CN109535855A - A kind of preparation method of efficient electric hotting mask - Google Patents
A kind of preparation method of efficient electric hotting mask Download PDFInfo
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- CN109535855A CN109535855A CN201811266590.7A CN201811266590A CN109535855A CN 109535855 A CN109535855 A CN 109535855A CN 201811266590 A CN201811266590 A CN 201811266590A CN 109535855 A CN109535855 A CN 109535855A
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- fiber
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- hotting mask
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 235000015099 wheat brans Nutrition 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000007598 dipping method Methods 0.000 claims abstract description 31
- 239000000835 fiber Substances 0.000 claims abstract description 28
- 239000000945 filler Substances 0.000 claims abstract description 25
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 19
- 239000004917 carbon fiber Substances 0.000 claims abstract description 19
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000004880 explosion Methods 0.000 claims abstract description 16
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 12
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 12
- 229940068984 polyvinyl alcohol Drugs 0.000 claims abstract description 12
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims abstract description 12
- 230000010355 oscillation Effects 0.000 claims description 33
- YQUVCSBJEUQKSH-UHFFFAOYSA-N 3,4-dihydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C(O)=C1 YQUVCSBJEUQKSH-UHFFFAOYSA-N 0.000 claims description 20
- 238000005422 blasting Methods 0.000 claims description 18
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 17
- 239000012065 filter cake Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 14
- 239000000758 substrate Substances 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 10
- 235000002906 tartaric acid Nutrition 0.000 claims description 10
- 239000011975 tartaric acid Substances 0.000 claims description 10
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 7
- WBIQQQGBSDOWNP-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid Chemical compound CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O WBIQQQGBSDOWNP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 229940060296 dodecylbenzenesulfonic acid Drugs 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- BFMKFCLXZSUVPI-UHFFFAOYSA-N ethyl but-3-enoate Chemical compound CCOC(=O)CC=C BFMKFCLXZSUVPI-UHFFFAOYSA-N 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 230000010356 wave oscillation Effects 0.000 claims 1
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 239000002184 metal Substances 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 238000009833 condensation Methods 0.000 abstract description 3
- 230000005494 condensation Effects 0.000 abstract description 3
- 239000002305 electric material Substances 0.000 abstract description 3
- 238000006068 polycondensation reaction Methods 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 229910021392 nanocarbon Inorganic materials 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 29
- 238000005485 electric heating Methods 0.000 description 9
- 230000008859 change Effects 0.000 description 7
- 239000003610 charcoal Substances 0.000 description 5
- 239000011159 matrix material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 102000003425 Tyrosinase Human genes 0.000 description 3
- 108060008724 Tyrosinase Proteins 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000005038 ethylene vinyl acetate Substances 0.000 description 3
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 3
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical group OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical group O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 1
- ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 2,3-dimethylbutane Chemical group CC(C)C(C)C ZFFMLCVRJBZUDZ-UHFFFAOYSA-N 0.000 description 1
- 238000006845 Michael addition reaction Methods 0.000 description 1
- 150000004054 benzoquinones Chemical group 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 150000001879 copper Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000916 dilatatory effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 230000002311 subsequent effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/06—Polyethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/003—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor characterised by the choice of material
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
- H05B3/14—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
- H05B3/145—Carbon only, e.g. carbon black, graphite
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/10—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/18—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor the conductor being embedded in an insulating material
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B3/00—Ohmic-resistance heating
- H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
- B29L2007/002—Panels; Plates; Sheets
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of preparation methods of efficient electric hotting mask, belong to thermo electric material technical field.The present invention carries out Steam explosion treatment to wheat-bran fiber first, under conditions of keeping fiber physical mechanics property itself and complete appearance, fibrous inside generates pressure difference during pressurization and moment discharge, condensation polycondensation occurs for the furfural between fiber, it is combined to anchor adjacent fiber, the present invention by after charing fiber and poly-vinyl alcohol solution be mixed with dipping, so that polyvinyl alcohol absorption anchors in carbon fiber hole abundant, to improve the electric conversion efficiency of Electric radiant Heating Film, electric thermal power is avoided to decay；The present invention is uniformly mixed Carbon fibe with metal salt by microwave action, the stable Carbon fibe of property-metallic self-control carbonaceous filler has been made, and between metallic and the interface of carbon fiber, the structure of Nano carbon is in graphite-structure, increase the conductivity of carbonaceous filler, the electric conversion efficiency for being conducive to carbonaceous filler improves, and has broad application prospects.
Description
Technical field
The invention discloses a kind of preparation methods of efficient electric hotting mask, belong to thermo electric material technical field.
Background technique
Electric radiant Heating Film is divided into high temperature, low temperature electric heating film.High-temperature electric heating membrane is generally used for electronic apparatus, military affairs etc., nowadays scientific and technological
The Electric radiant Heating Film of production.Low temperature electric heating film is the translucent polyester film that can be generated heat after a kind of energization, by conductive special ink,
Metal current-carrying item is processed, hot pressing is made between insulation polyester film.Using Electric radiant Heating Film as heater when work, by heat to radiate
Form be sent into space, obtain human body and object first warm, resultant effect be better than traditional convection current heating system.Low temperature
Radiating electrothermal membrane system is made of power supply, temperature controller, connector, insulating layer, Electric radiant Heating Film and finish coat.Power supply is connected to electricity through conducting wire
Hotting mask converts electrical energy into thermal energy.Since Electric radiant Heating Film is pure resistor element circuit, therefore its high conversion efficiency, except sub-fraction is lost, absolutely
It is mostly converted into thermal energy.Electric radiant Heating Film cannot be directly used to terrestrial surface radiation heat supply, need additional PVC vacuum envelope, ability
For ground heating, guarantee using effect and service life.
Electric radiant Heating Film can be divided into following three types according to developing stage and application model: (1) electric heating canopy film: first generation electric heating
Film is layed in roof；(2) electric heating wall film: second generation Electric radiant Heating Film is layed in metope；(3) electric heating ground film: third generation Electric radiant Heating Film, paving
Set on ground.Relative to preceding two generations Electric radiant Heating Film, third generation Electric radiant Heating Film has construction is simple, is heated evenly, health care (the warm head of foot
Cool, meet health) etc. unique advantages.Electric radiant Heating Film is most common there are three types of specification by face shaping classification: 50cm width, 80cm
Width, 100cm width.There are two types of specifications by power point for Electric radiant Heating Film: the every 220 watts of Electric radiant Heating Films of square meter of 220 watts of 400 watts of every square meters
Belong to low temperature electric heating film, be mainly used in floor heating industry: 400 watts of aspects being mainly used in addition to floor heating, such as drying etc.,
400 watts of Electric radiant Heating Films belong to high-temperature electric heating membrane, and temperature highest can reach to be spent more 70, for printing drying, drug drying etc..
Common Electric radiant Heating Film is compound obtained with high molecular material matrix and carbonaceous filler at present, and carbonaceous filler and macromolecule
Poor compatibility causes the electric conversion efficiency of Electric radiant Heating Film low between material matrix, and electric thermal power decaying is obvious.
Therefore, inventing a kind of Electric radiant Heating Film that electric conversion efficiency is high has positive effect to thermo electric material technical field.
Summary of the invention
Present invention mainly solves the technical issues of, for current common Electric radiant Heating Film filled out with high molecular material matrix and carbonaceous
Expect it is compound be made, and poor compatibility causes the electric conversion efficiency of Electric radiant Heating Film low between carbonaceous filler and high molecular material matrix,
The apparent defect of electric thermal power decaying, provides a kind of preparation method of efficient electric hotting mask.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of preparation method of efficient electric hotting mask, it is characterised in that specific preparation step are as follows:
(1) it weighs wheat bran to be put into steam blasting tank, tartaric acid solution heat temperature raising is formed into steam and is passed through steam blasting tank
In, sealing tank mouth after constant temperature and pressure stands 45~60min, opens outlet valve until pressure reaches 2~3MPa in steam blasting tank
Door, is injected into material moment in tank in receiving tank, collects material in receiving tank, obtains steam explosion wheat-bran fiber；
(2) steam explosion wheat-bran fiber obtained above is put into retort, obtains wheat bran after the heat preservation charing of argon gas guard mode
Carbon fiber, be placed on after the poly-vinyl alcohol solution that wheat bran carbon fiber and mass fraction are 30% is mixed oscillation dipping 1 on shaking table~
2h, oscillation are separated by filtration to obtain filter residue after impregnating；
(3) it is put into reaction kettle, stirs after mixing the 3,4-Dihydroxybenzoic acid solution that above-mentioned filter residue and mass fraction are 20%
Reaction, is naturally cooling to room temperature, then catechol-oxydase is added into reaction kettle after reaction, continue to be stirred to react 10~
15h, discharge filtering after being stirred to react, isolated filter cake；
(4) copper nitrate solution that filter cake obtained above and mass fraction are 40% is mixed, is put into microwave oscillation instrument, microwave
Oscillation dipping, oscillation are separated by filtration to obtain dipping filter residue after impregnating, are put into oven drying, discharge after drying, obtain
Make carbonaceous filler by oneself；
(5) according to parts by weight, 100~120 parts of polyvinyl resins are weighed, the ethyl vinyl acetate second that 50~60 parts of solid contents are 60%
Enoate copolymer, 15~20 parts of above-mentioned self-control carbonaceous fillers, 3~5 parts of odium stearate, 0.1~0.2 part of cumyl peroxide, 1
It is put into batch mixer after~2 parts of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；
(6) above-mentioned Electric radiant Heating Film slurry being fitted into coating machine, is coated on devitrified glass substrate surface, control coating thickness is 2~
Devitrified glass substrate is put into baking oven after coating, discharged after dry to get efficient electric hotting mask by 3mm.
The mass fraction of tartaric acid solution as described in step (1) is 30%, and the temperature of tartaric acid solution heat temperature raising is
220~230 DEG C.
The temperature of heat preservation charing described in step (2) is 300~400 DEG C, and the time for keeping the temperature charing is 1~2h, wheat bran
The mass ratio for the poly-vinyl alcohol solution that carbon fiber and mass fraction are 30% is 1:5.
The mass ratio for the 3,4- dihydroxy-benzoic acid solution that filter residue described in step (3) and mass fraction are 20% is 1:
5, the temperature being stirred to react be 70~80 DEG C, the revolving speed being stirred to react be 200~300r/min, the time being stirred to react be 3~
5h, the additional amount of catechol-oxydase are the 10% of filter residue quality.
The mass ratio for the copper nitrate solution that filter cake described in step (4) and mass fraction are 40% is 1:8, microwave oscillation
The power of dipping is 200~300W, and the time of microwave oscillation dipping is 5~6h, and dry temperature is 105~110 DEG C, dry
Time is 1~2h.
The temperature of drying described in step (6) is 60~70 DEG C, and the dry time is 5~6h.
The method have the benefit that:
(1) it is carried out explosion treatment with winestone acid vapor, obtains steam explosion wheat-bran fiber by the present invention using wheat bran as raw material, is carbonized
Afterwards with poly-vinyl alcohol solution be mixed with dipping, then will dipping filter residue and 3,4-Dihydroxybenzoic acid solution carry out esterification after with youngster
Tea phenol oxidase secondary response, obtains filter cake, and self-control carbonaceous is dried to obtain after being then mixed with dipping filter cake and copper salt solution and is filled out
Material is coated with after finally mixing self-control carbonaceous filler with polymeric matrix, finally obtained efficient electric hotting mask, and the present invention is first to wheat
Bran fiber carries out Steam explosion treatment, under conditions of keeping fiber physical mechanics property itself and complete appearance, in pressurization and wink
Between during discharge fibrous inside generate pressure difference so that form the high pressure draught impacted from inside to outside inside wheat-bran fiber,
Under the action of the high pressure draught, the weak tissue such as wheat-bran fiber cell wall and pit membrane expands wheat bran by high pressure dilating expansion
Fiber interior space capacity, while wheat-bran fiber absorbs thermal energy, strand hair under high pressure-temperature organic carboxyl acid steam condition
Raw stronger activity, intermolecular connection rupture, hydrolyzes, and hydrolysis can promote furfural to generate, and the furfural meeting generated
Condensation or polycondensation (resinification) occur under subsequent effect, finally obtains the wheat-bran fiber of resinification, it is fine during resinification
Condensation polycondensation occurs for the furfural between dimension, combines so that adjacent fiber be anchored, forms complicated cross-linked structure, into
One step enriches the space structure inside wheat-bran fiber, finally carbonizes, and has obtained that the porosity is higher, and internal structure is more complicated
Wheat bran Carbon fibe, and the increase of the porosity and interior spatial structure are more complicated, be more conducive to carbonaceous filler electric conductivity and
Heat conductivity improves, and increases the electric conversion efficiency of Electric radiant Heating Film；
(2) fiber and poly-vinyl alcohol solution of the invention by after charing is mixed with dipping, so that polyvinyl alcohol absorption anchors at carbon fiber
It ties up in hole abundant, then carries out esterification with 3,4-Dihydroxybenzoic acid solution, catechol function is introduced into carbon fiber
Energy group, is then carried out secondary response with catechol-oxydase again, is aoxidized catechol group using catechol-oxydase, shape
At adjacent benzoquinones structure, Michael addition reaction can occur between adjacent benzoquinones, form covalently cross-linked point, ultimately form high score subnet
The generation of shaped polymer, this shaped polymer of throwing the net can increase the compatibility between carbonaceous filler and polymeric substrates, be conducive to
Carbonaceous filler is evenly dispersed in polymeric substrates, to improve the electric conversion efficiency of Electric radiant Heating Film, electric thermal power is avoided to decay；
(3) present invention is uniformly mixed Carbon fibe with metal salt by microwave action, and the stable Carbon fibe-metal of property has been made
Particle makes carbonaceous filler by oneself, and between metallic and the interface of carbon fiber, due to the catalytic action of metallic, generates
One layer of charcoal conductive nano network, the structure of Nano carbon increase the conductivity of carbonaceous filler, are conducive to charcoal in graphite-structure
The electric conversion efficiency of matter filler improves, and has broad application prospects.
Specific embodiment
Wheat bran is weighed to be put into steam blasting tank, the tartaric acid solution that mass fraction is 30% is heated to 220~
230 DEG C of formation steam are simultaneously passed through in steam blasting tank, and sealing tank mouth is until pressure reaches 2~3MPa, constant temperature in steam blasting tank
After constant pressure stands 45~60min, discharge valve is opened, is injected into material moment in tank in receiving tank, collected in receiving tank
Material obtains steam explosion wheat-bran fiber；Obtained steam explosion wheat-bran fiber is put into retort, heats and rises under argon gas guard mode
Temperature obtains wheat bran carbon fiber after 1~2h of heat preservation charing to 300~400 DEG C, by wheat bran carbon fiber and mass fraction be 30% it is poly-
Glycohol solution is that 1~2h of oscillation dipping on shaking table is placed on after 1:5 is mixed in mass ratio, is separated by filtration after oscillation dipping
Obtain filter residue；It is in mass ratio to be put into instead after 1:5 is mixed by the 3,4- dihydroxy-benzoic acid solution that filter residue and mass fraction are 20%
It answers in kettle, 70~80 DEG C of heat temperature raising, 3~5h is stirred to react with the revolving speed of 200~300r/min, after reaction Temperature fall
To room temperature, then the catechol-oxydase of filter residue quality 10% is added into reaction kettle, continues to be stirred to react 10~15h, be stirred to react
After discharge filtering, isolated filter cake；It is in mass ratio by the copper nitrate solution that obtained filter cake and mass fraction are 40%
1:8 mixing, is put into microwave oscillation instrument, with power microwave oscillation 5~6h of dipping of 200~300W, mistake after oscillation impregnates
Isolated dipping filter residue is filtered, dry 1~2h is put into baking oven at 105~110 DEG C, discharges, made by oneself after drying
Carbonaceous filler；According to parts by weight, 100~120 parts of polyvinyl resins are weighed, the ethyl vinyl acetate that 50~60 parts of solid contents are 60%
Vinyl ester copolymers, 15~20 parts of above-mentioned self-control carbonaceous fillers, 3~5 parts of odium stearate, 0.1~0.2 part of peroxidating diisopropyl
It is put into batch mixer after benzene, 1~2 part of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；Electric radiant Heating Film slurry is packed into
In coating machine, it is coated on devitrified glass substrate surface, control coating thickness is 2~3mm, by devitrified glass substrate after coating
It is put into baking oven, is discharged at 60~70 DEG C after dry 5~6h to get efficient electric hotting mask.
Example 1
It weighs wheat bran to be put into steam blasting tank, the tartaric acid solution that mass fraction is 30% is heated to 220 DEG C of formation and is steamed
Vapour is simultaneously passed through in steam blasting tank, and for sealing tank mouth until pressure reaches 2MPa in steam blasting tank, constant temperature and pressure stands 45min
Afterwards, discharge valve is opened, is injected into material moment in tank in receiving tank, material in receiving tank is collected, obtains steam explosion wheat bran
Fiber；Obtained steam explosion wheat-bran fiber is put into retort, 300 DEG C are heated under argon gas guard mode, keeps the temperature charcoal
Wheat bran carbon fiber is obtained after changing 1h, is in mass ratio that 1:5 is mixed by the poly-vinyl alcohol solution that wheat bran carbon fiber and mass fraction are 30%
It is placed on oscillation dipping 1h on shaking table after conjunction, is separated by filtration to obtain filter residue after oscillation dipping；It is by filter residue and mass fraction
20% 3,4-Dihydroxybenzoic acid solution is to be put into reaction kettle after 1:5 is mixed in mass ratio, 70 DEG C of heat temperature raising, with 200r/
The revolving speed of min is stirred to react 3h, is naturally cooling to room temperature after reaction, then the youngster of filter residue quality 10% is added into reaction kettle
Tea phenol oxidase continues to be stirred to react 10h, and discharge filtering after being stirred to react, isolated filter cake；By obtained filter cake and
The copper nitrate solution that mass fraction is 40% is 1:8 mixing in mass ratio, is put into microwave oscillation instrument, with the power microwave of 200W
Oscillation dipping 5h, oscillation are separated by filtration to obtain dipping filter residue after impregnating, and are put into baking oven at 105 DEG C dry 1h, dry
After discharge, obtain self-control carbonaceous filler；According to parts by weight, 100 parts of polyvinyl resins are weighed, 50 parts of solid contents are 60%
Ethylene-vinyl acetate copolymer, 15 parts of above-mentioned self-control carbonaceous fillers, 3 parts of odium stearate, 0.1 part of cumyl peroxide,
It is put into batch mixer after 1 part of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；Electric radiant Heating Film slurry is packed into coating machine
In, it is coated on devitrified glass substrate surface, control coating thickness is 2mm, devitrified glass substrate is put into baking oven after coating,
It discharges at 60 DEG C after dry 5h to get efficient electric hotting mask.
Example 2
It weighs wheat bran to be put into steam blasting tank, the tartaric acid solution that mass fraction is 30% is heated to 225 DEG C of formation and is steamed
Vapour is simultaneously passed through in steam blasting tank, and for sealing tank mouth until pressure reaches 2MPa in steam blasting tank, constant temperature and pressure stands 50min
Afterwards, discharge valve is opened, is injected into material moment in tank in receiving tank, material in receiving tank is collected, obtains steam explosion wheat bran
Fiber；Obtained steam explosion wheat-bran fiber is put into retort, 350 DEG C are heated under argon gas guard mode, keeps the temperature charcoal
Wheat bran carbon fiber is obtained after changing 1.5h, is in mass ratio 1:5 by the poly-vinyl alcohol solution that wheat bran carbon fiber and mass fraction are 30%
It is placed on oscillation dipping 1.5h on shaking table after mixing, is separated by filtration to obtain filter residue after oscillation dipping；By filter residue and quality point
Number is to be put into reaction kettle after 1:5 is mixed for 20% 3,4-Dihydroxybenzoic acid solution in mass ratio, 75 DEG C of heat temperature raising, with
The revolving speed of 250r/min is stirred to react 4h, is naturally cooling to room temperature after reaction, then filter residue quality 10% is added into reaction kettle
Catechol-oxydase, continue to be stirred to react 12h, after being stirred to react discharge filtering, isolated filter cake；The filter that will be obtained
The copper nitrate solution that cake and mass fraction are 40% is 1:8 mixing in mass ratio, is put into microwave oscillation instrument, with the power of 250W
Microwave oscillation impregnates 5.5h, is separated by filtration to obtain dipping filter residue after oscillation dipping, be put into baking oven at 107 DEG C dry
1.5h discharges after drying, obtains self-control carbonaceous filler；According to parts by weight, weigh 110 parts of polyvinyl resins, 55 parts it is solid
Content be 60% ethylene-vinyl acetate copolymer, 17 parts of above-mentioned self-control carbonaceous fillers, 4 parts of odium stearate, 0.1 part of peroxidating
It is put into batch mixer after diisopropylbenzene (DIPB), 1 part of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；By Electric radiant Heating Film slurry
It is fitted into coating machine, is coated on devitrified glass substrate surface, control coating thickness is 2mm, by devitrified glass base after coating
Material is put into baking oven, discharges at 65 DEG C after dry 5.5h to get efficient electric hotting mask.
Example 3
It weighs wheat bran to be put into steam blasting tank, the tartaric acid solution that mass fraction is 30% is heated to 230 DEG C of formation and is steamed
Vapour is simultaneously passed through in steam blasting tank, and for sealing tank mouth until pressure reaches 3MPa in steam blasting tank, constant temperature and pressure stands 60min
Afterwards, discharge valve is opened, is injected into material moment in tank in receiving tank, material in receiving tank is collected, obtains steam explosion wheat bran
Fiber；Obtained steam explosion wheat-bran fiber is put into retort, 400 DEG C are heated under argon gas guard mode, keeps the temperature charcoal
Wheat bran carbon fiber is obtained after changing 2h, is in mass ratio that 1:5 is mixed by the poly-vinyl alcohol solution that wheat bran carbon fiber and mass fraction are 30%
It is placed on oscillation dipping 2h on shaking table after conjunction, is separated by filtration to obtain filter residue after oscillation dipping；It is by filter residue and mass fraction
20% 3,4-Dihydroxybenzoic acid solution is to be put into reaction kettle after 1:5 is mixed in mass ratio, 80 DEG C of heat temperature raising, with 300r/
The revolving speed of min is stirred to react 5h, is naturally cooling to room temperature after reaction, then the youngster of filter residue quality 10% is added into reaction kettle
Tea phenol oxidase continues to be stirred to react 15h, and discharge filtering after being stirred to react, isolated filter cake；By obtained filter cake and
The copper nitrate solution that mass fraction is 40% is 1:8 mixing in mass ratio, is put into microwave oscillation instrument, with the power microwave of 300W
Oscillation dipping 6h, oscillation are separated by filtration to obtain dipping filter residue after impregnating, and are put into baking oven at 110 DEG C dry 2h, dry
After discharge, obtain self-control carbonaceous filler；According to parts by weight, 120 parts of polyvinyl resins are weighed, 60 parts of solid contents are 60%
Ethylene-vinyl acetate copolymer, 20 parts of above-mentioned self-control carbonaceous fillers, 5 parts of odium stearate, 0.2 part of cumyl peroxide,
It is put into batch mixer after 2 parts of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；Electric radiant Heating Film slurry is packed into coating machine
In, it is coated on devitrified glass substrate surface, control coating thickness is 3mm, devitrified glass substrate is put into baking oven after coating,
It discharges at 70 DEG C after dry 6h to get efficient electric hotting mask.
Comparative example
With the efficient electric hotting mask of Shenzhen company production as a comparison case in efficient electric hotting mask produced by the present invention and comparative example
Efficient electric hotting mask progressive can detect, testing result is as shown in table 1:
Test method:
Leakage current testing is detected using HIOKI leakage current tester.
Resistance change rate test: operating temperature is from room temperature to resistance change rate under the conditions of 1500 DEG C, after work 5000 hours
Resistance change rate.
Electric conversion efficiency test is detected by JG/T286-2010 standard.
1 Electric radiant Heating Film performance measurement result of table
| Test item | Example 1 | Example 2 | Example 3 | Comparative example |
| Leakage current (mA) | 0.06 | 0.05 | 0.05 | 0.35 |
| It heats up resistance change rate (%) | 1.11 | 1.11 | 1.10 | 5.32 |
| Resistance change rate (%) after work 5000h | 1.89 | 1.86 | 1.85 | 8.96 |
| Electric conversion efficiency (%) | 99.52 | 99.54 | 99.56 | 89.45 |
According to above-mentioned detection data, efficient electric hotting mask leakage current of the invention is minimum, and heat up resistance change rate, long-term work
Resistance change rate effectively declines, and electric conversion is stablized, high-efficient, can prevent the rapid decay of its electric thermal power, have
Wide application prospect.
Claims (6)
1. a kind of preparation method of efficient electric hotting mask, it is characterised in that specific preparation step are as follows:
(1) it weighs wheat bran to be put into steam blasting tank, tartaric acid solution heat temperature raising is formed into steam and is passed through steam blasting tank
In, sealing tank mouth after constant temperature and pressure stands 45~60min, opens outlet valve until pressure reaches 2~3MPa in steam blasting tank
Door, is injected into material moment in tank in receiving tank, collects material in receiving tank, obtains steam explosion wheat-bran fiber；
(2) steam explosion wheat-bran fiber obtained above is put into retort, obtains wheat bran after the heat preservation charing of argon gas guard mode
Carbon fiber, be placed on after the poly-vinyl alcohol solution that wheat bran carbon fiber and mass fraction are 30% is mixed oscillation dipping 1 on shaking table~
2h, oscillation are separated by filtration to obtain filter residue after impregnating；
(3) it is put into reaction kettle, stirs after mixing the 3,4-Dihydroxybenzoic acid solution that above-mentioned filter residue and mass fraction are 20%
Reaction, is naturally cooling to room temperature, then catechol-oxydase is added into reaction kettle after reaction, continue to be stirred to react 10~
15h, discharge filtering after being stirred to react, isolated filter cake；
(4) copper nitrate solution that filter cake obtained above and mass fraction are 40% is mixed, is put into microwave oscillation instrument, microwave
Oscillation dipping, oscillation are separated by filtration to obtain dipping filter residue after impregnating, are put into oven drying, discharge after drying, obtain
Make carbonaceous filler by oneself；
(5) according to parts by weight, 100~120 parts of polyvinyl resins are weighed, the ethyl vinyl acetate second that 50~60 parts of solid contents are 60%
Enoate copolymer, 15~20 parts of above-mentioned self-control carbonaceous fillers, 3~5 parts of odium stearate, 0.1~0.2 part of cumyl peroxide, 1
It is put into batch mixer after~2 parts of dodecyl benzene sulfonic acid mixing, is mixed to get Electric radiant Heating Film slurry；
(6) above-mentioned Electric radiant Heating Film slurry being fitted into coating machine, is coated on devitrified glass substrate surface, control coating thickness is 2~
Devitrified glass substrate is put into baking oven after coating, discharged after dry to get efficient electric hotting mask by 3mm.
2. a kind of preparation method of efficient electric hotting mask according to claim 1, it is characterised in that: as described in step (1)
The mass fraction of tartaric acid solution is 30%, and the temperature of tartaric acid solution heat temperature raising is 220~230 DEG C.
3. a kind of preparation method of efficient electric hotting mask according to claim 1, it is characterised in that: described in step (2)
The temperature of heat preservation charing is 300~400 DEG C, and the time for keeping the temperature charing is 1~2h, and wheat bran carbon fiber and mass fraction are 30%
The mass ratio of poly-vinyl alcohol solution is 1:5.
4. a kind of preparation method of efficient electric hotting mask according to claim 1, it is characterised in that: described in step (3)
The mass ratio for the 3,4-Dihydroxybenzoic acid solution that filter residue and mass fraction are 20% is 1:5, and the temperature being stirred to react is 70~80
DEG C, the revolving speed being stirred to react is 200~300r/min, and the time being stirred to react is 3~5h, and the additional amount of catechol-oxydase is
The 10% of filter residue quality.
5. a kind of preparation method of efficient electric hotting mask according to claim 1, it is characterised in that: described in step (4)
The mass ratio for the copper nitrate solution that filter cake and mass fraction are 40% is 1:8, and the power of microwave oscillation dipping is 200~300W, micro-
The time of wave oscillation dipping is 5~6h, and dry temperature is 105~110 DEG C, and the dry time is 1~2h.
6. a kind of preparation method of efficient electric hotting mask according to claim 1, it is characterised in that: described in step (6)
Dry temperature is 60~70 DEG C, and the dry time is 5~6h.
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