CN105819514B - A kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing) - Google Patents
A kind of off-color material and preparation method thereof and a kind of early warning cable cover(ing) Download PDFInfo
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- CN105819514B CN105819514B CN201610116011.5A CN201610116011A CN105819514B CN 105819514 B CN105819514 B CN 105819514B CN 201610116011 A CN201610116011 A CN 201610116011A CN 105819514 B CN105819514 B CN 105819514B
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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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Abstract
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 for the off-color material that the present invention is provided; by in the solution that tungsten is mixed with hydrogen peroxide; add quantitative ammonium acetate and prepare precursor powder as additive; then precursor powder is heat-treated again; so that the pattern of the off-color material tungstic acid prepared is bar-shaped; and the bar-shaped tungstic acid is 10~20nm in 2 points of distance value of the lie farthest away on its axial section, and bar-shaped WO3Length reach 2~10 μm；The specific surface area of i.e. bar-shaped tungstic acid is larger; and it is difficult to reunite, performance is stable, and then can directly be entrained in the oversheath material of early warning cable protective sleeve; and then the preparation technology of early warning cable protective sleeve is simplified, and the early warning effect of obtained early warning cable protective sleeve is good.
Description
Technical field
The present invention relates to off-color material field, more particularly to a kind of off-color material and preparation method thereof and a kind of early warning electricity
Cable sheath.
Background technology
With expanding economy, electricity has become the energy essential in daily life, and Electrical Safety is also by people
Attention, arisen at the historic moment in particular for the various early warning cables of electrical transmission, such as：Patent CN201220569716.X is disclosed
A kind of early warning cable, including conductor, the coating conductor screen layer, insulating barrier, insulation screen, interior inside-out successively outside conductor
Sheath, oversheath, and in the luminous sheath of oversheath outsourcing heat discoloration；Its operation principle is：When cable occur electric leakage, short circuit or
During long-term g-load operation, cable local temperature rise, cable surface sheath is raised in noctilucence with temperature, occurs face daytime
The phenomenon of color change, to remind people that cable breaks down, allows one to away from trouble location and report cable maintenance in time
Member solves failure in time.But, the early warning cable needs individually to set up photochromic layer, and preparation technology is complicated, therefore, seeks one kind
Preparation technology is simple and the good early warning cable joint-box of early warning effect is the current technical issues that need to address.
The content of the invention
In view of this, the technical problems to be solved by the invention be the provision of a kind of off-color material and preparation method thereof with
And a kind of early warning cable cover(ing), preparation of the off-color material that the present invention is provided applied to early warning cable, not only preparation method is simple,
And the early warning effect of the early warning cable prepared is good.
The invention provides a kind of preparation method of off-color material of the present invention, including：
1) tungsten powder is mixed with hydrogen peroxide, obtains mixed solution；
2) by step 1) obtained mixed solution and ammonium acetate hybrid reaction, precursor powder is obtained,
Wherein, the mol ratio of the ammonium acetate and the tungsten powder is (0.8~1.5):1；
3) precursor powder is heat-treated under oxygen atmosphere, obtains bar-shaped tungstic acid.
It is preferred that, the step 2) be specially：
2-1) by step 1) obtained mixed solution and ammonium acetate mixed by ultrasonic vibration, obtains milky turbidity liquid；
2-2) by step 2-1) obtained milky turbidity liquid reacts under 2.5~3.5 atmospheric pressure, obtains precursor
End.
It is preferred that, the time of the ultrasonic mixing is 10~50min.
It is preferred that, the step 2-2) reaction temperature be 100~200 DEG C.
It is preferred that, the step 2-2) reaction time be 4~8 hours.
It is preferred that, the step 3) heat treatment temperature be 300~400 DEG C.
It is preferred that, the step 3) heat treatment time be 4~6 hours.
Present invention also offers a kind of off-color material, it is characterised in that the off-color material is bar-shaped tungstic acid；
The bar-shaped tungstic acid the lie farthest away on its axial section 2 points of distance value for 10~
20nm, the bar-shaped WO3Length be 2~10 μm.
Present invention also offers a kind of application of off-color material of the present invention in early warning cable protective sleeve is prepared.
A kind of early warning cable protective sleeve of the present invention, wherein, the external sheath layer of the early warning cable protective sleeve is by off-color material
Obtained with high polymer material blending extrusion molding, the off-color material that the off-color material present invention is provided.
Compared with prior art, the invention provides a kind of off-color material and preparation method thereof and a kind of early warning cable protection
Set, the preparation method for the off-color material that the present invention is provided, by the solution that tungsten is mixed with hydrogen peroxide, adding quantitative acetic acid
Ammonium prepares precursor powder as additive, and then precursor powder is heat-treated again so that the discoloration prepared
The pattern of material tungstic acid is bar-shaped, and the bar-shaped tungstic acid is two of the lie farthest away on its axial section
The distance value of point is 10~20nm, and bar-shaped WO3Length reach 2~10 μm；The specific surface area of i.e. bar-shaped tungstic acid is larger,
And it is difficult to reunite, performance is stable, and then can directly be entrained in the oversheath material of early warning cable protective sleeve, and then simplifies
The preparation technology of early warning cable protective sleeve, and the early warning effect of obtained early warning cable protective sleeve is good.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph for the tungstic acid that the embodiment of the present invention 1 is prepared；
Fig. 2 is the transmission electron microscope picture for the tungstic acid that the embodiment of the present invention 1 is prepared.
Embodiment
The invention provides a kind of preparation method of off-color material of the present invention, including：
1) tungsten powder is mixed with hydrogen peroxide, obtains mixed solution；
2) by step 1) obtained mixed solution and ammonium acetate hybrid reaction, precursor powder is obtained,
Wherein, the mol ratio of the ammonium acetate and the tungsten powder is (0.8~1.5):1；
3) precursor powder is heat-treated under oxygen atmosphere, obtains bar-shaped tungstic acid.
According to the present invention, the present invention mixes tungsten powder with hydrogen peroxide, obtains mixed solution；Wherein, the tungsten powder with it is described
The amount ratio 1g of hydrogen peroxide：(3~8) mL, more preferably 1g：(5~6) mL；The temperature of the mixing is preferably -5~5 DEG C, more
Preferably 0 DEG C；The present invention does not require that the purity of tungsten powder industrial tungsten powder, preferably purity are 99% particularly
Tungsten powder；The present invention does not have particular/special requirement, pair that commercially available hydrogen peroxide, such as weight/mass percentage composition are 30% to the concentration of hydrogen peroxide
Oxygen water, weight/mass percentage composition are 60% hydrogen peroxide etc..
According to the present invention, the present invention is by step 1) obtained mixed solution and ammonium acetate hybrid reaction, obtain precursor
End；Wherein, the mol ratio of the ammonium acetate and the tungsten powder is (0.8~1.5):1, be preferably (1~1.3):1.Specifically, being
Ammonium acetate is set to be sufficiently mixed with mixed solution, preferred steps 2 of the present invention) be specially：
2-1) by step 1) obtained mixed solution and ammonium acetate, by ultrasonic mixing, obtain milky turbidity liquid；
2-2) by step 2-1) obtained milky turbidity liquid reacts under 2.5~3.5 atmospheric pressure, obtains precursor
End.
Wherein, the present invention is first by step 1) obtained mixed solution and ammonium acetate mixed by ultrasonic vibration, obtains breast
White opacity liquid；Wherein, the time of the ultrasonic vibration is preferably 10~50min, more preferably 15~35min, more preferably
20~25min.
The present invention is also by step 2-1) obtained milky turbidity liquid reacts under 2.5~3.5 atmospheric pressure, obtains forerunner
Body powder.Wherein, the temperature of the reaction is preferably 100~200 DEG C, more preferably 150~180 DEG C；The time of the reaction
Preferably 4~8 hours, more preferably 5~6 hours, the pressure of the reaction was preferably 3~3.2 atmospheric pressure.And in order that
More preferably, the present invention will react the preferred natural cooling of reaction solution finished, remove supernatant for the precursor powder that arrives, then spend from
Sub- water washing 3~5 times, is then dried 6~8 hours with 40~60 DEG C, obtains precursor powder.
According to the present invention, obtained precursor powder is also heat-treated by the present invention under oxygen atmosphere, obtains bar-shaped three oxygen
Change tungsten；Wherein, the temperature of the heat treatment is preferably 300~400 DEG C, more preferably 350~380 DEG C；The time of the reaction
Preferably 4~6 hours, more preferably 5~5.5 hours；The present invention does not have particular/special requirement, ability to the oxygen for providing oxygen atmosphere
The industrial oxygen that field technique personnel are commercially available, present invention preferably employs the oxygen that purity is more than 99.9%.
Present invention also offers a kind of application of off-color material of the present invention in early warning cable protective sleeve is prepared, sheet
The off-color material that invention is provided is applied to the preparation of early warning cable protective sleeve, and preparation method is simple, and obtained early warning cable is protected
The early warning effect of sheath is good.
Present invention also offers a kind of early warning cable cover(ing) off-color material, it is characterised in that the off-color material is rod
Shape tungstic acid；
The bar-shaped tungstic acid the lie farthest away on its axial section 2 points of distance value for 10~
20nm, the bar-shaped WO3Length be 2~10 μm.Wherein, the bar-shaped WO3Length be preferably 2~8 μm, more preferably 4~
6μm。
Present invention also offers a kind of early warning cable protective sleeve, the external sheath layer of the early warning cable protective sleeve is by off-color material
Obtained with high polymer material blending extrusion molding, the bar-shaped tungstic acid off-color material that the off-color material provides for the present invention；This hair
The bright species to high polymer material does not have particular/special requirement, and the high polymer material well known in the art available for cable protective sleeve is equal
Can.
The invention provides a kind of early warning cable cover(ing) off-color material and its preparation method and application, what the present invention was provided
The preparation method of off-color material, is come by the solution that tungsten is mixed with hydrogen peroxide, adding quantitative ammonium acetate as additive
Precursor powder is prepared, then precursor powder is heat-treated again so that the off-color material tungstic acid prepared
Pattern is bar-shaped, and the bar-shaped tungstic acid is 10 in 2 points of distance value of the lie farthest away on its axial section
~20nm, and bar-shaped WO3Length reach 2~10 μm；The specific surface area of i.e. bar-shaped tungstic acid is larger, and it is not reunited, property
Can be stable, and then can directly be entrained in the oversheath material of early warning cable protective sleeve, and then simplify early warning cable protective sleeve
Preparation technology, and the early warning effect of obtained early warning cable protective sleeve is good.
Technical scheme below in conjunction with the embodiment of the present invention is clearly and completely described, 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 1
1) at 0 DEG C, the tungsten powder 5g (2.7mmol) of purity 99% is dissolved in 30ml hydrogen peroxide (30wt%), continued
Stirring is all dissolved to tungsten powder, obtains light yellow transparent solution；
2) 2.7mmol ammonium acetates (CH is added into above-mentioned solution3COONH4), sonic oscillation 25min obtains milky muddy
Turbid liquid；
3) turbid solution is transferred in the reactor of polytetrafluoroethylliner liner, 6 is handled under 3 atmospheric pressure, at 150 DEG C small
When, natural cooling is gone at supernatant, deionized water rinsing 5 times, 60 DEG C to dry 8 hours, obtains white precursor powder；
4) obtained white precursor powder is placed in tube furnace, under oxygen (purity is 99.99%) atmosphere, 350
Handled 5 hours at DEG C, obtain the bar-shaped WO of off-color material3。
The pattern of bar-shaped tungstic acid to obtaining is detected, as a result sees Fig. 1 and Fig. 2, wherein, Fig. 1 is real for the present invention
Apply the scanning electron microscope (SEM) photograph for the tungstic acid that example 1 is prepared；Fig. 2 is the saturating of the tungstic acid that the embodiment of the present invention 1 is prepared
Penetrate electron microscope；It can be seen that obtained bar-shaped tungstic acid lie farthest away on its axial section of the invention
2 points of distance value be 10~20nm, its length is about 2~6 microns, and its specific surface area is big, and does not reunite.
Bar-shaped tungstic acid of the present invention is obtained as off-color material, polyaniline, polyethylene as high polymer material
To the composite of doping off-color material, as a result show, off-color material is uniformly dispersed in the composite, and to temperature sense ratio
It is sensitiveer, change colour at 70 DEG C.
Embodiment 2
Preparation method according to embodiment 1 prepares tungstic acid, only changes the amount ratio of tungsten powder and ammonium acetate, other reactions
Condition is same as Example 1, prepares tungstic acid, as a result table 1, and table 1 is the embodiment of the present invention 2 in different tungsten powder and vinegar
The experimental result of the tungstic acid prepared under sour ammonium amount ratio.
Table 1 is the experiment knot for the tungstic acid that the embodiment of the present invention 2 is prepared under different tungsten powders and ammonium acetate amount ratio
Really
Embodiment 3
Preparation method according to embodiment 1 prepares tungstic acid, only changes step 3) the middle pressure reacted, other reaction bars
Part is same as Example 1, prepares tungstic acid, as a result table 2, and table 2 is the embodiment of the present invention 3 under different atmospheric pressures
The experimental result of the tungstic acid of preparation.
Table 2 is the experimental result for the tungstic acid that the embodiment of the present invention 3 is prepared under different atmospheric pressures
| 1 atmospheric pressure | Powder, without obvious shape |
| 2 atmospheric pressure | Powder coexists with bar-shaped |
| 2.6 atmospheric pressure | It is bar-shaped |
| 4 atmospheric pressure | Powder |
Embodiment 4
Preparation method according to embodiment 1 prepares tungstic acid, only changes step 4) the middle temperature being heat-treated, other reactions
Condition is same as Example 1, prepares tungstic acid, as a result table 3, and table 3 is the embodiment of the present invention 4 in different heat treatment temperature
The experimental result of the lower tungstic acid prepared of degree.
Table 3 is the experimental result for the tungstic acid that the embodiment of the present invention 4 is prepared at a temperature of different heat treatment
| 380℃ | It is 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 the method and its core concept for helping to understand the present invention.It should be pointed out that pair
, under the premise without departing from the principles of the invention, can also be to present invention progress for those skilled in the art
Some improvement and modification, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
Claims (8)
1. a kind of preparation method of off-color material, including：
1) tungsten powder is mixed with hydrogen peroxide, obtains mixed solution；
2-1) by step 1) obtained mixed solution and ammonium acetate mixed by ultrasonic vibration, obtains milky turbidity liquid；
Wherein, the mol ratio of the ammonium acetate and the tungsten powder is (0.8~1.5):1；
2-2) by step 2-1) obtained milky turbidity liquid reacts under 2.5~3.5 atmospheric pressure, obtains precursor powder；
3) precursor powder is heat-treated under oxygen atmosphere, obtains bar-shaped tungstic acid；
The step 3) heat treatment temperature be 300~400 DEG C.
2. preparation method according to claim 1, it is characterised in that the time of the ultrasonic mixing is 10~50min.
3. preparation method according to claim 1, it is characterised in that the step 2-2) temperature of reaction is 100~200
℃。
4. preparation method according to claim 1, it is characterised in that the step 2-2) time of reaction is small for 4~8
When.
5. preparation method according to claim 1, it is characterised in that the step 3) time of heat treatment is small for 4~6
When.
6. a kind of off-color material, the off-color material is that the preparation method described in Claims 1 to 5 any one is prepared
Bar-shaped tungstic acid；
The bar-shaped tungstic acid is 10~20nm, institute in 2 points of distance value of the lie farthest away on its axial section
State bar-shaped WO3Length be 2~10 μm.
7. the change described in off-color material or claim 6 prepared by the preparation method described in a kind of Claims 1 to 5 any one
Application of the color material in early warning cable protective sleeve is prepared.
8. a kind of early warning cable protective sleeve, it is characterised in that the external sheath layer of the early warning cable protective sleeve by off-color material and
High polymer material blending extrusion molding is obtained, and the off-color material is prepared by the preparation method described in Claims 1 to 5 any one
Off-color material described in off-color material or claim 6.
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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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| 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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| CN101381599B (en) * | 2008-10-20 | 2011-06-15 | 中国地质大学（武汉） | Nano WO3 photochromic powder 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. |
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