CN106131981B - A kind of preparation method of high-temperature electric heating plate - Google Patents

A kind of preparation method of high-temperature electric heating plate Download PDF

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Publication number
CN106131981B
CN106131981B CN201610457755.3A CN201610457755A CN106131981B CN 106131981 B CN106131981 B CN 106131981B CN 201610457755 A CN201610457755 A CN 201610457755A CN 106131981 B CN106131981 B CN 106131981B
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temperature
mass ratio
agent
ink
carbon ink
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CN106131981A (en
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李宝昌
陈家新
李玉宝
边喜龙
国丽荣
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Heilongjiang College of Construction
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Heilongjiang College of Construction
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    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/10Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12Heater 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
    • H05B3/14Heater 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
    • H05B3/145Carbon only, e.g. carbon black, graphite
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/52Electrically conductive inks
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00Ohmic-resistance heating
    • H05B3/20Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013Heaters using resistive films or coatings
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017Manufacturing methods or apparatus for heaters
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05BELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/032Heaters specially adapted for heating by radiation heating

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inks, Pencil-Leads, Or Crayons (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of preparation method of high-temperature electric heating plate, the present invention relates to the preparation methods of electric hot plate.Deposit that the temperature difference after powered up is larger, and power is inconsistent the invention solves existing electric hot plate, power attenuation, the poor problem of heat resistance.Method: one, high-temperature electric conduction carbon ink is prepared;Two, the production of high-temperature electric heating plate to get arrive high-temperature electric heating plate.The present invention is in a kind of preparation method of high-temperature electric heating plate.

Description

A kind of preparation method of high-temperature electric heating plate
Technical field
The present invention relates to the preparation methods of electric hot plate.
Background technique
Printed carbon ink heater element is divided into low temperature polyester electric heating film, middle temperature epoxy electric hot plate and high temperature mica electric hot plate.One As for electronics, electric appliance, industry heating, civil heating and military affairs etc..High-temperature electric heating plate is the mica that can be generated heat after a kind of energization Heating board.It is product under the action of electric current that electric hot plate, which heats principle, and the carbon molecules group in heater generates " Brownian movement ", carbon Violent friction and shock occur between molecule, the thermal energy of generation is externally transmitted in the form of far infrared radiation and convection current, electricity 98% or more can be up to the conversion ratio of thermal energy.The effect of carbon molecules is brought rapidly up system surfaces.By electric hot plate heating plant It is mounted on the wall, thermal energy will continuously be transmitted to each angle in room by far infrared radiation and convection current form It falls.Electric hot plate development potentiality is huge, meets low-carbon, economy, environmentally friendly development trend.Electric hot plate heating system not water consumption, do not take up an area, Intelligent temperature control, energy-saving material-saving meet the policy guidance of emission reduction low-carbon, have a extensive future.It is especially caused in heating industry extensively Concern.
But the temperature difference differs after traditional printed carbon ink heater element (Electric radiant Heating Film, electric hot plate) has the disadvantage that 1, is powered It is larger: since in printing technology, aluminum ink knife and silica gel print knife back and forth push conductive carbon ink to roll, and conductive carbon ink itself Can be because of stirring so that viscosity declines, mobility increases, therefore causes to leak through silk screen infiltration with the increase conductive carbon ink of number to be printed Amount is continuously increased, and is caused conductive carbon ink print thickness to increase resistance and is reduced, power increases.Conductive carbon ink-stick resistance from large to small, The product power that dispatches from the factory is inconsistent, and unstable product quality, electric hot plate (film) generates the larger temperature difference after being powered, and is unable to reach national mark Alignment request, the temperature difference is up to 10 DEG C between electric hot plate high temperature and low temperature;Since the electric hot plate high temperature carbon ink aging power that works long hours goes out Now decay.Power increase when the current solution of this kind of product is printing obtains the electric hot plate that power does not wait, then by hand first It breaks several carbon ink items and reaches design power.Second of method is the power number measured to be marked on product, but a batch produces Product factory power is inconsistent, influences corporate image.2, power attenuation: carbon ink bonding carrier heatproof is inadequate, and existing carbon ink bonding carries Body is epoxy resin board, 120 degree of maximum operating temperature, and wall warm up heater require it is 180~200 DEG C of heater operating temperature long Time service, such state's interior wall warm up product power and are just made very small generally at 300~500 watts, and operating temperature is at 80 degree hereinafter, one A room needs to fill 3~6 walls and warms up, and the too many metope of quantity is not enough while influencing indoor decorative effect, and the practicability is poor, and user is not Approve.Power attenuation problem can only be by replacing product or accelerating.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of high-temperature electric heating plate.It is deposited after powered up with solving existing electric hot plate The temperature difference is larger, and power is inconsistent, power attenuation, the poor problem of heat resistance.
A kind of preparation method of high-temperature electric heating plate of the present invention specifically carries out according to the following steps:
One, high-temperature electric conduction carbon ink is prepared:
1., the preparation of A agent:
Under conditions of temperature is 80 DEG C~100 DEG C, polyethylene glycol is placed in flask and heats and vacuumize dehydration 0.8h 4- toluene diisocynate is added to flask under conditions of temperature is 75 DEG C~85 DEG C in~1.2h, nitrogen charging gas shielded after dehydration Ester is stirred to react 2h~3h, is cooled to room temperature, and obtains A agent;
The mass ratio of the polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:(0.8~1.2);
2., the preparation of B agent:
Epoxy resin is placed in flask first, ethylene glycol ether acetate to epoxy resin is added and dissolves completely, so Afterwards in the case where temperature is 65 DEG C~75 DEG C, A agent is added into dissolved epoxy resin, reacts 8h~10h, obtains B agent;
The mass ratio of the epoxy resin and A agent is 1:(1.2~1.5);
3., the preparation of low-resistance carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min~40min is ground in machine, obtains low-resistance carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.005~0.02);The conductive carbon black and B agent Mass ratio be 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate be 2:(0.6~ 0.7);The mass ratio of the conductive carbon black and dispersing agent is 1:(0.005~0.015);
4., the preparation of high resistant carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min~40min is ground in machine, obtains high resistant carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.8~1.2);The conductive carbon black and B agent Mass ratio is 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate be 2:(0.5~ 0.6);The mass ratio of the conductive carbon black and dispersing agent is 1:(0.005~0.015);
5., the preparation of electrically conductive ink:
Low-resistance carbon ink is mixed with high resistant carbon ink by design power W, and stirs 30min~40min, obtains high-temperature electric conduction oil Ink;
Two, the production of high-temperature electric heating plate:
1., the spissatus motherboard of 0.2mm~1mm successively used sand paper be 100 mesh and the vibration grinding machine single side polishing of 300 mesh, Until the micarex after polishing without bright spot, is then placed in corona in corona machine, running speed 15m/ by micarex surfacing Min~25m/min obtains the micarex of static electrification;
2., high-temperature electric conduction ink stirred, obtain initial carbon ink oil;Curing agent is mixed with diluent, obtains curing agent With the mixture of diluent, finally the mixture of curing agent and diluent is added in initial carbon ink oil, obtains printable use Ink 3min~8min is stirred to printable ink first under conditions of revolving speed is 200r/min~300r/min, Then under conditions of revolving speed is 10r/min~15r/min, printable ink is stirred continuously, obtains printing stand-by carbon Ink;
The curing agent is N, N- dimethyl benzylamine;The diluent is the mixed solvent of butanone and ethyl alcohol;It is described Butanone and ethyl alcohol mass ratio be 1:(1.5~2);
The mass ratio of the curing agent and diluent is 1:(4~5);The mixture of the curing agent and diluent with The mass ratio of initial carbon ink oil is 1:(80~100);
3., the micarex of static electrification is put on the fixed position of screen process press, be 10r/ with revolving speed in printing process Under conditions of min~15r/min, it is stirred continuously to stand-by carbon ink is printed, then in the stirring condition of 10r/min~15r/min Under, stand-by carbon ink will be printed and be printed on the micarex of static electrification, first in the case where temperature is 50 DEG C~80 DEG C, heat preservation 5min~ 10min, then temperature is warming up to 100 DEG C~150 DEG C by 50 DEG C~80 DEG C, and in the case where temperature is 100 DEG C~150 DEG C, heat preservation Then 10min~15min comes out and cools down the fever mica boards half-finished product for obtaining being printed on conductive carbon ink to room temperature, described is printed on There is x carbon ink on the fever mica boards half-finished product of conductive carbon ink, the resistance that single carbon ink is measured after taking-up is r, single carbon ink Power is Wr, then Wr=2202/ r, the general power for being printed on the fever mica boards half-finished product of conductive carbon ink is WAlways, WAlways=xWr, obtain General power WAlways
As general power WAlwaysAnd 10 times of design power W deviation or more adjusts low-resistance carbon ink and high resistant carbon ink ratio until total work Rate WAlwaysAnd 10 times of design power W deviation or less;
As general power WAlwaysAnd 10 times of design power W deviation is hereinafter, first adjust thickness web plate, print knife hardness and print knife corner angle circle Degree, until WAlways=(W-15%)~(W+15%);Then adjustment print knife running speed, until WAlways=(W-5%)~(W+10%);
4., revolving speed be 15r/min~20r/min under conditions of, by conductive silver paste stir 5min~15min, stirred Conductive silver paste, conductive silver paste are printed in the fever mica boards half-finished product carbon ink both ends for being printed on conductive carbon ink by the conductive silver paste after mixing With a thickness of 0.1mm~0.5mm, width 10mm~20mm, be subsequently placed in temperature be toasted at 75 DEG C~85 DEG C 10min~ 15min obtains the micarex for being printed on conductive carbon ink and conductive silver paste;
5., the mica plate temperature for being printed on conductive carbon ink and conductive silver paste is warming up to 125 DEG C~135 by 75 DEG C~85 DEG C DEG C, and in the case where temperature is 125 DEG C~135 DEG C, 0.4h~0.6h is kept the temperature, is finally warming up to temperature by 125 DEG C~135 DEG C again 240 DEG C~250 DEG C, and in the case where temperature is 240 DEG C~250 DEG C, 0.8h~1.2h is kept the temperature, comes out and cools down to room temperature, obtains high temperature Electric hot plate.
The beneficial effects of the present invention are: (1) modified epoxy, is allowed to high temperature resistant, anti-aging, power is not easy to decay.(2) Control printing power consistency is improved by printing technology, individual plate temperature is uniform, produces power control in batches in national standard In range, reach the consistent purpose of power without the method for manually breaking partially electronically conductive carbon item after printing, to improve product matter Amount.
The present invention is in a kind of preparation method of high-temperature electric heating plate.
Specific embodiment
Technical solution of the present invention is not limited to the specific embodiment of act set forth below, further include each specific embodiment it Between any combination.
Specific embodiment 1: what a kind of preparation method of high-temperature electric heating plate specifically carried out according to the following steps:
One, high-temperature electric conduction carbon ink is prepared:
1., the preparation of A agent:
Under conditions of temperature is 80 DEG C~100 DEG C, polyethylene glycol is placed in flask and heats and vacuumize dehydration 0.8h 4- toluene diisocynate is added to flask under conditions of temperature is 75 DEG C~85 DEG C in~1.2h, nitrogen charging gas shielded after dehydration Ester is stirred to react 2h~3h, is cooled to room temperature, and obtains A agent;
The mass ratio of the polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:(0.8~1.2);
2., the preparation of B agent:
Epoxy resin is placed in flask first, ethylene glycol ether acetate to epoxy resin is added and dissolves completely, so Afterwards in the case where temperature is 65 DEG C~75 DEG C, A agent is added into dissolved epoxy resin, reacts 8h~10h, obtains B agent;
The mass ratio of the epoxy resin and A agent is 1:(1.2~1.5);
3., the preparation of low-resistance carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min~40min is ground in machine, obtains low-resistance carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.005~0.02);The conductive carbon black and B agent Mass ratio be 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate be 2:(0.6~ 0.7);The mass ratio of the conductive carbon black and dispersing agent is 1:(0.005~0.015);
4., the preparation of high resistant carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min~40min is ground in machine, obtains high resistant carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.8~1.2);The conductive carbon black and B agent Mass ratio is 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate be 2:(0.5~ 0.6);The mass ratio of the conductive carbon black and dispersing agent is 1:(0.005~0.015);
5., the preparation of electrically conductive ink:
Low-resistance carbon ink is mixed with high resistant carbon ink by design power W, and stirs 30min~40min, obtains high-temperature electric conduction oil Ink;
Two, the production of high-temperature electric heating plate:
1., the spissatus motherboard of 0.2mm~1mm successively used sand paper be 100 mesh and the vibration grinding machine single side polishing of 300 mesh, Until the micarex after polishing without bright spot, is then placed in corona in corona machine, running speed 15m/ by micarex surfacing Min~25m/min obtains the micarex of static electrification;
2., high-temperature electric conduction ink stirred, obtain initial carbon ink oil;Curing agent is mixed with diluent, obtains curing agent With the mixture of diluent, finally the mixture of curing agent and diluent is added in initial carbon ink oil, obtains printable use Ink 3min~8min is stirred to printable ink first under conditions of revolving speed is 200r/min~300r/min, Then under conditions of revolving speed is 10r/min~15r/min, printable ink is stirred continuously, obtains printing stand-by carbon Ink;
The curing agent is N, N- dimethyl benzylamine;The diluent is the mixed solvent of butanone and ethyl alcohol;It is described Butanone and ethyl alcohol mass ratio be 1:(1.5~2);
The mass ratio of the curing agent and diluent is 1:(4~5);The mixture of the curing agent and diluent with The mass ratio of initial carbon ink oil is 1:(80~100);
3., the micarex of static electrification is put on the fixed position of screen process press, be 10r/ with revolving speed in printing process Under conditions of min~15r/min, it is stirred continuously to stand-by carbon ink is printed, then in the stirring condition of 10r/min~15r/min Under, stand-by carbon ink will be printed and be printed on the micarex of static electrification, first in the case where temperature is 50 DEG C~80 DEG C, heat preservation 5min~ 10min, then temperature is warming up to 100 DEG C~150 DEG C by 50 DEG C~80 DEG C, and in the case where temperature is 100 DEG C~150 DEG C, heat preservation Then 10min~15min comes out and cools down the fever mica boards half-finished product for obtaining being printed on conductive carbon ink to room temperature, described is printed on There is x carbon ink on the fever mica boards half-finished product of conductive carbon ink, the resistance that single carbon ink is measured after taking-up is r, single carbon ink Power is Wr, then Wr=2202/ r, the general power for being printed on the fever mica boards half-finished product of conductive carbon ink is WAlways, WAlways=xWr, obtain General power WAlways
As general power WAlwaysAnd 10 times of design power W deviation or more adjusts low-resistance carbon ink and high resistant carbon ink ratio until total work Rate WAlwaysAnd 10 times of design power W deviation or less;
As general power WAlwaysAnd 10 times of design power W deviation is hereinafter, first adjust thickness web plate, print knife hardness and print knife corner angle circle Degree, until WAlways=(W-15%)~(W+15%);Then adjustment print knife running speed, until WAlways=(W-5%)~(W+10%);
4., revolving speed be 15r/min~20r/min under conditions of, by conductive silver paste stir 5min~15min, stirred Conductive silver paste, conductive silver paste are printed in the fever mica boards half-finished product carbon ink both ends for being printed on conductive carbon ink by the conductive silver paste after mixing With a thickness of 0.1mm~0.5mm, width 10mm~20mm, be subsequently placed in temperature be toasted at 75 DEG C~85 DEG C 10min~ 15min obtains the micarex for being printed on conductive carbon ink and conductive silver paste;
5., the mica plate temperature for being printed on conductive carbon ink and conductive silver paste is warming up to 125 DEG C~135 by 75 DEG C~85 DEG C DEG C, and in the case where temperature is 125 DEG C~135 DEG C, 0.4h~0.6h is kept the temperature, is finally warming up to temperature by 125 DEG C~135 DEG C again 240 DEG C~250 DEG C, and in the case where temperature is 240 DEG C~250 DEG C, 0.8h~1.2h is kept the temperature, comes out and cools down to room temperature, obtains high temperature Electric hot plate.
When present embodiment is produced in batches, 30 plates of every print replace a carbon inks, and carbon ink is spare and printed In journey always under stirring condition, so that every high-temperature electric heating plate power is all the same.
Present embodiment thickness web plate mesh number small-power is bigger, print knife hardness more supple-virtuosity rate is bigger, and print knife corner angle circularity r is got over High-power bigger, print knife running speed more small-power is bigger.
The beneficial effect of present embodiment is: (1) modified epoxy, is allowed to high temperature resistant, anti-aging, power is not easy to decline Subtract.(2) control printing power consistency is improved by printing technology, individual plate temperature is uniform, produces power control in batches in state In family's critical field, reach the consistent purpose of power without the method for manually breaking partially electronically conductive carbon item after printing, to improve Product quality.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: step 1 2. described in ring Oxygen resin is epoxy resin E-51,0.48 equivalent/100 gram of epoxide number~0.54 equivalent/100 gram.Other and specific embodiment One is identical.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: step 1 1. in The polyethylene glycol is polyethylene glycol 2000.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: step 1 1. in The mass ratio of the polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:0.8.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: step 1 2. in The mass ratio of the epoxy resin and A agent is 1:1.2.It is other identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: step 1 3. in The mass ratio of the conductive carbon black and electrically conductive graphite is 1:0.005;Step 1 3. described in conductive carbon black and B agent quality Than for 1:0.05;Step 1 3. described in conductive carbon black and ethylene glycol ether acetate mass ratio be 2:0.6;Step 1 is 3. Described in conductive carbon black and dispersing agent mass ratio be 1:0.005.It is other identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: step 1 4. in The mass ratio of the conductive carbon black and electrically conductive graphite is 1:0.8;Step 1 4. described in conductive carbon black and B agent mass ratio For 1:0.05;Step 1 4. described in conductive carbon black and ethylene glycol ether acetate mass ratio be 2:0.5;Step 1 4. in The mass ratio of the conductive carbon black and dispersing agent is 1:0.005.It is other identical as specific embodiment one to six.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: step 2 2. in The mass ratio of the curing agent and diluent is 1:4;Step 2 2. described in curing agent and diluent mixture and just The mass ratio of beginning carbon ink oil is 1:80.It is other identical as specific embodiment one to seven.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: step 2 3. in First in the case where temperature is 50 DEG C, 5min is kept the temperature, then temperature is warming up to 100 DEG C by 50 DEG C, and in the case where temperature is 100 DEG C, heat preservation 10min.It is other identical as specific embodiment one to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to eight: step 2 5. in The mica plate temperature for being printed on conductive carbon ink and conductive silver paste is warming up to 125 DEG C by 75 DEG C, and in the case where temperature is 125 DEG C, heat preservation Temperature is finally warming up to 240 DEG C by 125 DEG C again, and in the case where temperature is 240 DEG C, keeps the temperature 0.8h by 0.4h.Other and specific implementation Mode one to nine is identical.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment: the high-temperature electric heating plate of pre-designed 1000W;
What a kind of preparation method of high-temperature electric heating plate specifically carried out according to the following steps:
One, high-temperature electric conduction carbon ink is prepared:
1., the preparation of A agent:
Under conditions of temperature is 80 DEG C, polyethylene glycol is placed in flask and heats and vacuumize dehydration 0.8h, after dehydration Nitrogen charging gas shielded is added 4- toluene di-isocyanate(TDI) to flask, is stirred to react 2h, is cooled under conditions of temperature is 75 DEG C Room temperature obtains A agent;
The mass ratio of the polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:0.8;
2., the preparation of B agent:
Epoxy resin is placed in flask first, ethylene glycol ether acetate to epoxy resin is added and dissolves completely, so Afterwards in the case where temperature is 65 DEG C, A agent is added into dissolved epoxy resin, reacts 8h, obtains B agent;
The mass ratio of the epoxy resin and A agent is 1:1.2;
3., the preparation of low-resistance carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min is ground in machine, obtains low-resistance carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:0.005;The mass ratio of the conductive carbon black and B agent For 1:0.05;The mass ratio of the conductive carbon black and ethylene glycol ether acetate is 2:0.6;The conductive carbon black and dispersion The mass ratio of agent is 1:0.005;
4., the preparation of high resistant carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, is grinding 20min is ground in machine, obtains high resistant carbon ink;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:0.8;The conductive carbon black and the mass ratio of B agent are 1:0.05;The mass ratio of the conductive carbon black and ethylene glycol ether acetate is 2:0.5;The conductive carbon black and dispersing agent Mass ratio be 1:0.005;
5., the preparation of electrically conductive ink:
Low-resistance carbon ink is mixed with high resistant carbon ink by design power W=1000W, and stirs 30min, obtains high-temperature electric conduction oil Ink;
The mass ratio of the low-resistance carbon ink and high resistant carbon ink is 1:0.2;
Two, the production of high-temperature electric heating plate:
1., the spissatus motherboard of 0.2mm successively used sand paper be 100 mesh and the vibration grinding machine single side polishing of 300 mesh, until cloud The smooth no bright spot of master surface, is then placed in corona in corona machine for the micarex after polishing, and running speed 15m/min is obtained To the micarex of static electrification;
2., high-temperature electric conduction ink stirred, obtain initial carbon ink oil;Curing agent is mixed with diluent, obtains curing agent With the mixture of diluent, finally the mixture of curing agent and diluent is added in initial carbon ink oil, obtains printable use Ink 3min is stirred to printable ink first under conditions of revolving speed is 200r/min, be then 10r/ in revolving speed Under conditions of min, printable ink is stirred continuously, obtains printing stand-by carbon ink;
The curing agent is N, N- dimethyl benzylamine;The diluent is the mixed solvent of butanone and ethyl alcohol;It is described Butanone and ethyl alcohol mass ratio be 1:1.5;
The mass ratio of the curing agent and diluent is 1:4;The mixture of the curing agent and diluent and initial The mass ratio of carbon ink oil is 1:80;
3., the micarex of static electrification is put on the fixed position of screen process press, be 10r/ with revolving speed in printing process It under conditions of min, is stirred continuously to stand-by carbon ink is printed, then revolving speed is 10r/min, thickness web plate is that 80 mesh, print knife are hard Degree is 80 degree, print knife corner angle circularity is r=0.4mm and is printed under conditions of knife running speed is 10m/min, and stand-by carbon ink will be printed It is printed on the micarex of static electrification, first in the case where temperature is 50 DEG C, keeps the temperature 5min, then temperature is warming up to 100 DEG C by 50 DEG C, And in the case where temperature is 100 DEG C, 10min is kept the temperature, then comes out and cools down the fever micarex half for obtaining being printed on conductive carbon ink to room temperature Finished product has x=40 carbon ink on the fever mica boards half-finished product for being printed on conductive carbon ink, and single carbon ink is measured after taking-up Resistance is r=3872 ohm, and the power of single carbon ink is Wr, then Wr=2202/ r=48400/3872=50 watts, it is printed on conductive carbon The general power of the fever mica boards half-finished product of ink is WAlways, WAlways=xWr=40 × 50=2000 watts, obtain general power WAlways=2000 Watt;
It is computed general power WAlwaysAnd 10 times of design power W deviation is hereinafter, first adjustment thickness web plate is 100 mesh, print knife hardness For 80 degree and print knife corner angle circularity is r=0.05mm, obtains WAlways=1300 watts;Then adjustment print knife running speed is 18m/min, is obtained WAlways=1000 watts;
4., revolving speed be 15r/min under conditions of, conductive silver paste is stirred into 5min, the conductive silver paste after stir, general Be printed on conductive carbon ink fever mica boards half-finished product carbon ink both ends printing conductive silver paste, conductive silver paste with a thickness of 0.1mm, width 10mm, being subsequently placed in temperature is to toast 10min at 75 DEG C, obtains the micarex for being printed on conductive carbon ink and conductive silver paste;
5., the mica plate temperature for being printed on conductive carbon ink and conductive silver paste is warming up to 125 DEG C by 75 DEG C, and be in temperature At 125 DEG C, 0.4h is kept the temperature, temperature is finally warming up to 240 DEG C by 125 DEG C again, and in the case where temperature is 240 DEG C, keep the temperature 0.8h, out Furnace is cooled to room temperature, and obtains high-temperature electric heating plate;
Step 1 2. described in epoxy resin be epoxy resin E-51,0.48 equivalent/100 gram~0.54 of epoxide number is worked as / 100 grams of amount;
Step 1 1. described in polyethylene glycol be polyethylene glycol 2000.
When the present embodiment adjusts thickness web plate, print knife hardness, print knife corner angle circularity and print knife running speed, it is required to take out The resistance for measuring single carbon ink afterwards obtains general power;
The high-temperature electric heating plate prepared in the present embodiment is tested according to GB4706.1-2005 and JG/T286-2010, Shown in test result is as follows:
The high-temperature electric heat plate surface prepared in the present embodiment is smooth, smooth, and without apparent bubble, no marking, is broken at embrittlement The obvious shortcomings such as split, deform, being layered, polluting.
The high-temperature electric heating plate prepared in the present embodiment in normal working conditions, input power and rated power The deviation of (1000W) is no more than 10%.Actual measurement input power is 989.2W, deviation 1.08%.Surveying input power is 964.7W, deviation 3.53%.
The high-temperature electric heating plate prepared in the present embodiment is worked in normal working conditions when establishing steady-working state, The temperature that its shell radiates plate surface is no more than 80 DEG C, and 180 DEG C of built-in high-temperature electric heating plate surface temperature, convection current is radiated while being dissipated Heat.
The high-temperature electric heating plate prepared in the present embodiment is worked in normal working conditions when establishing steady-working state, The maximum temperature on its surface and the difference of minimum temperature are not more than 7 DEG C.
The high-temperature electric heating plate prepared in the present embodiment works in normal working conditions, from room temperature electrified regulation to stablizing work Time when making temperature 90% is not more than 10min.
The high-temperature electric heating plate prepared in the present embodiment is with 1.24 times of rated input power work until establishing steady operation State continues 8h, and shell radiant panel hot face temperature is no more than 90 DEG C during work, and it is existing rupture, deformation, layering etc. do not occur As.
The Leakage Current of the high-temperature electric heating plate prepared in the present embodiment in normal working conditions is not more than 0.25mA.
The high-temperature electric heating plate prepared in the present embodiment in normal working conditions, applies the exchange that frequency is 50Hz, 3000V Test voltage, lasts 1min, does not occur puncturing and flashover.
Leakage Current of the high-temperature electric heating plate prepared in the present embodiment under dampness is not more than 0.25mA.
The high-temperature electric heating plate dampness prepared in the present embodiment can bear the ac test electricity that frequency is 50Hz, 3000V Pressure, lasts 1min, does not occur puncturing and flashover.
The cold insulation resistance and hot resistance of the high-temperature electric heating plate insulation prepared in the present embodiment are not less than 50M Ω.
The conductor nominal cross section product of the high-temperature electric heating plate power supply lead wire prepared in the present embodiment meets GB4706.1-2005 The regulation of middle table 11, >=0.5mm2.Actual measurement is 0.54mm twice2
Cumulative operation time of the high-temperature electric heating plate prepared in the present embodiment under normal operating condition is not less than 30000h.

Claims (10)

1. a kind of preparation method of high-temperature electric heating plate, it is characterised in that a kind of preparation method of high-temperature electric heating plate be specifically press it is following What step carried out:
One, high-temperature electric conduction carbon ink is prepared:
1., the preparation of A agent:
Temperature be 80 DEG C~100 DEG C under conditions of, polyethylene glycol is placed in flask heat and vacuumize dehydration 0.8h~ 4- toluene di-isocyanate(TDI) is added to flask under conditions of temperature is 75 DEG C~85 DEG C in 1.2h, nitrogen charging gas shielded after dehydration, It is stirred to react 2h~3h, is cooled to room temperature, A agent is obtained;
The mass ratio of the polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:(0.8~1.2);
2., the preparation of B agent:
Epoxy resin is placed in flask first, ethylene glycol ether acetate to epoxy resin is added and dissolves completely, then exist Temperature is that A agent is added into dissolved epoxy resin at 65 DEG C~75 DEG C, reacts 8h~10h, obtains B agent;
The mass ratio of the epoxy resin and A agent is 1:(1.2~1.5);
3., the preparation of low-resistance carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, in grinder 20min~40min is ground, low-resistance carbon ink is obtained;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.005~0.02);The matter of the conductive carbon black and B agent Amount is than being 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate is 2:(0.6~0.7); The mass ratio of the conductive carbon black and dispersing agent is 1:(0.005~0.015);
4., the preparation of high resistant carbon ink:
Conductive carbon black, electrically conductive graphite are mixed with B agent, ethylene glycol ether acetate and dispersing agent is then added, in grinder 20min~40min is ground, high resistant carbon ink is obtained;
The dispersing agent is dinethylformamide;
The mass ratio of the conductive carbon black and electrically conductive graphite is 1:(0.8~1.2);The quality of the conductive carbon black and B agent Than for 1:(0.05~0.07);The mass ratio of the conductive carbon black and ethylene glycol ether acetate is 2:(0.5~0.6);Institute The mass ratio of the conductive carbon black and dispersing agent stated is 1:(0.005~0.015);
5., the preparation of electrically conductive ink:
Low-resistance carbon ink is mixed with high resistant carbon ink by design power W, and stirs 30min~40min, obtains high-temperature electric conduction ink;
Two, the production of high-temperature electric heating plate:
1., the spissatus motherboard of 0.2mm~1mm successively used sand paper be 100 mesh and the vibration grinding machine single side polishing of 300 mesh, until Then micarex after polishing is placed in corona in corona machine without bright spot by micarex surfacing, running speed be 15m/min~ 25m/min obtains the micarex of static electrification;
2., high-temperature electric conduction ink stirred, obtain initial carbon ink oil;Curing agent is mixed with diluent, obtain curing agent with it is dilute The mixture of agent is released, finally the mixture of curing agent and diluent is added in initial carbon ink oil, obtains printable oil Ink stirs 3min~8min to printable ink, then first under conditions of revolving speed is 200r/min~300r/min Under conditions of revolving speed is 10r/min~15r/min, printable ink is stirred continuously, obtains printing stand-by carbon ink;
The curing agent is N, N- dimethyl benzylamine;The diluent is the mixed solvent of butanone and ethyl alcohol;The fourth The mass ratio of ketone and ethyl alcohol is 1:(1.5~2);
The mass ratio of the curing agent and diluent is 1:(4~5);The mixture of the curing agent and diluent and initial The mass ratio of carbon ink oil is 1:(80~100);
3., the micarex of static electrification is put on the fixed position of screen process press, be 10r/min with revolving speed in printing process Under conditions of~15r/min, it is stirred continuously to stand-by carbon ink is printed, then under the stirring condition of 10r/min~15r/min, Stand-by carbon ink will be printed to be printed on the micarex of static electrification, first in the case where temperature is 50 DEG C~80 DEG C, heat preservation 5min~ 10min, then temperature is warming up to 100 DEG C~150 DEG C by 50 DEG C~80 DEG C, and in the case where temperature is 100 DEG C~150 DEG C, heat preservation Then 10min~15min comes out and cools down the fever mica boards half-finished product for obtaining being printed on conductive carbon ink to room temperature, described is printed on There is x carbon ink on the fever mica boards half-finished product of conductive carbon ink, the resistance that single carbon ink is measured after taking-up is r, single carbon ink Power is Wr, then Wr=2202/ r, the general power for being printed on the fever mica boards half-finished product of conductive carbon ink is WAlways, WAlways=xWr, obtain General power WAlways
As general power WAlwaysAnd 10 times of design power W deviation or more adjusts low-resistance carbon ink and high resistant carbon ink ratio until general power WAlways And 10 times of design power W deviation or less;
As general power WAlwaysAnd 10 times of design power W deviation hereinafter, first adjust thickness web plate, print knife hardness and print knife corner angle circularity, Until WAlways=(W-15%)~(W+15%);Then adjustment print knife running speed, until WAlways=(W-5%)~(W+10%);
4., revolving speed be 15r/min~20r/min under conditions of, by conductive silver paste stir 5min~15min, after obtaining stirring Conductive silver paste, will be printed on conductive carbon ink fever mica boards half-finished product carbon ink both ends printing conductive silver paste, the thickness of conductive silver paste Degree is 0.1mm~0.5mm, width 10mm~20mm, and being subsequently placed in temperature is that 10min~15min is toasted at 75 DEG C~85 DEG C, is obtained To the micarex for being printed on conductive carbon ink and conductive silver paste;
5., the mica plate temperature for being printed on conductive carbon ink and conductive silver paste is warming up to 125 DEG C~135 DEG C by 75 DEG C~85 DEG C, and Temperature be 125 DEG C~135 DEG C at, keep the temperature 0.4h~0.6h, finally by temperature again by 125 DEG C~135 DEG C be warming up to 240 DEG C~ 250 DEG C, and in the case where temperature is 240 DEG C~250 DEG C, 0.8h~1.2h is kept the temperature, comes out and cools down to room temperature, obtains high-temperature electric heating plate.
2. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 2. described in Epoxy resin is epoxy resin E-51,0.48 equivalent/100 gram of epoxide number~0.54 equivalent/100 gram.
3. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 1. described in Polyethylene glycol is polyethylene glycol 2000.
4. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 1. described in The mass ratio of polyethylene glycol and 4- toluene di-isocyanate(TDI) is 1:0.8.
5. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 2. described in Epoxy resin and the mass ratio of A agent are 1:1.2.
6. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 3. described in The mass ratio of conductive carbon black and electrically conductive graphite is 1:0.005;Step 1 3. described in conductive carbon black and B agent mass ratio be 1: 0.05;Step 1 3. described in conductive carbon black and ethylene glycol ether acetate mass ratio be 2:0.6;Step 1 3. described in Conductive carbon black and dispersing agent mass ratio be 1:0.005.
7. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 1 4. described in The mass ratio of conductive carbon black and electrically conductive graphite is 1:0.8;Step 1 4. described in conductive carbon black and B agent mass ratio be 1: 0.05;Step 1 4. described in conductive carbon black and ethylene glycol ether acetate mass ratio be 2:0.5;Step 1 4. described in Conductive carbon black and dispersing agent mass ratio be 1:0.005.
8. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 2 2. described in The mass ratio of curing agent and diluent is 1:4;Step 2 2. described in curing agent and diluent mixture and initial carbon ink The mass ratio of oil is 1:80.
9. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 2 3. in exist first Temperature is to keep the temperature 5min, then temperature is warming up to 100 DEG C by 50 DEG C, and in the case where temperature is 100 DEG C, keep the temperature 10min at 50 DEG C.
10. a kind of preparation method of high-temperature electric heating plate according to claim 1, it is characterised in that step 2 5. in will be printed on The mica plate temperature of conductive carbon ink and conductive silver paste is warming up to 125 DEG C by 75 DEG C, and in the case where temperature is 125 DEG C, keeps the temperature 0.4h, most Temperature is warming up to 240 DEG C by 125 DEG C again afterwards, and in the case where temperature is 240 DEG C, keeps the temperature 0.8h.
CN201610457755.3A 2016-06-22 2016-06-22 A kind of preparation method of high-temperature electric heating plate Expired - Fee Related CN106131981B (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201690627U (en) * 2010-04-16 2010-12-29 佛山市达利亚热能科技有限公司 Electric heating plate
CN101969703A (en) * 2010-10-28 2011-02-09 上海尚诺碳晶科技有限公司 Medium-high temperature carbon crystal electric heating material, medium-high temperature carbon crystal electric heating plate and relevant preparation method
CN103269528A (en) * 2011-08-12 2013-08-28 李春学 Macromolecule composite electric heating material, preparation method thereof and application thereof
CN103468159A (en) * 2013-03-11 2013-12-25 苏州牛剑新材料有限公司 Silver coated nickel powder conductive adhesive and preparation method thereof
CN104080209A (en) * 2014-07-17 2014-10-01 哈尔滨工业大学 Method for manufacturing electric hot plate
CN102858036B (en) * 2012-08-27 2014-11-05 苏州喜仁新材料科技有限公司 High-resistance low-temperature heating carbon paste and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN201690627U (en) * 2010-04-16 2010-12-29 佛山市达利亚热能科技有限公司 Electric heating plate
CN101969703A (en) * 2010-10-28 2011-02-09 上海尚诺碳晶科技有限公司 Medium-high temperature carbon crystal electric heating material, medium-high temperature carbon crystal electric heating plate and relevant preparation method
CN103269528A (en) * 2011-08-12 2013-08-28 李春学 Macromolecule composite electric heating material, preparation method thereof and application thereof
CN103281811A (en) * 2011-08-12 2013-09-04 李春学 Polymer composite electric heating material, preparation method thereof and application of polymer composite electric heating material
CN102858036B (en) * 2012-08-27 2014-11-05 苏州喜仁新材料科技有限公司 High-resistance low-temperature heating carbon paste and preparation method thereof
CN103468159A (en) * 2013-03-11 2013-12-25 苏州牛剑新材料有限公司 Silver coated nickel powder conductive adhesive and preparation method thereof
CN104080209A (en) * 2014-07-17 2014-10-01 哈尔滨工业大学 Method for manufacturing electric hot plate

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