CN107311149A - A kind of preparation method of CNT - Google Patents
A kind of preparation method of CNT Download PDFInfo
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- CN107311149A CN107311149A CN201710558666.2A CN201710558666A CN107311149A CN 107311149 A CN107311149 A CN 107311149A CN 201710558666 A CN201710558666 A CN 201710558666A CN 107311149 A CN107311149 A CN 107311149A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
Abstract
The present invention proposes a kind of preparation method of CNT, comprises the following steps：Catalyst is added in tube furnace, leads to nitrogen 1L/min, maintaining nitrogen purge；Body of heater is heated up again, 15 DEG C/min of programming rate is warming up to 850 ± 50 DEG C；Then acetylene gas is passed through with 5L/min flow velocity, leads to acetylene gas after 45 minutes, close acetylene；After reaction terminates, take out and lead to acetylene gas after product nanotube, and more catalyst changeout, synthesized, building-up process circulation is carried out；The CNT of preparation, purer nano-tube material is obtained after pickling, washing.The present invention is reduced the synthesis cost of CNT, the yield of catalyst is improved, it is determined that being suitable for the process route of industrialized production using efficient catalyst, the suitable synthetic parameters of selection.
Description
Technical field
The present invention relates to carbon nanotube technology field, more particularly, to a kind of preparation method of CNT.
Background technology
CNT is a kind of a kind of crystal material of carbon by six face carbon planes by axial self assembly curling
Material.Single-walled carbon nanotube and multi-walled carbon nanotube are divided into according to the number of the curved surface number of plies, 3-15 nanometers of single-walled carbon nanotube caliber,
10-30 nanometers of multi-walled carbon nanotube caliber.CNT be applied to Waste tire regeneration processing, lithium battery manufacture, hydrogen storage material,
The fields such as catalyst carrier, high duty metal.
Junked tire processing is always high pollution, an industry for low recovery value, the substantial amounts of junked tire heap of one side
Product such as mountain, but the scrap rubber reclaimed is unable to regeneration, is only used for refining oil, manufactures carbon black etc., is actually by social resources
The utilization of the low recovery of high pollution has been done, the serious wasting of resources is caused.CNT introducing so that the recovery of junked tire turns into
May.After solid recovery glue is well mixed with CNT, tire tread is molded into.This retread mixed with CNT, in reality
Road conditions test data on occupy obvious advantage.The service life of virgin rubber tire is traveling 100,000 according to the regulation of national standard
Kilometer, and mixed with certain proportion CNT retread actual life more than 200,000 kilometers.The test result adds newly respectively
Relevant unit's progress road conditions test of slope and Thailand, has as a result obtained German triumphant rich, green section of Singapore, solid special, U.S. of Italy
The consistent accreditation of the enterprises such as Michelin of state, the Hangzhou China second best plan.
Applications of the CNT in lithium ion battery, can effectively improve pole piece compacted density, improve battery specific energy and
High rate performance so that the discharge and recharge of battery is uniform, and the part for being especially that of avoiding pole piece overcharges phenomenon, significantly improves big times of battery
Security during rate performance and use.Special making on automobile power cell, oily mixed doubles mould tank Vehicular dynamic battery
With the problems such as effectively solving the problems, such as low temperature multiplying power discharging, security.
CNT specific surface area reaches every gram of 225 square meters, and this causes CNT to turn into more satisfactory catalyst carrier material, with
Conventional alumina carrier, iron catalyst carrier etc., which is compared, has obvious advantage.The carrier of phase homogenous quantities can be carried more
Many catalyst particles.
Specific surface area big CNT so that CNT turns into the preferable storage material of hydrogen.The storage and transport of hydrogen be always
The study hotspot of global Hydrogen Energy plan, it is final because failing to find the suitable good method stored with transporting and finally abandon.CNT
Big surface area and to gas very strong adsorption capacity so that CNT turns into a kind of feasible method of hydrogen storage.
The content of the invention
The present invention proposes a kind of preparation method of CNT, is joined using efficient catalyst, the suitable synthesis of selection
Number, reduces the synthesis cost of CNT, the yield of catalyst is improved, it is determined that being suitable for the process route of industrialized production.
The technical proposal of the invention is realized in this way：A kind of preparation method of CNT, comprises the following steps：
S1, catalyst added in tube furnace, lead to nitrogen 1L/min, maintaining nitrogen purge；
S2, body of heater heated up again, 15 DEG C/min of programming rate is warming up to 850 ± 50 DEG C；
S3 and then acetylene gas is passed through with 5L/min flow velocity, leads to acetylene gas after 45 minutes, close acetylene；
After S4, reaction terminate, take out and lead to acetylene gas after product nanotube, and more catalyst changeout, synthesized, synthesize
Process circulation is carried out；
S5, the CNT prepared, purer nano-tube material is obtained after pickling, washing.
As a kind of perferred technical scheme, the catalyst be nickel protoxide powder, the compound powder containing copper or
In metallic iron powder, Co2O3, Al2O3, MgO, the compound powder containing ferro element or metallic iron powder any one or it is any
Several mixtures.
As a kind of perferred technical scheme, the catalyst includes by weight percentage：23-45.2 nickel protoxide
Powder, the 0.5-6.0 compound powder or metallic copper powder containing copper, 3.0-15.0Co2O3,6.9-9.3 Al2O3,
11.5-68.4 MgO, 3-45 compound powder or metallic iron powder containing ferro element.
As a kind of perferred technical scheme, the preparation method of the catalyst comprises the following steps：
1) by 23-45.2 grams of nickel protoxide powder, 0.5-6.0 grams of compound powder or metallic copper powder containing copper,
3.0-15.0 grams of Co2O3 powder is added in mixing apparatus, is sufficiently mixed；
2) well mixed mixed powder is sent into atmosphere furnace, under the protection of protective gas, in 900 ± 20 DEG C of temperature
Under be sintered, sintering time 3 hours；
3) mixture after sintering is added in ball grinder, weighs 6.9-9.3 grams of aluminum oxide, weigh magnesia 11.5-
68.4 grams, weigh the compound powder containing ferro element or 3-45 grams of metallic iron powder is added in ball grinder, grind uniform together, mix
Sifted out after closing uniformly, as catalyst.
As a kind of perferred technical scheme, the compound powder or metallic iron powder containing ferro element can be Fe
Any of powder, Fe2O3, Fe3O4 or FeS.
As a kind of perferred technical scheme, the compound powder or metallic copper powder containing copper can be Cu
Any of powder, CuO powder or CuS powder.
As a kind of perferred technical scheme, the protective gas can be any of nitrogen, argon gas and hydrogen.
As a kind of perferred technical scheme, as described in requiring 4, the protective gas air velocity be 0.1L/min-
50L/min。
As a kind of perferred technical scheme, as described in requiring 4, synthesis temperature can be 460 DEG C -- 1350 DEG C.
Above-mentioned technical proposal is employed, beneficial effects of the present invention are：The unstrpped gas of the present invention is split using junked tire
The carbonaceous gas such as waste gas, methane, ethene, acetylene, second diene, carbon monoxide are solved, catalyst uses nickel powder, copper powder, cobalt oxide powder
Deng.The building-up process of CNT, is to use tube furnace mostly, the use of acetylene, hydrogen or nitrogen is diluent gas, using nickel
The mixtures such as powder, cobalt oxide powder, copper powder or alloy carry out the synthesis of CNT as catalyst.Building-up process is substantially all
It is that single is carried out, for laboratory operation, it is impossible to carry out mass production.Using the program, the production of every gram of mixed catalyst
Rate reaches 37.5 grams, catalyst efficiency high, and catalyst production and production efficiency meet the requirement of industrialized production.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example only a part of embodiment of the invention, rather than whole embodiments.Based on the embodiment in the present invention, this area is common
The every other embodiment that technical staff is obtained under the premise of creative work is not made, belongs to the model that the present invention is protected
Enclose.
Embodiment one
In the present embodiment, the purity of nickel powder is pure, the granularity ＜ 3um of chemistry.The purity of copper powder is pure, the granularity ＜ 3um of chemistry.
The purity of cobalt oxide point is pure, the granularity ＜ 15um of chemistry.The purity of aluminum oxide is pure, the granularity ＜ 15um of chemistry.Magnesia it is pure
Spend for pure, the granularity ＜ 15um of chemistry.
A kind of preparation method of CNT, comprises the following steps：Catalyst is added in tube furnace, leads to nitrogen 1L/
Min, maintaining nitrogen purge；Body of heater is heated up again, 15 DEG C/min of programming rate is warming up to 800 DEG C；Then it is logical with 5L/min flow velocity
Enter acetylene gas, lead to acetylene gas after 45 minutes, close acetylene；After reaction terminates, product nanotube is taken out, and change catalysis
Lead to acetylene gas after agent, synthesized, 460 DEG C of synthesis temperature, building-up process circulation is carried out；The CNT of preparation, through pickling,
Purer nano-tube material is obtained after washing.
The preparation method of catalyst comprises the following steps：
1) by 23 grams of nickel protoxide powder, 0.5 gram of Cu powder, 3.0 grams of Co2O3 powder are added in mixing apparatus, are sufficiently mixed；
2) well mixed mixed powder is sent into atmosphere furnace, under the protection of protective gas nitrogen, protective gas air-flow
Speed is that 0.1L/min is sintered at a temperature of 880 DEG C, sintering time 3 hours；
3) mixture after sintering is added in ball grinder, weighs 6.9 grams of aluminum oxide, weigh 11.5 grams of magnesia, weigh
3 grams of Fe powder is added in ball grinder, is ground uniform together, is sifted out after being well mixed, as catalyst.
Embodiment two
In the present embodiment, the purity of nickel powder is pure, the granularity ＜ 3um of chemistry.The purity of copper powder is pure, the granularity ＜ 3um of chemistry.
The purity of cobalt oxide point is pure, the granularity ＜ 15um of chemistry.The purity of aluminum oxide is pure, the granularity ＜ 15um of chemistry.Magnesia it is pure
Spend for pure, the granularity ＜ 15um of chemistry.
A kind of preparation method of CNT, comprises the following steps：Catalyst is added in tube furnace, leads to nitrogen 1L/
Min, maintaining nitrogen purge；Body of heater is heated up again, 15 DEG C/min of programming rate is warming up to 850 DEG C；Then it is logical with 5L/min flow velocity
Enter acetylene gas, lead to acetylene gas after 45 minutes, close acetylene；After reaction terminates, product nanotube is taken out, and change catalysis
Lead to acetylene gas after agent, synthesized, synthesis temperature can be 900 DEG C, building-up process circulation is carried out；The CNT of preparation,
Purer nano-tube material is obtained after pickling, washing.
The preparation method of catalyst comprises the following steps：
1) by 30 grams of nickel protoxide powder, 3.0 grams of CuO powder, 10.0 grams of Co2O3 powder are added in mixing apparatus, fully mix
Close；
2) well mixed mixed powder is sent into atmosphere furnace, under the protection of protective gas argon gas, protective gas air-flow
Speed is 10L/min, is sintered at a temperature of 900 DEG C, sintering time 3 hours；
3) mixture after sintering is added in ball grinder, weighs 8.0 grams of aluminum oxide, weigh 20.0 grams of magnesia, weigh
15 grams of Fe2O3 are added in ball grinder, are ground uniform together, are sifted out after being well mixed, as catalyst.
Embodiment three
In the present embodiment, the purity of nickel powder is pure, the granularity ＜ 3um of chemistry.The purity of copper powder is pure, the granularity ＜ 3um of chemistry.
The purity of cobalt oxide point is pure, the granularity ＜ 15um of chemistry.The purity of aluminum oxide is pure, the granularity ＜ 15um of chemistry.Magnesia it is pure
Spend for pure, the granularity ＜ 15um of chemistry.
A kind of preparation method of CNT, comprises the following steps：Catalyst is added in tube furnace, leads to nitrogen 1L/
Min, maintaining nitrogen purge；Body of heater is heated up again, 15 DEG C/min of programming rate is warming up to 900 DEG C；Then it is logical with 5L/min flow velocity
Enter acetylene gas, lead to acetylene gas after 45 minutes, close acetylene；After reaction terminates, product nanotube is taken out, and change catalysis
Lead to acetylene gas after agent, synthesized, 1350 DEG C of synthesis temperature, building-up process circulation is carried out；The CNT of preparation, through acid
Wash, wash after obtain purer nano-tube material.
The preparation method of catalyst comprises the following steps：
1) by 45.2 grams of nickel protoxide powder, 6.0 grams of CuS, 15.0 grams of Co2O3 powder are added in mixing apparatus, fully mix
Close；
2) well mixed mixed powder is sent into atmosphere furnace, under the protection of protective gas hydrogen, protective gas air-flow
Speed is 50L/min, is sintered at a temperature of 920 DEG C, sintering time 3 hours；
3) mixture after sintering is added in ball grinder, weighs 9.3 grams of aluminum oxide, weigh 68.4 grams of magnesia, weigh
45 grams of Fe3O4 are added in ball grinder, are ground uniform together, are sifted out after being well mixed, as catalyst.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (9)
1. a kind of preparation method of CNT, it is characterised in that comprise the following steps：
S1, catalyst added in tube furnace, lead to nitrogen 1L/min, maintaining nitrogen purge；
S2, body of heater heated up again, 15 DEG C/min of programming rate is warming up to 850 ± 50 DEG C；
S3 and then acetylene gas is passed through with 5L/min flow velocity, leads to acetylene gas after 45 minutes, close acetylene；
After S4, reaction terminate, take out and lead to acetylene gas after product nanotube, and more catalyst changeout, synthesized, building-up process
Circulation is carried out；
S5, the CNT prepared, purer nano-tube material is obtained after pickling, washing.
2. a kind of preparation method of CNT as claimed in claim 1, it is characterised in that the catalyst is nickel protoxide
Powder, the compound powder containing copper or metallic iron powder, Co2O3, Al2O3, MgO, compound powder or gold containing ferro element
Belong to any one in iron powder or any several mixture.
3. a kind of preparation method of CNT as claimed in claim 1, it is characterised in that catalyst percentage by weight
Than including：23-45.2 nickel protoxide powder, the 0.5-6.0 compound powder or metallic copper powder containing copper, 3.0-
15.0Co2O3,6.9-9.3 Al2O3,11.5-68.4 MgO, 3-45 compound powder or metal iron powder containing ferro element
End.
4. a kind of preparation method of CNT as claimed in claim 1, it is characterised in that the preparation method of the catalyst
Comprise the following steps：
1) by 23-45.2 grams of nickel protoxide powder, 0.5-6.0 grams of compound powder or metallic copper powder containing copper, 3.0-
15.0 grams of Co2O3 powder are added in mixing apparatus, are sufficiently mixed；
2) well mixed mixed powder is sent into atmosphere furnace, under the protection of protective gas, entered at a temperature of 900 ± 20 DEG C
Row sintering, sintering time 3 hours；
3) mixture after sintering is added in ball grinder, weighs 6.9-9.3 grams of aluminum oxide, weigh 11.5-68.4 grams of magnesia,
Weigh the compound powder containing ferro element or 3-45 grams of metallic iron powder is added in ball grinder, grind uniform together, be well mixed
After sift out, as catalyst.
5. a kind of preparation method of CNT as claimed in claim 2, it is characterised in that the compound containing ferro element
Powder or metallic iron powder can be any of Fe powder, Fe2O3, Fe3O4 or FeS.
6. a kind of preparation method of CNT as claimed in claim 2, it is characterised in that the compound containing copper
Powder or metallic copper powder can be any of Cu powder, CuO powder or CuS powder.
7. a kind of preparation method of CNT as claimed in claim 4, it is characterised in that the protective gas can be nitrogen
Gas, argon gas and hydrogen it is any.
8. a kind of preparation method of CNT as claimed in claim 4, it is characterised in that as described in requiring 4, the protection
Gas flow speed is 0.1L/min -50L/min.
9. a kind of preparation method of CNT as claimed in claim 1, it is characterised in that as described in requiring 4, synthesis temperature
Can be 460 DEG C -- 1350 DEG C.
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| CN201710558666.2A CN107311149A (en) | 2017-07-11 | 2017-07-11 | A kind of preparation method of CNT |
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| CN201710558666.2A CN107311149A (en) | 2017-07-11 | 2017-07-11 | A kind of preparation method of CNT |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN110844900A (en) * | 2019-11-11 | 2020-02-28 | 天津大学 | Method for preparing carbon nano tube by taking waste tire as raw material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804355A (en) * | 2009-02-13 | 2010-08-18 | 锦湖石油化学株式会社 | Catalyst composition for the synthesis of thin multi-walled carbon nanotube and its manufacturing method |
| CN105964268A (en) * | 2016-05-17 | 2016-09-28 | 深圳市河科科技有限公司 | Metal catalyst preparation method and preparation method of carbon nanotube |
-
2017
- 2017-07-11 CN CN201710558666.2A patent/CN107311149A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804355A (en) * | 2009-02-13 | 2010-08-18 | 锦湖石油化学株式会社 | Catalyst composition for the synthesis of thin multi-walled carbon nanotube and its manufacturing method |
| CN105964268A (en) * | 2016-05-17 | 2016-09-28 | 深圳市河科科技有限公司 | Metal catalyst preparation method and preparation method of carbon nanotube |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN110252304B (en) * | 2018-03-12 | 2021-12-17 | 中国石油化工股份有限公司 | Iron-based catalyst, preparation method and application thereof, carbon nano tube and preparation method thereof |
| CN110844900A (en) * | 2019-11-11 | 2020-02-28 | 天津大学 | Method for preparing carbon nano tube by taking waste tire as raw material |
| CN110844900B (en) * | 2019-11-11 | 2022-05-24 | 天津大学 | Method for preparing carbon nano tube by taking waste tire as raw material |
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