CN105819514A - Chromic material, preparation method thereof, and early warning cable sheath - Google Patents
Chromic material, preparation method thereof, and early warning cable sheath Download PDFInfo
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- CN105819514A CN105819514A CN201610116011.5A CN201610116011A CN105819514A CN 105819514 A CN105819514 A CN 105819514A CN 201610116011 A CN201610116011 A CN 201610116011A CN 105819514 A CN105819514 A CN 105819514A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/02—Polyamines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/32—Insulated conductors or cables characterised by their form with arrangements for indicating defects, e.g. breaks or leaks
- H01B7/324—Insulated conductors or cables characterised by their form with arrangements for indicating defects, e.g. breaks or leaks comprising temperature sensing means
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Electrochromic Elements, Electrophoresis, Or Variable Reflection Or Absorption Elements (AREA)
Abstract
The invention provides a chromic material, a preparation method thereof, and an early warning cable sheath. The preparation method of the chromic material comprises the following steps: adding a quantified amount of ammonium acetate to a tungsten and hydrogen peroxide mixed solution as an additive to prepare precursor powder, and carrying out heat treatment on the precursor powder to obtain the prepared chromic material tungsten trioxide have a rod-shaped shape, wherein a distance between two remote points in the cross section of the rod-shaped tungsten trioxide, vertical to the axial direction, is 10-20nm, and the length of the rod-shaped WO3 reaches 2-10[mu]m. The rod-shaped tungsten trioxide has the advantages of large specific surface area, difficult aggregation, stable performances, and can be directly doped in the outer sheath material of the early warning cable sheath to simplify the production technology of the early warning cable sheath, and the early warning cable sheath obtained in the invention has a good early warning effect.
Description
Technical field
The present invention relates to off-color material field, particularly relate to a kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing).
Background technology
Along with expanding economy, electricity has become as the requisite energy in daily life, and Electrical Safety is also subject to people's attention, the various early warning cables defeated in particular for fax arise at the historic moment, as: patent CN201220569716.X discloses a kind of early warning cable, including conductor, coating conductor screen layer, insulating barrier, insulation screen, inner sheath, oversheath the most inside-out outside conductor, and at oversheath outsourcing heat discoloration luminescence sheath；Its operation principle is: when cable leak electricity, short circuit or long-term g-load run time, cable local temperature raises, cable surface sheath raises at noctilucence along with temperature, there is the phenomenon that color changes daytime, to remind people's cable to break down, allow one in time away from trouble location and report cable maintenance person to solve fault in time.But, this early warning cable needs individually to set up photochromic layer, complicated process of preparation, and therefore, seeking the early warning cable joint-box that a kind of preparation technology is simple and early warning is effective is to be presently required to solve the technical problem that.
Summary of the invention
In view of this, the technical problem to be solved there are provided a kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing), the off-color material that the present invention provides is applied to the preparation of early warning cable, not only preparation method is simple, and the early warning of the early warning cable prepared is effective.
The invention provides the preparation method of a kind of off-color material of the present invention, including:
1) tungsten powder is mixed with hydrogen peroxide, obtain mixed solution；
2) by step 1) mixed solution that obtains and ammonium acetate hybrid reaction, obtain precursor powder,
Wherein, described ammonium acetate is (0.8～1.5) with the mol ratio of described tungsten powder: 1；
3) by precursor powder heat treatment under oxygen atmosphere, bar-shaped Tungstic anhydride. is obtained.
Preferably, described step 2) particularly as follows:
2-1) by step 1) mixed solution that obtains and ammonium acetate mixed by ultrasonic vibration, obtains milky turbidity liquid；
2-2) by step 2-1) the milky turbidity liquid that obtains reacts under 2.5～3.5 atmospheric pressure, obtains precursor powder.
Preferably, the time of described ultrasonic mixing is 10～50min.
Preferably, described step 2-2) temperature reacted is 100～200 DEG C.
Preferably, described step 2-2) time of reacting is 4～8 hours.
Preferably, described step 3) temperature of heat treatment is 300～400 DEG C.
Preferably, described step 3) time of heat treatment is 4～6 hours.
Present invention also offers a kind of off-color material, it is characterised in that described off-color material is bar-shaped Tungstic anhydride.；
Described bar-shaped Tungstic anhydride. is 10～20nm being perpendicular to the distance value of 2 of lie farthest away on its axial cross section, described bar-shaped WO3A length of 2～10 μm.
Present invention also offers the application in preparation early warning cable protective sleeve of a kind of off-color material of the present invention.
One early warning cable protective sleeve of the present invention, wherein, the external sheath layer of described early warning cable protective sleeve is blended extrusion molding by off-color material and macromolecular material and obtains, the off-color material that the described off-color material present invention provides.
Compared with prior art; the invention provides a kind of off-color material and preparation method thereof and a kind of early warning cable protective sleeve; the preparation method of the off-color material that the present invention provides; by in the solution that tungsten mixes with hydrogen peroxide; add quantitative ammonium acetate and prepare precursor powder as additive; the most again precursor powder is carried out heat treatment; the pattern making the off-color material Tungstic anhydride. prepared is bar-shaped; and described bar-shaped Tungstic anhydride. is 10～20nm being perpendicular to the distance value of 2 of lie farthest away on its axial cross section, and bar-shaped WO3Length reach 2～10 μm；The specific surface area of the most bar-shaped Tungstic anhydride. is bigger; and it is difficult to reunite, stable performance, and then can directly be entrained in the oversheath material of early warning cable protective sleeve; and then simplify the preparation technology of early warning cable protective sleeve, and the early warning of the early warning cable protective sleeve obtained is effective.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the Tungstic anhydride. that the embodiment of the present invention 1 prepares；
Fig. 2 is the transmission electron microscope picture of the Tungstic anhydride. that the embodiment of the present invention 1 prepares.
Detailed description of the invention
The invention provides the preparation method of a kind of off-color material of the present invention, including:
1) tungsten powder is mixed with hydrogen peroxide, obtain mixed solution；
2) by step 1) mixed solution that obtains and ammonium acetate hybrid reaction, obtain precursor powder,
Wherein, described ammonium acetate is (0.8～1.5) with the mol ratio of described tungsten powder: 1；
3) by precursor powder heat treatment under oxygen atmosphere, bar-shaped Tungstic anhydride. is obtained.
According to the present invention, tungsten powder is mixed by the present invention with hydrogen peroxide, obtains mixed solution；Wherein, described tungsten powder and the amount ratio 1g:(3～8 of described hydrogen peroxide) mL, more preferably 1g:(5～6) mL；The temperature of described mixing is preferably-5～5 DEG C, more preferably 0 DEG C；The present invention purity not particularly requirement to tungsten powder, industrial tungsten powder, preferably purity are the tungsten powder of 99%；The present invention does not has particular/special requirement, commercially available hydrogen peroxide to the concentration of hydrogen peroxide, and hydrogen peroxide, weight/mass percentage composition if weight/mass percentage composition is 30% are the hydrogen peroxide etc. of 60%.
According to the present invention, the present invention is by step 1) mixed solution that obtains and ammonium acetate hybrid reaction, obtain precursor powder；Wherein, described ammonium acetate is (0.8～1.5) with the mol ratio of described tungsten powder: 1, is preferably (1～1.3): 1.Concrete, in order to enable ammonium acetate to be sufficiently mixed with mixed solution, preferred steps 2 of the present invention) particularly as follows:
2-1) by step 1) mixed solution that obtains and ammonium acetate by ultrasonic mixing, obtain milky turbidity liquid；
2-2) by step 2-1) the milky turbidity liquid that obtains reacts under 2.5～3.5 atmospheric pressure, obtains precursor powder.
Wherein, the present invention is first by step 1) mixed solution that obtains and ammonium acetate mixed by ultrasonic vibration, obtains milky turbidity liquid；Wherein, the time of described ultrasonic vibration is preferably 10～50min, more preferably 15～35min, more preferably 20～25min.
The present invention is also by step 2-1) the milky turbidity liquid that obtains reacts under 2.5～3.5 atmospheric pressure, obtains precursor powder.Wherein, the temperature of described reaction is preferably 100～200 DEG C, more preferably 150～180 DEG C；The time of described reaction is preferably 4～8 hours, and more preferably 5～6 hours, the pressure of described reaction was preferably 3～3.2 atmospheric pressure.And so that the precursor powder arrived is more preferable, the present invention, by the preferred natural cooling of reactant liquor complete for reaction, removes supernatant, is then washed with deionized 3～5 times, is then dried 6～8 hours with 40～60 DEG C, obtains precursor powder.
According to the present invention, precursor powder heat treatment under oxygen atmosphere that the present invention also will obtain, obtain bar-shaped Tungstic anhydride.；Wherein, the temperature of described heat treatment is preferably 300～400 DEG C, more preferably 350～380 DEG C；The time of described reaction is preferably 4～6 hours, more preferably 5～5.5 hours；The present invention does not has particular/special requirement to the oxygen providing oxygen atmosphere, and the industrial oxygen that those skilled in the art are commercially available present invention preferably employs the oxygen that purity is more than 99.9%.
Present invention also offers the application in preparation early warning cable protective sleeve of a kind of off-color material of the present invention; the off-color material that the present invention provides is applied to the preparation of early warning cable protective sleeve; preparation method is simple, and the early warning of the early warning cable protective sleeve obtained is effective.
Present invention also offers a kind of early warning cable cover(ing) off-color material, it is characterised in that described off-color material is bar-shaped Tungstic anhydride.；
Described bar-shaped Tungstic anhydride. is 10～20nm being perpendicular to the distance value of 2 of lie farthest away on its axial cross section, described bar-shaped WO3A length of 2～10 μm.Wherein, described bar-shaped WO3Length be preferably 2～8 μm, more preferably 4～6 μm.
Present invention also offers a kind of early warning cable protective sleeve, the external sheath layer of this early warning cable protective sleeve is blended extrusion molding by off-color material and macromolecular material and obtains, the bar-shaped Tungstic anhydride. off-color material that described off-color material provides for the present invention；The present invention does not has particular/special requirement, the macromolecular material that can be used for cable protective sleeve well known in the art to the kind of macromolecular material.
The invention provides a kind of early warning cable cover(ing) off-color material and its preparation method and application, the preparation method of the off-color material that the present invention provides, by in the solution that tungsten mixes with hydrogen peroxide, add quantitative ammonium acetate and prepare precursor powder as additive, the most again precursor powder is carried out heat treatment, the pattern making the off-color material Tungstic anhydride. prepared is bar-shaped, and described bar-shaped Tungstic anhydride. is 10～20nm being perpendicular to the distance value of 2 of lie farthest away on its axial cross section, and bar-shaped WO3Length reach 2～10 μm；The specific surface area of the most bar-shaped Tungstic anhydride. is bigger; and it does not reunites, stable performance, and then can directly be entrained in the oversheath material of early warning cable protective sleeve; and then simplify the preparation technology of early warning cable protective sleeve, and the early warning of the early warning cable protective sleeve obtained is effective.
Technical scheme below in conjunction with the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
Embodiment 1
1) at 0 DEG C, the tungsten powder 5g (2.7mmol) of purity 99% is dissolved in 30ml hydrogen peroxide (30wt%), continues stirring until tungsten powder and all dissolve, obtain light yellow transparent solution；
2) in above-mentioned solution, 2.7mmol ammonium acetate (CH is added3COONH4), sonic oscillation 25min, obtain milky turbidity liquid；
3) turbid solution is transferred in the reactor of polytetrafluoroethylliner liner, under 3 atmospheric pressure, process 6 hours at 150 DEG C, natural cooling, remove supernatant, deionized water rinsing 5 times, be dried 8 hours at 60 DEG C, obtain white precursor powder；
4) the white precursor powder obtained is placed in tube furnace, under oxygen (purity is 99.99%) atmosphere, processes 5 hours at 350 DEG C, obtain the bar-shaped WO of off-color material3。
Detecting the pattern of the bar-shaped Tungstic anhydride. obtained, result is shown in Fig. 1 and Fig. 2, and wherein, Fig. 1 is the scanning electron microscope (SEM) photograph of the Tungstic anhydride. that the embodiment of the present invention 1 prepares；Fig. 2 is the transmission electron microscope picture of the Tungstic anhydride. that the embodiment of the present invention 1 prepares；It can be seen that it is 10～20nm that the bar-shaped Tungstic anhydride. that the present invention obtains is perpendicular to the distance value of 2 of lie farthest away on its axial cross section, its length is about 2～6 microns, and its specific surface area is big, and does not reunites.
Bar-shaped Tungstic anhydride. of the present invention is obtained as off-color material, polyaniline, polyethylene as macromolecular material the composite of doping off-color material, result shows, off-color material is uniformly dispersed in the composite, and sensitiveer to temperature sense, at 70 DEG C, variable color i.e. occurs.
Embodiment 2
Tungstic anhydride. is prepared according to the preparation method of embodiment 1, only change the amount ratio of tungsten powder and ammonium acetate, other reaction condition is same as in Example 1, prepare Tungstic anhydride., result table 1, table 1 is the embodiment of the present invention 2 experimental result of the Tungstic anhydride. of preparation under different tungsten powders with ammonium acetate amount ratio.
Table 1 is the embodiment of the present invention 2 experimental result of the Tungstic anhydride. of preparation under different tungsten powders with ammonium acetate amount ratio
Embodiment 3
Tungstic anhydride. is prepared according to the preparation method of embodiment 1, only change step 3) the middle pressure reacted, other reaction condition is same as in Example 1, prepares Tungstic anhydride., result table 2, table 2 is the experimental result of the Tungstic anhydride. that the embodiment of the present invention 3 is prepared under different atmospheric pressures.
Table 2 is the experimental result of the Tungstic anhydride. that the embodiment of the present invention 3 is prepared under different atmospheric pressures
| 1 atmospheric pressure | Powder body, without obvious shape |
| 2 atmospheric pressure | Powder body coexists with bar-shaped |
| 2.6 atmospheric pressure | Bar-shaped |
| 4 atmospheric pressure | Powder body |
Embodiment 4
Tungstic anhydride. is prepared according to the preparation method of embodiment 1, only change step 4) in the temperature of heat treatment, other reaction condition is same as in Example 1, prepares Tungstic anhydride., result table 3, table 3 is the experimental result of the Tungstic anhydride. that the embodiment of the present invention 4 is prepared under different heat treatment temperatures.
Table 3 is the experimental result of the Tungstic anhydride. that the embodiment of the present invention 4 is prepared at a temperature of different heat treatment
| 380℃ | Bar-shaped | Specific surface area is big, and color changeable effect is good |
| 450℃ | Bar-shaped (reunion) | Specific surface area reduces, and color changeable effect is deteriorated |
The explanation of above example is only intended to help to understand method and the core concept thereof of the present invention.It should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention, it is also possible to the present invention is carried out some improvement and modification, these improve and modify in the protection domain also falling into the claims in the present invention.
Claims (10)
1. a preparation method for off-color material, including:
1) tungsten powder is mixed with hydrogen peroxide, obtain mixed solution；
2) by step 1) mixed solution that obtains and ammonium acetate hybrid reaction, obtain precursor powder,
Wherein, described ammonium acetate is (0.8～1.5) with the mol ratio of described tungsten powder: 1；
3) by precursor powder heat treatment under oxygen atmosphere, bar-shaped Tungstic anhydride. is obtained.
Preparation method the most according to claim 1, it is characterised in that described step 2) particularly as follows:
2-1) by step 1) mixed solution that obtains and ammonium acetate mixed by ultrasonic vibration, obtains milky turbidity liquid；
2-2) by step 2-1) the milky turbidity liquid that obtains reacts under 2.5～3.5 atmospheric pressure, obtains precursor powder.
Preparation method the most according to claim 2, it is characterised in that the time of described ultrasonic mixing is 10～50min.
Preparation method the most according to claim 2, it is characterised in that described step 2-2) temperature reacted is 100～200 DEG C.
Preparation method the most according to claim 2, it is characterised in that described step 2-2) time of reacting is 4～8 hours.
Preparation method the most according to claim 1, it is characterised in that described step 3) temperature of heat treatment is 300～400 DEG C.
Preparation method the most according to claim 1, it is characterised in that described step 3) time of heat treatment is 4～6 hours.
8. an off-color material, described off-color material is the bar-shaped Tungstic anhydride. that the preparation method described in claim 1～7 any one prepares；
Described bar-shaped Tungstic anhydride. is 10～20nm being perpendicular to the distance value of 2 of lie farthest away on its axial cross section, described bar-shaped WO3A length of 2～10 μm.
9. the application in preparation early warning cable protective sleeve of the off-color material described in the off-color material that prepared by the preparation method described in a claim 1～7 or claim 8.
10. an early warning cable protective sleeve; it is characterized in that; the external sheath layer of described early warning cable protective sleeve is blended extrusion molding by off-color material and macromolecular material and obtains, and described off-color material is the off-color material described in the off-color material prepared of the preparation method described in claim 1～7 or claim 8.
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| CN201610116011.5A CN105819514B (en) | 2016-03-01 | 2016-03-01 | A kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing) |
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| CN201610116011.5A CN105819514B (en) | 2016-03-01 | 2016-03-01 | A kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing) |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358719A (en) * | 2020-11-17 | 2021-02-12 | 安徽伊法拉电力科技有限公司 | Reversible thermosensitive high-voltage incoming early-warning insulating protective sleeve material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004196628A (en) * | 2002-12-20 | 2004-07-15 | National Institute For Materials Science | Tungsten oxide nano-structure, its composite body and their producing methods |
| CN101381599A (en) * | 2008-10-20 | 2009-03-11 | 中国地质大学（武汉） | Nano WO3 photochromic powder and preparation method thereof |
| CN103420424A (en) * | 2013-05-21 | 2013-12-04 | 新疆大学 | Preparation of rod-shaped nano tungsten trioxide and technology of catalytic synthesis of adipic acid therethrough |
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2016
- 2016-03-01 CN CN201610116011.5A patent/CN105819514B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004196628A (en) * | 2002-12-20 | 2004-07-15 | National Institute For Materials Science | Tungsten oxide nano-structure, its composite body and their producing methods |
| CN101381599A (en) * | 2008-10-20 | 2009-03-11 | 中国地质大学（武汉） | Nano WO3 photochromic powder and preparation method thereof |
| CN103420424A (en) * | 2013-05-21 | 2013-12-04 | 新疆大学 | Preparation of rod-shaped nano tungsten trioxide and technology of catalytic synthesis of adipic acid therethrough |
Non-Patent Citations (1)
| Title |
|---|
| SANGEETA ADHIKARI ET AL.: "Electrochemical Response for Spherical and Rod Shaped WO3 Nanoparticles", 《ISRN NANOTECHNOLOGY》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112358719A (en) * | 2020-11-17 | 2021-02-12 | 安徽伊法拉电力科技有限公司 | Reversible thermosensitive high-voltage incoming early-warning insulating protective sleeve material and preparation method thereof |
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Effective date of registration: 20180427 Address after: 311400 Zhejiang Hangzhou Fuyang District golden autumn Avenue Fortis Technology Patentee after: HANGZHOU FUTONG ELECTRIC WIRE & CABLE CO., LTD. Address before: 311400 Fu Tong Science and Technology Park, 1-8 golden autumn Avenue, Fuyang District, Hangzhou, Zhejiang Patentee before: Futong Group Co., Ltd. |