CN101386407A - Method for preparing nano carbon tube/titanium carbide(nitride) composite powder - Google Patents
Method for preparing nano carbon tube/titanium carbide(nitride) composite powder Download PDFInfo
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- CN101386407A CN101386407A CNA2008101973578A CN200810197357A CN101386407A CN 101386407 A CN101386407 A CN 101386407A CN A2008101973578 A CNA2008101973578 A CN A2008101973578A CN 200810197357 A CN200810197357 A CN 200810197357A CN 101386407 A CN101386407 A CN 101386407A
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Abstract
The invention relates to a preparation method for carbon nano-tube/titanium carbide (nitride) composite powder. The method comprises: after grinding, ilmenite concentrate powder is put into a microwave sintering furnace, then hydrogen and carbon source gas are inlet, so as to conduct ilmenite reduction treatment; the iron which is obtained from the reduction of the ilmenite is catalyzed to form a carbon nano-tube and the titanium oxide is reduced and carbonized into titanium carbide; or after grinding, the ilmenite concentrate powder is put into the microwave sintering furnace, then hydrogen, nitrogen as well as carbon source gas are inlet, so as to conduct ilmenite reduction treatment; the iron which is obtained from the reduction of the ilmenite is catalyzed to form the carbon nano-tube and the titanium oxide is reduced and carbonized into titanium carbonitride. The obtained carbon nano-tube/titanium carbide (nitride) composite powder has the advantages that: 1) the carbon nano-tube/titanium carbide (nitride) are evenly dispersed; 2) the raw materials are available, the price is low, the two components of the titanium and the iron in the raw materials can be comprehensively utilized, and the environment is not polluted.
Description
Technical field
The present invention relates to a kind of CNT (carbon nano-tube)/carbon (nitrogen) and change the preparation method of titanium composite granule.
Background technology
The ilmenite resource of China is very abundant, spreads all over 20 provinces and regions.But the aspect that utilizes for the ilmenite resource mainly is the production that utilizes sulfuric acid process and chlorination process to produce titanium white and titanium sponge at present, in the production process, how to handle a large amount of byproducts and spent acid waste liquid, how to improve that rate of energy reduces production costs and how more rationally to utilize iron in the ilmenite, two kinds of components of titanium to become this industry problem demanding prompt solution.
Summary of the invention
Problem to be solved by this invention is to propose the method that a kind of ilmenite with cheapness is feedstock production CNT (carbon nano-tube)/carbon (nitrogen) change titanium composite granule at above-mentioned prior art, this method can fully utilize the two kinds of components of titanium, iron in the raw material, and environmentally safe.
The present invention for the solution that problem adopts of the above-mentioned proposition of solution is: CNT (carbon nano-tube)/carbon (nitrogen) is changed the preparation method of titanium composite granule, it is characterized in that behind the ilmenite concentrate grinding, put into microwave agglomerating furnace, feed hydrogen and carbon-source gas, carrying out ilmenite reduction handles, the iron catalysis that ilmenite reduction obtains forms CNT (carbon nano-tube), it is titanium carbide that titanium oxide is reduced carbonization, perhaps with behind the ilmenite concentrate grinding, put into microwave agglomerating furnace, feed hydrogen, nitrogen and carbon-source gas carry out ilmenite reduction and handle, the iron catalysis that ilmenite reduction obtains forms CNT (carbon nano-tube), and it is titanium carbonitride that titanium oxide is reduced carbonization.
It is 500-1000 ℃ in CNT (carbon nano-tube) growth phase temperature that the present invention needs the controlled microwave sintering oven, and titanium oxide carbonation stage working temperature is 1200-1600 ℃.
Carbon-source gas of the present invention is Sweet natural gas, methane, acetylene, carbon monoxide, ethanol or acetone.
The present invention is according to the difference that feeds gas, can produce the composite granule of two kinds of forms, when the gas that feeds only is hydrogen and carbon-source gas, obtain CNT (carbon nano-tube)/titanium carbide composite granule, and when containing nitrogen in the gas that feeds, obtain CNT (carbon nano-tube)/titanium carbonitride composite granule.
The principal feature that CNT (carbon nano-tube)/carbon that the present invention obtained (nitrogen) is changed the titanium composite granule is:
1) CNT (carbon nano-tube)/carbon (nitrogen) is changed titanium the two is uniformly dispersed;
2) abundant raw material, cheap can fully utilize two kinds of components of ferrotianium, environmentally safe in the raw material.
Embodiment
The invention will be further described below in conjunction with embodiment, but can not be as limitation of the invention.
Embodiment 1
2 gram ilmenite concentrate powder (sample) are milled to 1-10 μ m, put in the microwave agglomerating furnace, feed hydrogen and Sweet natural gas, hydrogen flow rate is 10 cc/min, the Sweet natural gas flow velocity is 1 cc/min, and microwave power is 300W, and sample temperature is about 650 ℃, synthetic after 30 minutes, increase microwave output power to 800W, sample temperature is 1250 ℃, after 40 minutes, stop to synthesize, can obtain 11.5 gram finely dispersed CNT (carbon nano-tube)/titanium carbide composite granules.
Embodiment 2
2 gram ilmenite concentrate powder (sample) are milled to 1-10 μ m, put in the microwave agglomerating furnace, feed hydrogen and methane.Hydrogen flow rate is 20 cc/min, methane flow rate is 2 cc/min, microwave power 400W, sample temperature is 800 ℃, and is synthetic after 30 minutes, increases microwave power to 1000W, sample temperature is 1300 ℃, after 30 minutes, stop to synthesize, can obtain 14.2 gram finely dispersed CNT (carbon nano-tube)/titanium carbide composite granules.
Embodiment 3
2 gram ilmenite concentrate powder (sample) are milled to 1-10 μ m, put in the microwave agglomerating furnace, feed nitrogen, hydrogen and acetylene.Nitrogen flow rate is 20 cc/min, hydrogen flow rate is 10 cc/min, the acetylene flow velocity is 1 cc/min, and microwave power 400W, sample temperature are 800 ℃, synthetic after 30 minutes, increase microwave power to 1000W, sample temperature is 1300 ℃, after 30 minutes, stop to synthesize, can obtain 13.8 gram finely dispersed CNT (carbon nano-tube)/titanium carbonitride composite granules.
Embodiment 4
2 gram ilmenite concentrate powder (sample) are milled to 1-10 μ m, put in the microwave agglomerating furnace, feed hydrogen and methane.Hydrogen flow rate is 20 cc/min, methane flow rate is 2 cc/min, microwave power 500W, sample temperature is 1000 ℃, and Synthetic 2 increased microwave power to 1200W after 0 minute, sample temperature is 1600 ℃, after 20 minutes, stop to synthesize, can obtain 14.0 gram finely dispersed CNT (carbon nano-tube)/titanium carbide composite granules.
Claims (3)
1, CNT (carbon nano-tube)/carbon (nitrogen) is changed the preparation method of titanium composite granule, it is characterized in that behind the ilmenite concentrate grinding, put into microwave agglomerating furnace, feed hydrogen and carbon-source gas, carrying out ilmenite reduction handles, the iron catalysis that ilmenite reduction obtains forms CNT (carbon nano-tube), it is titanium carbide that titanium oxide is reduced carbonization, perhaps with behind the ilmenite concentrate grinding, put into microwave agglomerating furnace, feed hydrogen, nitrogen and carbon-source gas carry out ilmenite reduction and handle, the iron catalysis that ilmenite reduction obtains forms CNT (carbon nano-tube), and it is titanium carbonitride that titanium oxide is reduced carbonization.
2, method according to claim 1 is characterized in that the controlled microwave sintering oven is 500-1000 ℃ in CNT (carbon nano-tube) growth phase temperature, and titanium oxide carbonation stage working temperature is 1200-1600 ℃.
3, method according to claim 1 and 2 is characterized in that described carbon-source gas is Sweet natural gas, methane, acetylene, carbon monoxide, ethanol or acetone.
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CNA2008101973578A CN101386407A (en) | 2008-10-23 | 2008-10-23 | Method for preparing nano carbon tube/titanium carbide(nitride) composite powder |
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CNA2008101973578A CN101386407A (en) | 2008-10-23 | 2008-10-23 | Method for preparing nano carbon tube/titanium carbide(nitride) composite powder |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
CN106276939A (en) * | 2016-08-08 | 2017-01-04 | 浙江工业大学之江学院 | A kind of fatty acid amide modified method for preparing organobentonite |
CN106315584A (en) * | 2016-08-29 | 2017-01-11 | 重庆大学 | Method for preparing carbon-doped titanium oxide or/and titanium carbide from titanium-containing mineral or slag |
CN106744960A (en) * | 2016-11-15 | 2017-05-31 | 重庆大学 | A kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction |
CN107416781A (en) * | 2017-07-25 | 2017-12-01 | 华南理工大学 | A kind of two-dimentional titanium nitride carbon nano-tube compound film and preparation method thereof |
CN107555414A (en) * | 2017-09-15 | 2018-01-09 | 佛山科学技术学院 | A kind of garden waste biomass carbon and its production and use |
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2008
- 2008-10-23 CN CNA2008101973578A patent/CN101386407A/en active Pending
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106044771A (en) * | 2016-06-01 | 2016-10-26 | 重庆大学 | Titanium carbide preparation method based on carbonization titanium extraction treatment of titanium-bearing blast furnace slag |
CN106276939A (en) * | 2016-08-08 | 2017-01-04 | 浙江工业大学之江学院 | A kind of fatty acid amide modified method for preparing organobentonite |
CN106276939B (en) * | 2016-08-08 | 2018-01-05 | 浙江工业大学之江学院 | A kind of fatty acid amide modified method for preparing organobentonite |
CN106315584A (en) * | 2016-08-29 | 2017-01-11 | 重庆大学 | Method for preparing carbon-doped titanium oxide or/and titanium carbide from titanium-containing mineral or slag |
CN106744960A (en) * | 2016-11-15 | 2017-05-31 | 重庆大学 | A kind of method that oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction |
CN106744960B (en) * | 2016-11-15 | 2019-01-01 | 重庆大学 | A method of oxidation of coal titanium or/and titanium carbide are prepared with carburetted hydrogen gas reduction |
CN107416781A (en) * | 2017-07-25 | 2017-12-01 | 华南理工大学 | A kind of two-dimentional titanium nitride carbon nano-tube compound film and preparation method thereof |
CN107555414A (en) * | 2017-09-15 | 2018-01-09 | 佛山科学技术学院 | A kind of garden waste biomass carbon and its production and use |
CN107555414B (en) * | 2017-09-15 | 2020-09-29 | 佛山科学技术学院 | Garden waste biomass charcoal and preparation method and application thereof |
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