CN107099059A - A kind of hydroxyethyl cellulose for humidity-sensitive material is combined mixed liquor of nitration mixture modifying multiwall carbon nano-tube and preparation method thereof - Google Patents
A kind of hydroxyethyl cellulose for humidity-sensitive material is combined mixed liquor of nitration mixture modifying multiwall carbon nano-tube and preparation method thereof Download PDFInfo
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- CN107099059A CN107099059A CN201710328396.6A CN201710328396A CN107099059A CN 107099059 A CN107099059 A CN 107099059A CN 201710328396 A CN201710328396 A CN 201710328396A CN 107099059 A CN107099059 A CN 107099059A
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- nitration mixture
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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Abstract
The invention discloses the mixed liquor that a kind of hydroxyethyl cellulose for humidity-sensitive material is combined nitration mixture modifying multiwall carbon nano-tube, and its preparation technology, it is characterised in that, nitration mixture is added into multi-walled carbon nanotube, constant temperature oil bath flows back, then freeze-day with constant temperature, obtains the multi-walled carbon nanotube of nitration mixture modification；Add deionized water into polyvinylpyrrolidone, stir to being completely dissolved, obtain surfactant solution；Plus the multi-walled carbon nanotube of nitration mixture modification, continue after stirring, be placed in ultrasonic cell disintegration instrument ultrasonic, centrifugation, obtain carbon nano tube dispersion liquid；Deionized water is added into the dispersion liquid of multi-walled carbon nanotube, magnetic agitation is disperseed, add hydroxyethyl cellulose, then magnetic agitation, obtain uniform mixed liquor.
Description
Technical field
The present invention relates to temperature sensing material field, and in particular to a kind of hydroxyethyl cellulose for humidity-sensitive material is combined nitration mixture
The mixed liquor of modifying multiwall carbon nano-tube, and its preparation technology.
Background technology
Production, the life of ambient humidity and people are closely bound up, and as easy moisture detection device, humidity sensor is
Through being widely used in the fields such as industry, agricultural, medical treatment, meteorology, electronics, aviation.Humidity-sensitive material is the core of humidity sensor
Part, oneself warp of Development of Novel wet sensory material turns into the emphasis that people study.Multi-walled carbon nanotube is that one kind of sensor field is new
Section bar material, with unique characterization of adsorption, humidity sensor of the research based on multi-walled carbon nanotube is to development of new humidity sensor
Device and widen its application field there is practical significance.
The content of the invention
The present invention solves the technical problem of provide a kind of hydroxyethyl cellulose for humidity-sensitive material to be combined nitration mixture
The mixed liquor and its preparation technology of modifying multiwall carbon nano-tube, have good temperature sensitive spy according to mixed liquor prepared by the technique
Property.
The technical problems to be solved by the invention are realized using following technical scheme：
A kind of hydroxyethyl cellulose for humidity-sensitive material is combined the preparation method of the mixed liquor of nitration mixture modifying multiwall carbon nano-tube,
Characterized in that, carrying out according to the following steps：
A. into 5-10 parts by weight multi-walled carbon nanotubes 1:5-10 adds nitration mixture, is warming up to 130-150 DEG C of constant temperature oil bath backflow 1-
2h, then in 50-60 DEG C of freeze-day with constant temperature 2-4h, obtains the multi-walled carbon nanotube of nitration mixture modification；
B. ultrasonic disperse technique：Into 8-15 weight account polyethylene pyrrolidones 1:5-10 adds deionized water, uses magnetic stirring apparatus
Stirring obtains surfactant solution to being completely dissolved；The multi-walled carbon nanotube of gained nitration mixture modification in a is added, continues to use magnetic force
After agitator stirring 10-20min, ultrasound 30-40min in ultrasonic cell disintegration instrument is placed in, 20-30min is centrifuged, obtains many wall carbon
The dispersion liquid of nanotube；
C. into b 1 in the dispersion liquid of resultant multi-wall CNT:15-20 adds deionized water, and magnetic agitation disperses 20-
30min, adds 20-30 parts by weight hydroxyethyl celluloses, then magnetic agitation 20-30min, obtains uniform mixed liquor.
Wherein, nitration mixture described in step a is the concentrated sulfuric acid, concentrated nitric acid with volume ratio 3:1-2 is mixed.In step b
The centrifugal speed is 2000-3000rpm.
The reaction mechanism of the present invention is as follows：
Nitration mixture modification is carried out to multi-walled carbon nanotube with the concentrated sulfuric acid-concentrated nitric acid, multi-walled carbon nanotube is improved in water and ethoxy
Dispersiveness in cellulose, is conducive to improving the wet sensitive performance of composite.Multi-walled carbon nanotube (MWCNT) has high major diameter
Than being added in composite has fiber reinforced and nano-filled characteristic, and gained composite has high intensity, height
Volume stability and high permeability resistance；With nonionic surface active agent polyvinylpyrrolidone (PVP) for modifying agent, with reference to super
Sound dispersing technology is good to MWCNT dispersion effect, significantly improves the mechanical property of composite.
Embodiment
In order that the technical means, the inventive features, the objects and the advantages of the present invention are easy to understand, tie below
Specific embodiment is closed, the present invention is expanded on further.
Embodiment
A kind of hydroxyethyl cellulose for humidity-sensitive material is combined the preparation of the mixed liquor of nitration mixture modifying multiwall carbon nano-tube
Method, it is characterised in that carry out according to the following steps：
A. into 10kg multi-walled carbon nanotubes 1:5 add nitration mixture, are warming up to 140-150 DEG C of constant temperature oil bath backflow 1h, Ran Hou
50-60 DEG C of freeze-day with constant temperature 2h, obtains the multi-walled carbon nanotube of nitration mixture modification；
B. ultrasonic disperse technique：Into 15kg polyvinylpyrrolidones 1:10 plus deionized water, with magnetic stirrer to complete
Fully dissolved, obtains surfactant solution；The multi-walled carbon nanotube of gained nitration mixture modification in a is added, continuation is stirred with magnetic stirring apparatus
Mix after 20min, be placed in ultrasound 40min in ultrasonic cell disintegration instrument, centrifuge 30min, obtain the dispersion liquid of multi-walled carbon nanotube；
C. into b 1 in the dispersion liquid of resultant multi-wall CNT:20 add deionized water, and magnetic agitation disperses 30min, add
30kg hydroxyethyl celluloses, then magnetic agitation 30min, obtain uniform mixed liquor.
Wherein, nitration mixture described in step a is the concentrated sulfuric acid, concentrated nitric acid with volume ratio 3:2 mixing.In step b
The centrifugal speed is 3000rpm.
Claims (4)
1. a kind of hydroxyethyl cellulose for humidity-sensitive material is combined the mixed liquor of nitration mixture modifying multiwall carbon nano-tube, its feature exists
In：
Nitration mixture is added into multi-walled carbon nanotube, constant temperature oil bath flows back, then freeze-day with constant temperature, many wall carbon for obtaining nitration mixture modification are received
Mitron；Add deionized water into polyvinylpyrrolidone, stir to being completely dissolved, obtain surfactant solution；Plus nitration mixture modification
Multi-walled carbon nanotube, continue after stirring, be placed in ultrasonic cell disintegration instrument ultrasonic, centrifugation, obtain carbon nano tube dispersion liquid；To
Deionized water is added in the dispersion liquid of multi-walled carbon nanotube, magnetic agitation is disperseed, adds hydroxyethyl cellulose, then magnetic agitation,
Be uniformly mixed liquid.
2. a kind of hydroxyethyl cellulose for humidity-sensitive material according to claim 1 is combined nitration mixture modifying multiwall carbon nanometer
The preparation method of the mixed liquor of pipe, it is characterised in that carry out according to the following steps：
A. into 5-10 parts by weight multi-walled carbon nanotubes 1:5-10 adds nitration mixture, is warming up to 130-150 DEG C of constant temperature oil bath backflow 1-
2h, then in 50-60 DEG C of freeze-day with constant temperature 2-4h, obtains the multi-walled carbon nanotube of nitration mixture modification；
B. ultrasonic disperse technique：Into 8-15 weight account polyethylene pyrrolidones 1:5-10 adds deionized water, uses magnetic stirring apparatus
Stirring obtains surfactant solution to being completely dissolved；The multi-walled carbon nanotube of gained nitration mixture modification in a is added, continues to use magnetic force
After agitator stirring 10-20min, ultrasound 30-40min in ultrasonic cell disintegration instrument is placed in, 20-30min is centrifuged, obtains many wall carbon
The dispersion liquid of nanotube；
C. into b 1 in the dispersion liquid of resultant multi-wall CNT:15-20 adds deionized water, and magnetic agitation disperses 20-
30min, adds 20-30 parts by weight hydroxyethyl celluloses, then magnetic agitation 20-30min, obtains uniform mixed liquor.
3. a kind of hydroxyethyl cellulose for humidity-sensitive material according to claim 2 is combined nitration mixture modifying multiwall carbon nanometer
The preparation method of the mixed liquor of pipe, it is characterised in that nitration mixture described in step a is the concentrated sulfuric acid, concentrated nitric acid with volume ratio 3:1-2 is mixed
Close.
4. a kind of hydroxyethyl cellulose for humidity-sensitive material according to claim 2 is combined nitration mixture modifying multiwall carbon nanometer
The preparation method of the mixed liquor of pipe, it is characterised in that centrifugal speed described in step b is 2000-3000rpm.
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| CN201710328396.6A CN107099059A (en) | 2017-05-11 | 2017-05-11 | A kind of hydroxyethyl cellulose for humidity-sensitive material is combined mixed liquor of nitration mixture modifying multiwall carbon nano-tube and preparation method thereof |
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| CN201710328396.6A CN107099059A (en) | 2017-05-11 | 2017-05-11 | A kind of hydroxyethyl cellulose for humidity-sensitive material is combined mixed liquor of nitration mixture modifying multiwall carbon nano-tube and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107902640A (en) * | 2017-11-22 | 2018-04-13 | 河北工业大学 | A kind of preparation method of boron nitride cladding multi-walled carbon nanotube |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219925A (en) * | 2011-05-17 | 2011-10-19 | 太原理工大学 | Surface modification method of multi-walled carbon nanotubes |
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2017
- 2017-05-11 CN CN201710328396.6A patent/CN107099059A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219925A (en) * | 2011-05-17 | 2011-10-19 | 太原理工大学 | Surface modification method of multi-walled carbon nanotubes |
Non-Patent Citations (2)
| Title |
|---|
| 王国建等: "《功能高分子材料》", 31 January 2010, 同济大学出版社 * |
| 王大月: "多壁碳纳米管/羟乙基纤维素复合材料的湿敏特性及应用研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107902640A (en) * | 2017-11-22 | 2018-04-13 | 河北工业大学 | A kind of preparation method of boron nitride cladding multi-walled carbon nanotube |
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