CN108468252A - A kind of surface modifying method improving cellulose insulation paper electric durability energy - Google Patents
A kind of surface modifying method improving cellulose insulation paper electric durability energy Download PDFInfo
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- CN108468252A CN108468252A CN201810126872.0A CN201810126872A CN108468252A CN 108468252 A CN108468252 A CN 108468252A CN 201810126872 A CN201810126872 A CN 201810126872A CN 108468252 A CN108468252 A CN 108468252A
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- reaction kettle
- insulation paper
- cellulose insulation
- fluorine
- cellulose
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/002—Tissue paper; Absorbent paper
- D21H27/004—Tissue paper; Absorbent paper characterised by specific parameters
- D21H27/005—Tissue paper; Absorbent paper characterised by specific parameters relating to physical or mechanical properties, e.g. tensile strength, stretch, softness
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Organic Insulating Materials (AREA)
Abstract
The present invention discloses a kind of surface modifying method of raising cellulose insulation paper electric durability energy, and key step includes:Samples dried vacuumizes, and cleans reaction kettle, and injection fluorine, nitrogen mixture gas, reaction kettle is cleaned in molecular structure modification, after ensureing that fluorine gas is fully drained, opens reaction kettle, finally takes out sample.The present invention is handled by molecular structure, and oil immersion cellulose insulation paper direct current electric durability can obtain to be promoted to a certain extent.
Description
Technical field
The invention belongs to the resistance to electrical domains of insulating paper more particularly to a kind of surface for improving cellulose insulation paper electric durability energy to change
Property method.
Background technology
With converter valve collectively as the connection hinge of AC and DC system, value side bushing should be born converter power transformer
AC field, bears that direct current, alternating current-direct current be compound and polarity reversion electric field action again, and insulation breakdown easily occurs.Make in electric field
Under, the accumulation on surface, interface and space charge will lead to oilpaper combined insulation electric field distortion, cause Oil-Paper Insulation aging
And the problems such as failure of insulation.Therefore the regulation and control of paper oil insulation charge are problem in science urgently to be resolved hurrily, and have actual engineering
Meaning
Invention content
It is an object of the invention to overcome the deficiencies in the prior art, fill the blank of research field, propose that a kind of raising is fine
The surface modifying method of the plain insulating paper electric durability energy of dimension, by carrying out molecular structure processing to traditional fibre element insulating paper,
Influence of the modification to cellulose insulation paper chemical composition and physical pattern is studied, and in this, as basis, is analyzed at modified
The mechanism of action to oil-immersed insulating paper electric-charge-dissipating and trap level characteristic is managed, modification is disclosed and spy is punctured to oil-immersed insulating paper
Property affecting laws, explore cellulose insulation paper charge regulate and control method, to improve the insulation characterisitic of cellulose insulation paper.
The technical solution adopted by the present invention to solve the technical problems is:It is a kind of improve cellulose insulation paper electric durability can
Surface modifying method is modified place using the strong oxidizing property of fluorine gas using cellulose insulation paper as matrix to cellulose insulation paper
Reason, is replaced as F atom so that c h bond is higher by highly polar and bond energy by the H atom in the cellulose chain of cellulose insulation paper
C-F keys are replaced, and are specifically comprised the following steps:
1) samples dried:Cellulose paper is cut first to 45 × 45mm sizes;Then it is placed in vacuum drying chamber,
At 90 DEG C, vacuum degree is to carry out vacuum drying treatment for 24 hours under 50pa states, the cellulose insulation paper sample fully dried;
It after fully dry cellulose insulation paper sample is cooled to room temperature again, is positioned in reaction kettle, seals reaction kettle;
2) it vacuumizes:Air in the quick extraction kettle of vane vacuum pump is opened, until gauge hand reaches on reaction kettle
After to -0.1MPa, vacuum pump is closed;
3) reaction kettle is cleaned:
(1) nitrogen cylinder pressure reducing valve is opened, high pure nitrogen is injected into reaction kettle and reaches ambient pressure;
(2) it is again turned on vacuum pump and is evacuated to vacuum;
(3) it repeats the above steps (1) and (2) five times or more, ensures that reaction kettle and gas in pipelines thoroughly empty;
4) fluorine, nitrogen mixture gas are injected:Reactor temperature is set as 20 DEG C, fluorine gas volume is slowly filled with into reaction kettle
Fluorine, nitrogen mixture gas of the score for 20%, make air pressure in reaction kettle reach preset pressure 500mbr, obtaining fluorine gas volume fraction is
20% fluorine, nitrogen mixture gas, and be allowed to and cellulose insulation paper specimen reaction;
5) molecular structure modification:After being fluorinated time 2-10min, opens vacuum pump and interior residual gas is discharged;
6) reaction kettle is cleaned:It is cleaned repeatedly using high pure nitrogen according to (1) step by step to (3) in step 3);
7) after ensureing that fluorine gas is fully drained, reaction kettle is opened;
8) sample is taken out.
To ensure that fluorine gas can fully be reacted with cellulose insulation paper in reaction process, the examination in the step 1) in reaction kettle
Sample is maintained within 10.
Cellulose insulation paper thickness is 0.13mm in the step 1).
Time preferred 5min is fluorinated in the step 5).
Advantageous effect
1, pass through molecular structure as seen from Figure 4 to handle, oil immersion cellulose insulation paper direct current electric durability can obtain
It is promoted to a certain degree, while as the reaction time increases, downward trend after first raising is presented in dc breakdown intensity.It is hit from Fig. 5
Same conclusions can also be obtained by wearing the Weibull probability distribution results of voltage.
2, the fluorination time is that the electric durability of cellulose insulation paper can be most strong for 5min.
Description of the drawings
Fig. 1 is cellulose paper molecular structure process chart;
Fig. 2 is dc breakdown experimental electrode schematic diagram;
Fig. 3 is dc breakdown measuring principle figure;
Fig. 4 is differential responses time oil-immersed insulating paper dc breakdown result;
Fig. 5 is differential responses time oil-immersed insulating paper dc breakdown Weibull probability result.
Specific implementation mode
A kind of surface modifying method improving cellulose insulation paper electric durability energy of the present invention, utilizes molecular structure device
Fluorination treatment is carried out to the cellulose insulation paper of purchase, is as follows:
(1) cellulose paper is cut to suitable dimension, be then placed in vacuum drying chamber, at 90 DEG C, vacuum degree
To carry out vacuum drying treatment for 24 hours under 50pa states, to remove contained humidity in insulating paper.
(2) it after being cooled to room temperature fully dry insulating paper sample, is positioned in reaction kettle, seals reaction kettle.It needs
Illustrate, to ensure that fluorine gas can fully be reacted with insulating paper in reaction process, the sample in reaction kettle should not be excessive.
(3) open the quick extraction kettle of vane vacuum pump in air, until reaction kettle on gauge hand reach-
After 0.1MPa, vacuum pump is closed;Nitrogen cylinder pressure reducing valve is opened, high pure nitrogen is injected into reaction kettle and reaches ambient pressure;Again
Secondary opening vacuum pump is evacuated to vacuum.It is iteratively repeated above process five times or more, ensures that reaction kettle and gas in pipelines thoroughly empty.
(4) reaction temperature required in reaction kettle is set, it is 20% that fluorine gas volume fraction is slowly filled with into reaction kettle
Fluorine, nitrogen mixture gas make air pressure in reaction kettle reach preset pressure value, obtain a certain concentration fluorine, nitrogen mixture gas, and be allowed to
Insulating paper specimen reaction.After certain reaction time, opens vacuum pump and interior residual gas is discharged.
(5) reaction kettle is cleaned repeatedly using high pure nitrogen according to step described in (3), ensure to beat after fluorine gas is fully drained
Reaction kettle is opened, sample is taken out.The cellulose of differential responses time, reaction temperature and gas pressure is obtained using above-mentioned processing method
Paper sample.
1, using cellulose insulation paper as matrix, processing is modified to cellulose insulation paper using the strong oxidizing property of fluorine gas,
H atom in the cellulose chain of cellulose insulation paper is replaced as F atom so that c h bond is by the higher C-F of highly polar and bond energy
Key is replaced.Using the cellulose insulation paper of 0.13mm, the fluorinated time is respectively 2min, 5min and 10min for experiment.At fluorination
It is as shown in Figure 1 to manage flow.
1) samples dried:Cellulose paper is cut first to 45 × 45mm;Then it is placed in vacuum drying chamber, 90
DEG C, vacuum degree is to carry out vacuum drying treatment for 24 hours under 50pa states, the cellulose insulation paper sample fully dried;Again will
It after fully dry cellulose insulation paper sample is cooled to room temperature, is positioned in reaction kettle, seals reaction kettle;
2) it vacuumizes:Air in the quick extraction kettle of vane vacuum pump is opened, until gauge hand reaches on reaction kettle
After to -0.1MPa, vacuum pump is closed;
3) reaction kettle is cleaned:
(1) nitrogen cylinder pressure reducing valve is opened, high pure nitrogen is injected into reaction kettle and reaches ambient pressure;
(2) it is again turned on vacuum pump and is evacuated to vacuum;
(3) it repeats the above steps (1) and (2) five times or more, ensures that reaction kettle and gas in pipelines thoroughly empty;
4) fluorine, nitrogen mixture gas are injected:20 DEG C of reaction kettle interior reaction temperature is set, fluorine gas is slowly filled with into reaction kettle
Fraction be 20% fluorine, nitrogen mixture gas, so that air pressure in reaction kettle is reached preset pressure 500mbr, obtain a certain concentration fluorine,
Nitrogen mixture gas, and be allowed to and cellulose insulation paper specimen reaction;
5) molecular structure modification:After being fluorinated time 2-10min, opens vacuum pump and interior residual gas is discharged;
6) reaction kettle is cleaned:It is cleaned repeatedly using high pure nitrogen according to (1) step by step to (3) in step 3);
7) after ensureing that fluorine gas is fully drained, reaction kettle is opened;
8) sample is taken out.
2, electrode used by oil-immersed insulating paper dc breakdown performance test is as shown in Figure 2.According to IEC60243 standards, electricity
Pole uses column-plate electrode model.Column electrode high 25mm, diameter 25mm, plate electrode a diameter of 75mm, high 15mm.Two electricity of column plate
Pole is brass material, and chamfered is made at edge.Measuring principle is as shown in Figure 3.Before test, by cellulose insulation paper sample
It is dried and immersion oil is handled, while experiment being fully dried with transformer oil.When measurement, by oil-immersed insulating paper and
Test electrode is placed in transformer oil, and control high-voltage DC power supply boosts by 1kV/s rates, records breakdown voltage result.It repeats
Above step, every group of sample duplicate measurements 10 times record total data.
3, it is fitted by carrying out two-parameter Weibull (Weibull) to oil-immersed insulating paper breakdown voltage, it can analyzing molecules knot
Influence result of the structure regulation and control processing to oil-impregnated paper insulation performance.Two-parameter Weibull Distribution has extensive in lifetime data analysis
Application.Two-parameter Weibull distribution can be used succinct cumulative distribution function to indicate:
Wherein, two-parameter to respectively refer to scale parameter η and form parameter β.Form parameter be transient failure probability at any time
Change rate, form parameter is bigger, and breakdown voltage dispersibility is smaller, i.e., this group of breakdown voltage data more tend to concentrate at small electric
In pressure section.Scale parameter is commonly known as character voltage, indicates that sample exists when experiment is carried out to character voltage η
Punch-through occurs for 63.2% probability.F is accumulative breakdown probability, and t is that experiment measures breakdown voltage value.
Claims (4)
1. a kind of surface modifying method improving cellulose insulation paper electric durability energy, which is characterized in that be with cellulose insulation paper
Matrix is modified processing using the strong oxidizing property of fluorine gas to cellulose insulation paper, will be in the cellulose chain of cellulose insulation paper
H atom be replaced as F atom so that c h bond is replaced by the higher C-F keys of highly polar and bond energy, specifically comprises the following steps:
1) samples dried:Cellulose paper is cut first to 45 × 45mm sizes;Then it is placed in vacuum drying chamber, 90
DEG C, vacuum degree is to carry out vacuum drying treatment for 24 hours under 50pa states, the cellulose insulation paper sample fully dried;Again will
It after fully dry cellulose insulation paper sample is cooled to room temperature, is positioned in reaction kettle, seals reaction kettle;
2) it vacuumizes:Open the quick extraction kettle of vane vacuum pump in air, until reaction kettle on gauge hand reach-
After 0.1MPa, vacuum pump is closed;
3) reaction kettle is cleaned:
(1) nitrogen cylinder pressure reducing valve is opened, high pure nitrogen is injected into reaction kettle and reaches ambient pressure;
(2) it is again turned on vacuum pump and is evacuated to vacuum;
(3) it repeats the above steps (1) and (2) five times or more, ensures that reaction kettle and gas in pipelines thoroughly empty;
4) fluorine, nitrogen mixture gas are injected:Reactor temperature is set as 20 DEG C, fluorine gas volume fraction is slowly filled with into reaction kettle
Fluorine, nitrogen mixture gas for 20% make air pressure in reaction kettle reach preset pressure 500mbr, and it is 20% to obtain fluorine gas volume fraction
Fluorine, nitrogen mixture gas, and be allowed to and cellulose insulation paper specimen reaction;
5) molecular structure modification:After being fluorinated time 2-10min, opens vacuum pump and interior residual gas is discharged;
6) reaction kettle is cleaned:It is cleaned repeatedly using high pure nitrogen according to (1) step by step to (3) in step 3);
7) after ensureing that fluorine gas is fully drained, reaction kettle is opened;
8) sample is taken out.
2. the surface modifying method according to claim 1 for improving cellulose insulation paper electric durability energy, which is characterized in that institute
The sample in step 1) in reaction kettle is stated to be maintained within 10.
3. the surface modifying method according to claim 1 for improving cellulose insulation paper electric durability energy, which is characterized in that institute
It is 0.13mm to state cellulose insulation paper thickness in step 1).
4. the surface modifying method according to claim 1 for improving cellulose insulation paper electric durability energy, which is characterized in that institute
It states and is fluorinated time preferred 5min in step 5).
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111363121A (en) * | 2020-03-26 | 2020-07-03 | 上海稳优实业有限公司 | Method for improving tracking resistance of epoxy resin material |
CN111856227A (en) * | 2020-08-04 | 2020-10-30 | 江西理工大学 | Method for improving thermal aging resistance of converter transformer oil paper insulation and testing method |
CN114293394A (en) * | 2021-12-31 | 2022-04-08 | 湖南金博氢能科技有限公司 | Hydrophobic carbon paper, preparation method thereof, gas diffusion layer and fuel cell |
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US3808115A (en) * | 1969-07-23 | 1974-04-30 | Allis Chalmers Mfg Co | Surface fluorinated hydrogen containing material and process for making |
CN105316938A (en) * | 2015-11-04 | 2016-02-10 | 扬州纳佰成纳米科技有限公司 | Method for preparing CA (cellulose acetate) nanofiber composite |
CN106782941A (en) * | 2016-12-22 | 2017-05-31 | 同济大学 | A kind of method for improving the resistance to discharge performance of epoxy insulation in Electrode in Gas Insulated System |
CN106847422A (en) * | 2017-02-28 | 2017-06-13 | 天津大学 | Direct current cables annex silicon rubber insulation surface molecules structure regulating device and method |
CN107602900A (en) * | 2017-08-23 | 2018-01-19 | 天津大学 | Surface state improves high-voltage direct-current cable accessory insulator interface charge restraining method |
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2018
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Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US3808115A (en) * | 1969-07-23 | 1974-04-30 | Allis Chalmers Mfg Co | Surface fluorinated hydrogen containing material and process for making |
CN105316938A (en) * | 2015-11-04 | 2016-02-10 | 扬州纳佰成纳米科技有限公司 | Method for preparing CA (cellulose acetate) nanofiber composite |
CN106782941A (en) * | 2016-12-22 | 2017-05-31 | 同济大学 | A kind of method for improving the resistance to discharge performance of epoxy insulation in Electrode in Gas Insulated System |
CN106847422A (en) * | 2017-02-28 | 2017-06-13 | 天津大学 | Direct current cables annex silicon rubber insulation surface molecules structure regulating device and method |
CN107602900A (en) * | 2017-08-23 | 2018-01-19 | 天津大学 | Surface state improves high-voltage direct-current cable accessory insulator interface charge restraining method |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111363121A (en) * | 2020-03-26 | 2020-07-03 | 上海稳优实业有限公司 | Method for improving tracking resistance of epoxy resin material |
CN111856227A (en) * | 2020-08-04 | 2020-10-30 | 江西理工大学 | Method for improving thermal aging resistance of converter transformer oil paper insulation and testing method |
CN114293394A (en) * | 2021-12-31 | 2022-04-08 | 湖南金博氢能科技有限公司 | Hydrophobic carbon paper, preparation method thereof, gas diffusion layer and fuel cell |
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