410514933 A CN 201410514933A CN 104308143 A CN104308143 A CN 104308143A
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Abstract
The invention provides a production method of ternary copper powder, i.e., a production method of ternary copper powder catalysts used for organic silicon monomer production by a direct method. The method comprises the steps of powder preparation, heat treatment, primary crushing, oxygenation and secondary crushing. The production method has the beneficial effects that the produced ternary copper powder has the characteristics that Cu-CuO-Cu2O materials are relatively stable, the specific surface area of the powder is large, and the selectivity in the use process is good.
Description
Technical field
The present invention relates to organic silicon monomer catalyst for synthesizing field, more specifically, relate to a kind of production method of ternary copper powder.
Background technology
Methylchlorosilane is also called organic silicon monomer, under the condition adding catalyst and heating, in fluid bed, carried out chemical reaction by metallic silicon, chloromethanes and obtained, Gu its synthetic reaction belongs to gas-solid-heterogeneous contact catalysis exothermic reaction, reaction mechanism is complicated, except main reaction, multiple side reaction exists simultaneously.Course of reaction influence factor is many, and comprise fluidized-bed structure, raw material silica flour chloromethanes, catalyst, technological parameter etc., especially the conformability of catalyst plays very important effect to this synthetic reaction.
Copper powder is the classical catalyst using the earliest in organic silicon monomer synthetic reaction and still using so far, its contact activity (productive rate of silica flour conversion ratio and monomer) and dimethyldichlorosilane selective not only relevant with its chemical composition, particle diameter and size distribution, surface state and preparation method etc., also relevant with the contact that the performance such as silica flour, co-catalyst and they and copper powder are formed jointly.
The catalyst system and catalyzing that current organic silicon monomer synthesis uses mainly contains copper powder catalyst system and catalyzing and ternary copper powder catalyst system and catalyzing, wherein, ternary copper powder catalyst system and catalyzing is mainly the ternary copper powder catalyst of Cu-CuO-Cu2O, existing ternary copper powder uses CuSO45H2O to obtain through dehydration, hydrogen reducing and oxidation processes, the ternary copper powder catalyst impurities content that the method is produced is high, powder diameter is large, makes in organic silicon monomer synthetic reaction selective not high.
Summary of the invention
In order to solve in above-mentioned prior art, one is that ternary copper powder catalyst impurities content is high; Two is drawbacks that ternary copper powder powder diameter is large, the invention provides a kind of production method of ternary copper powder.
A production method for ternary copper powder, described method comprises the steps:
(1) powder is joined: preparation oxygen content is 7.0% ~ 15.0%, and particle diameter is less than the copper powder mixed powder of 500um.
(2) heat treatment: in described step (1), gained copper powder mixed powder is heat-treat in the heat-treatment furnace of nitrogen or vacuum state at heat-treating atmosphere, and heat treatment temperature is 450 DEG C ~ 1000 DEG C.
(3) primary fragmentation: to gained powder in described step (2), primary fragmentation becomes particle diameter to be less than 500um powder.
(4) oxygenation: carry out oxygenation to the powder of described step (3) gained, oxygen content increment is 0.5% ~ 6.0%, and oxidizing temperature is 200 DEG C ~ 600 DEG C.
(5) second-time breakage: second-time breakage is carried out to described step (4) gained powder.
Preferably, the particle diameter of the described copper powder mixed powder in described step (1) is less than 300um.
Preferably, copper powder mixed powder described in described step (1) can by least one oxygen content be 0 ~ 20% raw material copper powder or a kind of oxygen content be 7% ~ 15% copper powder prepare.
Preferably, in described step (2), heat treatment temperature is 500 DEG C ~ 850 DEG C.
Preferably, heat treatment process and the cooling procedure of the middle powder of described step (2) need be carried out under nitrogen or vacuum state, and cooling procedure with stove cooling or can cool in cooling zone.
Preferably, in described step (3), gained powder diameter is less than 300um.
Preferably, in described step (3), fragmentation can be crusher in crushing or grinding machine fragmentation.
It will be appreciated that, when using grinding machine broken in described step (3), can in process of lapping or after powder fragmentation, add the raw material copper powder of pure copper powder or oxygen content 0 ~ 20%, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, and preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder.
Preferably, in described step (4), Powder Oxidation atmosphere can be air natural flowing or air blast or passes into compressed air.
It will be appreciated that, when after described step (4) oxygenation process, the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% can be added, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder.
Preferably, in described step (4), oxidizing temperature and can need oxygenation amount to adjust according to powder diameter.
Preferably, in described step (5) after powder fragmentation, the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% can be added.
It will be appreciated that, when using grinding machine broken in described step (5), the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% can be added in process of lapping, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder.
It is to be appreciated that when using grinding machine broken in described step (3) and described step (5), grinding grinding aid can be added, cold welding between powder during to avoid grinding.
The invention has the beneficial effects as follows, the ternary copper powder of production has Cu-CuO-Cu
2o thing Phase Proportion is stablized controlled, and Specific Surface Area Measurement is large, produces in the reaction of organic silicon monomer have selective high feature for dimethyldichlorosilane in direct method.
Specific embodiment
Specific embodiment 1
A production method for ternary copper powder, described method comprises the steps:
(1) powder is joined: preparation oxygen content is 11.0%, and particle diameter is less than the copper powder mixed powder of 300um.
(2) heat treatment: in described step (1), gained copper powder mixed powder is heat-treat in the heat-treatment furnace of nitrogen at heat-treating atmosphere, and heat treatment temperature is 800 DEG C; Heat treatment process and cooling procedure need be carried out under a nitrogen, and cooling procedure cools with stove.
(3) primary fragmentation: use disintegrating machine to gained powder in described step (2), primary fragmentation becomes particle diameter to be less than 300um powder.
(4) oxygenation: oxygenation is carried out to the powder of described step (3) gained, oxygen content increment is 0.5% ~ 4.0%, and oxidizing temperature is 300 DEG C; Oxygenation oxidizing atmosphere is for passing into compressed air, and after oxygenation process, adding percent mass ratio is in the powder the pure copper powder of 18%.
(5) second-time breakage: use high-energy stirring ball mill machine to carry out second-time breakage to described step (4) gained powder, grind broken time controling 1h.
Specific embodiment 2
A production method for ternary copper powder, described method comprises the steps:
(1) powder is joined: preparation oxygen content is 12.0%, and particle diameter is less than the copper powder mixed powder of 300um.
(2) heat treatment: in described step (1), gained copper powder mixed powder is heat-treat in the heat-treatment furnace of nitrogen at heat-treating atmosphere, and heat treatment temperature is 800 DEG C; Heat treatment process and cooling procedure need be carried out under a nitrogen, and cooling procedure cools with stove.
(3) primary fragmentation: use high-energy stirring ball mill machine to gained powder in described step (2), once grind 40min, be broken into particle diameter and be less than 300um powder, before grinding starts, adding percent mass ratio is in the powder the pure copper powder of 20%.
(4) oxygenation: oxygenation is carried out to the powder of described step (3) gained, oxygen content increment is 0.5% ~ 4.0%, and oxidizing temperature is 300 DEG C; Oxygenation oxidizing atmosphere is for passing into compressed air.
(5) second-time breakage: use high-energy stirring ball mill machine to carry out second-time breakage to described step (4) gained powder, grind broken time controling 1h.
In specific embodiment 1 and specific embodiment 2, the test data of ternary copper powder is as following table.
Claims (10)
1. a production method for ternary copper powder, is characterized in that described method comprises the steps:
(1) powder is joined: preparation oxygen content is 7.0% ~ 15.0%, and particle diameter is less than the copper powder mixed powder of 500um.
(2) heat treatment: in described step (1), gained copper powder mixed powder is heat-treat in the heat-treatment furnace of nitrogen or vacuum state at heat-treating atmosphere, and heat treatment temperature is 450 DEG C ~ 1000 DEG C.
(3) primary fragmentation: to gained powder in described step (2), primary fragmentation becomes particle diameter to be less than 500um powder.
(4) oxygenation: carry out oxygenation to the powder of described step (3) gained, oxygen content increment is 0.5% ~ 6.0%, and oxidizing temperature is 200 DEG C ~ 600 DEG C.
(5) second-time breakage: second-time breakage is carried out to described step (4) gained powder.
2. method according to claim 1, is characterized in that the particle diameter of the described copper powder mixed powder in described step (1) is less than 300um.
3. method according to claim 1, it is characterized in that copper powder mixed powder described in described step (1) can by least one oxygen content be 0 ~ 20% raw material copper powder or a kind of oxygen content be 7% ~ 15% copper powder prepare.
4. method according to claim 1, is characterized in that in described step (2), heat treatment temperature is 500 DEG C ~ 850 DEG C; The heat treatment process of powder and cooling procedure need be carried out under nitrogen or vacuum state, and cooling procedure with stove cooling or can cool in cooling zone.
5. method according to claim 1, to is characterized in that in described step (3) that primary fragmentation can be crusher in crushing or grinding machine is broken; Gained powder diameter is less than 300um.
6. method according to claim 1 or 6, it is characterized in that when using grinding machine broken in described step (3), can in process of lapping or after powder fragmentation, add the raw material copper powder of pure copper powder or oxygen content 0 ~ 20%, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, and preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder.
7. method according to claim 1, is characterized in that in described step (4), Powder Oxidation atmosphere can be air natural flowing or air blast or passes into compressed air.
8. method according to claim 1, it is characterized in that when after described step (4) oxygenation process, the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% can be added, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder; Oxidizing temperature and can need oxygenation amount to adjust according to powder diameter.
9. method according to claim 1, is characterized in that after powder fragmentation, can adding the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% in described step (5); When using grinding machine broken in described step (5), the raw material copper powder of pure copper powder or oxygen content 0 ~ 20% can be added in process of lapping, wherein, the percent mass ratio of the raw material copper powder of described pure copper powder or oxygen content 0 ~ 20% is 0 ~ 50%, preferably, its percent mass ratio is 0 ~ 25%; The raw material copper powder of wherein said pure copper powder or oxygen content 0 ~ 20% can be flake copper, copper reduction, electrolytic copper powder, water atomization copper powder, aerosolization copper powder.
10. method according to claim 1, is characterized in that, when using grinding machine broken in described step (3) and described step (5), can adding grinding grinding aid, cold welding between powder during to avoid grinding.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104760988A (en) * | 2015-03-11 | 2015-07-08 | 白晓光 | Environmental-protective preparation method of Cu2O and CuCl |
| CN105458275A (en) * | 2015-12-10 | 2016-04-06 | 湖南省天心博力科技有限公司 | Preparing method of copper-tin 10 alloy powder for powder metallurgy |
| CN110270328A (en) * | 2018-03-16 | 2019-09-24 | 苏州铜宝锐纳米科技有限公司 | Three-phase copper-based catalysts and the preparation method and application thereof |
| CN110665504A (en) * | 2019-10-22 | 2020-01-10 | 合盛硅业股份有限公司 | Preparation method of composite ternary copper powder |
| CN111451491A (en) * | 2020-04-29 | 2020-07-28 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material |
| CN115740431A (en) * | 2022-12-21 | 2023-03-07 | 北京有研粉末新材料研究院有限公司 | Compound copper powder and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104760988A (en) * | 2015-03-11 | 2015-07-08 | 白晓光 | Environmental-protective preparation method of Cu2O and CuCl |
| CN105458275A (en) * | 2015-12-10 | 2016-04-06 | 湖南省天心博力科技有限公司 | Preparing method of copper-tin 10 alloy powder for powder metallurgy |
| CN110270328A (en) * | 2018-03-16 | 2019-09-24 | 苏州铜宝锐纳米科技有限公司 | Three-phase copper-based catalysts and the preparation method and application thereof |
| CN110270328B (en) * | 2018-03-16 | 2022-03-15 | 苏州铜宝锐纳米科技有限公司 | Three-phase copper-based catalyst and preparation method and application thereof |
| CN110665504A (en) * | 2019-10-22 | 2020-01-10 | 合盛硅业股份有限公司 | Preparation method of composite ternary copper powder |
| CN111451491A (en) * | 2020-04-29 | 2020-07-28 | 西安稀有金属材料研究院有限公司 | Preparation method of graphene reinforced copper-based composite material |
| CN115740431A (en) * | 2022-12-21 | 2023-03-07 | 北京有研粉末新材料研究院有限公司 | Compound copper powder and preparation method and application thereof |
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Application publication date: 20150128 |