CN103395770A - Preparation method for stable carbon nanotube aqueous dispersion - Google Patents
Preparation method for stable carbon nanotube aqueous dispersion Download PDFInfo
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- CN103395770A CN103395770A CN2013103309135A CN201310330913A CN103395770A CN 103395770 A CN103395770 A CN 103395770A CN 2013103309135 A CN2013103309135 A CN 2013103309135A CN 201310330913 A CN201310330913 A CN 201310330913A CN 103395770 A CN103395770 A CN 103395770A
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Abstract
The invention belongs to the technical field of carbon nanotubes, and specifically relates to a preparation method for a stable carbon nanotube aqueous dispersion. In the preparation method, no concentrated acid is used to pretreat carbon nanotubes, thereby causing no chemical damage to the carbon nanotubes and generating no pollutants such as wastewater, waste acid and the like. The preparation method is simple in process. The prepared carbon nanotubes are dispersed well in water and have high stability. Besides, no obvious bubble is introduced; and the problems of damage on the carbon nanotubes, generation of pollutants such as wastewater, waste acid and the like, and poor dispersity and stability which are caused by a conventional dispersion technology can be prevented.
Description
Technical field
The invention belongs to the technical field of carbon nanotube, be specially a kind of preparation method of stable carbon nano-tube aqueous dispersion.
Background technology
Carbon nanotube is a kind of nano material, owing to there being powerful intermolecular Van der Waals force, very easily reunites, and affects its dispersion in aqueous solution.
At present, the dispersion technology of carbon nanotube in water mainly contains following several situation: 1) by carbon nanotube in the situation that add water reducer to carry out ultrasonic dispersion, the advantage of this technology is that technique is simple, but dispersion effect is not good.2) by carbon nanotube in the situation that add the dispersion agent such as sodium laurylsulfonate to carry out ultrasonic dispersion, the advantage of this technology is also that technique is simple, but exist, introduces more bubble and the shortcomings such as dispersion effect and less stable.3) carbon nanotube is soaked or hydro-thermal reaction under concentrated acid, then with alkali, neutralize, the techniques such as washing are carried out pre-treatment, pretreated carbon nanotube adds dispersion agent to carry out ultrasonic dispersion again, application number is that 2011104366206 patent documentation discloses a kind of high-concentration carbon nano tube water dispersoid and preparation method thereof, its preparation method is carbon nanotube dense mineral acid kind soaking at room temperature at least 10 hours, then ultra-sonic oscillation are at least 2 hours, finally with sodium hydroxide solution, be neutralized to pH less than or equal to 6, separate, washing to neutral rear drying obtains the pre-treatment carbon nanotube.The pre-treatment carbon nanotube dispersed is just obtained to high-concentration carbon nano tube water dispersoid half an hour at least in the deionized water kind that contains dispersion agent ultra-sonic oscillation, can stablize and deposit at least one year.The advantage of the method is that dispersiveness and stability are better, but the carbon nanotube after acid treatment is subjected to damage to a certain extent, affects its result of use, and complex process, also can produce the pollutents such as waste water, spent acid.
Summary of the invention
The object of the invention is to for the defect of above-mentioned existence and a kind of preparation method of stable carbon nano-tube aqueous dispersion is provided.Do not adopt concentrated acid to carry out pre-treatment to carbon nanotube, can not cause chemical damage to carbon nanotube, do not produce the pollutents such as any waste water, spent acid, technique is simple, good dispersity, stability in water are high, and it is not obvious to introduce bubble, and having solved existing dispersion technology can be to the carbon nanotube injury, produce the problems such as pollutent, dispersiveness and the stabilitys such as waste water, spent acid are poor.
Technical scheme of the present invention is:
A kind of preparation method of stable carbon nano-tube aqueous dispersion, step is as follows:
A. the polycarboxylate water-reducer of 0.1-0.5 weight part is added in the water of 20-100 weight part, mechanical stirring 1-3min, the dispersion agent that adds the 1-2 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Described polycarboxylate water-reducer is 0.3 weight part.
Described dispersion agent is polyethylene or methyl-2-pyrrolidone.
Described preparation method carries out under normal temperature condition.
A kind of preparation method of stable carbon nano-tube aqueous dispersion, carry out under normal temperature condition, step is as follows:
A. the polycarboxylate water-reducer of 0.1-0.5 weight part is added in the water of 20-100 weight part, mechanical stirring 1-3min, the polyethylene or the methyl-2-pyrrolidone that add the 1-2 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
A kind of preparation method of stable carbon nano-tube aqueous dispersion, step is as follows:
A. the dispersion agent of 1-2 weight part is added in the water of 20-100 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Described dispersion agent is poly-is ethene or methyl-2-pyrrolidone.
Described preparation method carries out under normal temperature condition.
A kind of preparation method of stable carbon nano-tube aqueous dispersion, carry out under normal temperature condition, step is as follows:
A. the ethene of 1-2 weight part or methyl-2-pyrrolidone are added in the water of 20-100 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Beneficial effect of the present invention is:
1, do not need to adopt the solution such as concentrated acid to carry out pre-treatment, the damage of having avoided concentrated acid to cause carbon nanotube structure, can not produce the secondary pollutants such as waste water, spent acid simultaneously, and whole preparation method has simplified schedule of operation.
2, the bubble of this dispersion technology introducing is less.
3, the carbon nanotube concentration of aqueous liquid dispersion is higher, can be up to 2-5%, and the dispersiveness of carbon nanotube in the aqueous solution is better, and dispersity can reach more than 95%, the good stability of carbon nanotube aqueous liquid dispersion, but stable storage is more than 2 years.
Embodiment
Below by specific embodiment, technical scheme of the present invention is described in detail.
The present invention's polycarboxylate water-reducer used blocks purchased from the Germany west, and solid content is 40%.
Embodiment 1
A. the polycarboxylate water-reducer of 0.3 part is added in the water of 50 parts, mechanical stirring 1-3min, add the polyethylene of 1 part, and magnetic agitation 1-2min, after being uniformly dispersed, add 1 part of carbon nanotube, continues magnetic agitation 1-2min, obtains containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 60min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 2
A. the polycarboxylate water-reducer of 0.1 part is added in the water of 20 parts, mechanical stirring 1-3min, add the methyl-2-pyrrolidone of 2 parts, magnetic agitation 1-2min, after being uniformly dispersed, add 1 part of carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 3
A. the polycarboxylate water-reducer of 0.15 part is added in the water of 30 parts, mechanical stirring 1-3min, add the methyl-2-pyrrolidone of 1 part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 part of carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 120min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 4
A. the polycarboxylate water-reducer of 0.5 part is added in the water of 100 parts, mechanical stirring 3min, add the polyethylene of 1 part, and magnetic agitation 1min, after being uniformly dispersed, add 1 part of carbon nanotube, continues magnetic agitation 2min, obtains containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 70min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 5
A. the polycarboxylate water-reducer of 0.2 part is added in the water of 40 parts, mechanical stirring 1min, add the polyethylene of 2 parts, and magnetic agitation 2min, after being uniformly dispersed, add 1 part of carbon nanotube, continues magnetic agitation 2min, obtains containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 90min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 6
A. the polycarboxylate water-reducer of 0.4 part is added in the water of 80 parts, mechanical stirring 3min, add the polyethylene of 2 parts, and magnetic agitation 1min, after being uniformly dispersed, add 1 part of carbon nanotube, continues magnetic agitation 2min, obtains containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 100min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 7
A. the polycarboxylate water-reducer of 0.35 part is added in the water of 60 parts, mechanical stirring 3min, add the polyethylene of 1 part, and magnetic agitation 1min, after being uniformly dispersed, add 1 part of carbon nanotube, continues magnetic agitation 2min, obtains containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
Embodiment 8
A. the polyvinylpyrrolidone of 1 part is added in the water of 100 parts, magnetic agitation 1-2min, after being uniformly dispersed, add 1 part of carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 30min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Embodiment 9
A. the methyl-2-pyrrolidone of 2 parts is added in the water of 20 parts, magnetic agitation 2min, after being uniformly dispersed, add 1 part of carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 120min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Embodiment 10
A. the methyl-2-pyrrolidone of 1 part is added in the water of 80 parts, magnetic agitation 2min, after being uniformly dispersed, add 1 part of carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 70min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Embodiment 11
A. the methyl-2-pyrrolidone of 2 parts is added in the water of 90 parts, magnetic agitation 1min, after being uniformly dispersed, add 1 part of carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 40min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
Claims (9)
1. the preparation method of a stable carbon nano-tube aqueous dispersion, step is as follows:
A. the polycarboxylate water-reducer of 0.1-0.5 weight part is added in the water of 20-100 weight part, mechanical stirring 1-3min, the dispersion agent that adds the 1-2 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
2. preparation method according to claim 1, is characterized in that, described polycarboxylate water-reducer is 0.3 weight part.
3. preparation method according to claim 1, is characterized in that, described dispersion agent is polyethylene or methyl-2-pyrrolidone.
4. preparation method according to claim 1, is characterized in that, described preparation method carries out under normal temperature condition.
5. the preparation method of a stable carbon nano-tube aqueous dispersion, carry out under normal temperature condition, and step is as follows:
A. the polycarboxylate water-reducer of 0.1-0.5 weight part is added in the water of 20-100 weight part, mechanical stirring 1-3min, the polyethylene or the methyl-2-pyrrolidone that add the 1-2 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube, continue magnetic agitation 1-2min, obtain containing the dispersion liquid of carbon nanotube;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, obtains the stable carbon nano-tube aqueous dispersion of polymolecularity.
6. the preparation method of a stable carbon nano-tube aqueous dispersion, step is as follows:
A. the dispersion agent of 1-2 weight part is added in the water of 20-100 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
7. preparation method according to claim 6, is characterized in that, described dispersion agent is poly-is ethene or methyl-2-pyrrolidone.
8. preparation method according to claim 6, is characterized in that, described preparation method carries out under normal temperature condition.
9. the preparation method of a stable carbon nano-tube aqueous dispersion, carry out under normal temperature condition, and step is as follows:
A. the ethene of 1-2 weight part or methyl-2-pyrrolidone are added in the water of 20-100 weight part, magnetic agitation 1-2min, after being uniformly dispersed, add 1 weight part carbon nanotube in dispersion liquid, continues magnetic agitation 1-2min;
The dispersion liquid that b. will contain carbon nanotube disperses 30-120min with ultrasonic scattering method, just can obtain the carbon nanotube aqueous dispersion of polymolecularity.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691280A (en) * | 2009-10-30 | 2010-04-07 | 上海交通大学 | Method for preparing carbon nano tube film |
| CN102172488A (en) * | 2010-12-17 | 2011-09-07 | 哈尔滨工业大学 | Carbon nano tube/carbon nano fiber dispersing method |
| CN103189310A (en) * | 2010-10-08 | 2013-07-03 | 拜耳知识产权有限责任公司 | Production of dispersions containing carbon nanotubes |
-
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- 2013-08-01 CN CN2013103309135A patent/CN103395770A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101691280A (en) * | 2009-10-30 | 2010-04-07 | 上海交通大学 | Method for preparing carbon nano tube film |
| CN103189310A (en) * | 2010-10-08 | 2013-07-03 | 拜耳知识产权有限责任公司 | Production of dispersions containing carbon nanotubes |
| CN102172488A (en) * | 2010-12-17 | 2011-09-07 | 哈尔滨工业大学 | Carbon nano tube/carbon nano fiber dispersing method |
Non-Patent Citations (1)
| Title |
|---|
| 张姣龙等: "碳纳米管在水泥基复合材料中的分散性研究", 《武汉理工大学学报》, vol. 34, no. 5, 31 May 2012 (2012-05-31), pages 6 - 9 * |
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Application publication date: 20131120 |