CN108156675A - Electrothermal film sol and preparation method thereof - Google Patents
Electrothermal film sol and preparation method thereof Download PDFInfo
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- CN108156675A CN108156675A CN201711383475.3A CN201711383475A CN108156675A CN 108156675 A CN108156675 A CN 108156675A CN 201711383475 A CN201711383475 A CN 201711383475A CN 108156675 A CN108156675 A CN 108156675A
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- phosphoric acid
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- 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—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
- H05B3/12—Heater 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
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Abstract
The invention discloses a kind of electrothermal film sol and preparation method thereof, the electrothermal film sol is prepared by following raw materials：Butter of tin, potassium acetate, titanium tetrachloride, cosolvent, zinc acetate, cobalt salt additive, ethyl alcohol, coupling agent.Electrothermal film sol of the present invention and preparation method thereof, solution component is simple, it is convenient to prepare, without discharging of waste liquid, the electrothermal film sol uniformity is high, and homogeney is good, thus the structural compactness of Electric radiant Heating Film prepared by colloidal sol, it extends the service life of Electric radiant Heating Film, bear that voltage is high, power is big, there is good performance.
Description
Technical field
The present invention relates to electrothermal film technology field, specifically, being related to a kind of electrothermal film sol and preparation method thereof.
Background technology
Relative to resistance wire class heating element, the heating area of Electric radiant Heating Film class heating element is combined tightly greatly, with heated object
Close, so electric conversion efficiency is very high, energy-saving effect is notable, and shape can arbitrarily manufacture and watt level is arbitrarily adjustable, institute
To be easy to apply on some complex-shaped electric heating appliances, and it is not take up any using space.Meanwhile Electric radiant Heating Film class electricity
Thermal element is using and any air, noise or visual pollution is not generated in production process, do not generate yet any waste, waste water and
Exhaust gas is real environment-friendly products.
Chinese patent application No. is 99107995.7 discloses technical recipe and the processing side of a kind of semiconductor thermoelectric film
Method, it is using stannic oxide, boron, titanium tetrachloride, fluorine, cadmium, four nickel chlorides as raw material, using absolute ethyl alcohol as main solution, is carried out
Saturated solution is sufficiently stirred into, the Electric radiant Heating Film that 700 ° of DEG C of shallow lake stain sintering are made is carried out on the base material of resistance to violent change, it is described
Its component content of saturated solution, weight percent:Butter of tin 47-60, absolute ethyl alcohol 28-48, hydrofluoric acid 5-15, boric acid 0.1-
1, titanium tetrachloride 0.1-2, potassium chloride 1-4, four nickel chloride 2-8, antimony trichloride 2-8.
Chinese patent application No. is 201410756037.7 discloses a kind of saturation for being used to prepare semiconductor thermoelectric film
Solution.Its composition is by weight percentage：Butter of tin 40-60, titanium tetrachloride 0.5-2, four nickel chloride 2-8, potassium chloride 1-3,
Antimony trichloride 5-8, surplus absolute ethyl alcohol.Above-mentioned saturated solution is fully vaporized, in high insulation, resistance to violent change, heat safe base material
Upper progress surface capillary hole infiltration, is sintered the Electric radiant Heating Film that is made at shallow lake stain.
There is a collection of patent and element in relation to electrothermal film technology one by one since late nineteen eighties in the country, but by
In formula not perfect and manufacture craft not science all there are power is unstable, attenuation is big, operating temperature range is small etc. asks
Topic.So the product of neither one maturation appears on the market so far in application process, enter market reluctantly even if there is an other product
It is short-lived, just dies young due to quality problems in a short period of time.In electrothermal film sol film forming procedure, the form of film with
Compatible situation between dispersion situation and raw material of the raw material between solvent has very important relationship.Electric radiant Heating Film in the prior art
The problems such as dispersibility of colloidal sol in a solvent is poor, the easy rupture for generating Electric radiant Heating Film and unbalanced stress, therefore obtained electric heating
Element performance is unstable, and working efficiency is relatively low.
Invention content
The object of the present invention is to provide a kind of temperature in use is high, service life is long, low manufacture cost electrothermal film sol and
Preparation method.
In order to achieve the above object, the technical scheme is that：
A kind of electrothermal film sol is prepared by following raw materials：Butter of tin, potassium acetate, titanium tetrachloride, cosolvent, vinegar
Sour zinc, cobalt salt additive, ethyl alcohol, coupling agent.
In the present invention, a kind of electrothermal film sol is prepared by the raw material of following weight parts：40-60 parts of butter of tin,
2-5 parts of potassium acetate, 1-3 parts of titanium tetrachloride, 1-5 parts of cosolvent, 2-5 parts of zinc acetate, 1-3 parts of cobalt salt additive, ethyl alcohol 20-30
Part, 2-5 parts of coupling agent.
The cosolvent is acetic acid or hydrochloric acid.
The coupling agent is isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters.
In the present invention preferably, the coupling agent is modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters.
The preparation method of modified isopropyl three (the dioctyl phosphoric acid acyloxy) titanate esters is：By isopropyl three, (two is pungent
Base phosphoric acid acyloxy) titanate esters and ceria be (3-7) in molar ratio：1 mixing is stirred anti-at being 115-125 DEG C in temperature
It answers 2-4 hours, obtains reactant；By reactants dry 5-10 hours to obtain the final product.
The rotating speed of the stirring is 100-300r/min.
The temperature of the drying is 70-90 DEG C, vacuum degree 0.04-0.08MPa.
The cobalt salt additive is cobaltous dichloride and/or cobalt acetate.In one embodiment of the present invention, the cobalt salt adds
Agent is added to be made of 25-35wt% cobaltous dichlorides and 65-75wt% cobalt acetates.
A kind of preparation method of electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, cosolvent, zinc acetate, cobalt
Salt additives, coupling agent are added in ethyl alcohol, are heated to 60-80 DEG C, are stirred 2-5 hours and mixed with 100-500 revs/min of rotating speed
Uniformly, after being cooled to room temperature to get.
Beneficial effects of the present invention：Electrothermal film sol of the present invention and preparation method thereof, solution component is simple, and it is convenient to prepare,
Without discharging of waste liquid, the electrothermal film sol uniformity is high, and homogeney is good, thus the structural compactness of Electric radiant Heating Film prepared by colloidal sol, extends
The service life of Electric radiant Heating Film bears that voltage is high, power is big, has good performance.
Specific embodiment
Heating element preparation is carried out using electrothermal film sol prepared by embodiment：
(1) it is cleaned with ethanol Quartz glass surfaces, is subsequently placed in air dry oven 80 DEG C of dryings 2 hours,
Quartz glass after being dried；
(2) electrothermal film sol is heated as steam, vapor (steam) temperature is 230 DEG C, and steam is by nitrogen jet in quartzy glass
The surface of glass, quartz glass temperature are 600 DEG C, jet length 25cm, carrier gas flux 50L/min, and steam shallow lake stain is in quartz
Glass surface forms the film that thickness is 5 μm；
(3) film is sintered, sintering temperature is 760 DEG C, and sintering time is 20 minutes, then by sintered film
Natural cooling in air obtains Electric radiant Heating Film；
(4) in Electric radiant Heating Film surface smear silver paste, the heat treatment of 10 minutes is carried out at being then 800 DEG C in temperature, is obtained
Heating element.
Adhesion property is tested：According to national machinery industry standard JB/T 8554-1997《Vapor deposition film is attached with matrix
The scratch method for test puted forth effort》It carries out.It is tested using the automatic scratching instrument of WS-2005 type coating adhesion, test method is sound
Emission measurement mode is tested, loading speed 5N/min, cut rate 2mm/min.
Resistance change rate is tested：The resistance change rate of heating element is tested, using the on-load voltage of 190V, uses VC
9801A types multimeter measures line current virtual value, and the heating rate of heating element is 2 DEG C/min, and one was read every ten minutes
Secondary numerical value calculates resistance value according to institute's measured data, then asks for average resistance, the long-life heating element obtained
Resistance change rate when at 1000 DEG C relative to room temperature is denoted as A (%)；It works at 1000 DEG C after 1000h, according to test data
Calculate resistance value, the resistance after the 1000h that then asks for working at 1000 DEG C relative to work at 1000 DEG C 1h when resistance
Change rate, be denoted as B (%).
Butter of tin in embodiment, No. CAS：10026-06-9.
Cobalt acetate in embodiment, No. CAS：71-48-7.
Cobaltous dichloride in embodiment, No. CAS：7646-79-9.
Isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters in embodiment, No. CAS：65345-34-8.
Ceria in embodiment, No. CAS：1306-38-3.
Potassium acetate in embodiment, No. CAS：127-08-2.
Zinc acetate in embodiment, No. CAS：557-34-6.
Ethyl alcohol in embodiment, No. CAS：64-17-5.
Titanium tetrachloride in embodiment, No. CAS：7550-45-0.
Acetic acid in embodiment, No. CAS：64-19-7.
Two oleic acid acyloxy of isopropyl (dioctyl phosphoric acid acyloxy) titanate esters are by the excellent general chemical science and technology in Nanjing in embodiment
Co., Ltd provides, model UP-101.
Embodiment 1
Electrothermal film sol raw material (parts by weight)：50 parts of butter of tin, 3 parts of potassium acetate, 2 parts of titanium tetrachloride, 2 parts of acetic acid, vinegar
Sour 3 parts of zinc, 2 parts of cobalt acetate, 25 parts of ethyl alcohol, modified isopropyl three (dioctyl phosphoric acid acyloxy) 3 parts of titanate esters.
The preparation method of modified isopropyl three (the dioctyl phosphoric acid acyloxy) titanate esters is：By isopropyl three, (two is pungent
Base phosphoric acid acyloxy) titanate esters and ceria be 5.5 in molar ratio：1 mixing, using rotating speed as 150r/ at being 120 DEG C in temperature
Min is stirred to react 3 hours, obtains reactant；By reactant temperature be 80 DEG C, vacuum degree be 0.07MPa dry 7 hours to obtain the final product
Modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters.
The preparation method of above-mentioned electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, acetic acid, zinc acetate, acetic acid
Cobalt, modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters are added in ethyl alcohol, are heated to 70 DEG C, with 300 revs/min turn
Speed stirring is uniformly mixed for 3 hours, is cooled to room temperature after 20 DEG C to get electrothermal film sol.
Embodiment 2
Electrothermal film sol raw material (parts by weight)：50 parts of butter of tin, 3 parts of potassium acetate, 2 parts of titanium tetrachloride, 2 parts of acetic acid, vinegar
Sour 3 parts of zinc, 2 parts of cobalt acetate, 25 parts of ethyl alcohol, modified isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) 3 parts of titanate esters.
The preparation method of two oleic acid acyloxy of modified isopropyl (the dioctyl phosphoric acid acyloxy) titanate esters is：By isopropyl
Two oleic acid acyloxy of base (dioctyl phosphoric acid acyloxy) titanate esters are 5.5 in molar ratio with ceria：1 mixes, and is in temperature
It is stirred to react 3 hours by 150r/min of rotating speed at 120 DEG C, obtains reactant；By reactant temperature is 80 DEG C, vacuum degree is
0.07MPa dries 7 hours up to modified isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters.
The preparation method of above-mentioned electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, acetic acid, zinc acetate, acetic acid
Cobalt, modified isopropyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanate esters are added in ethyl alcohol, 70 DEG C are heated to, with 300
Rev/min rotating speed stir 3 hours be uniformly mixed, be cooled to room temperature after 20 DEG C to get electrothermal film sol.
Embodiment 3
Electrothermal film sol raw material (parts by weight)：50 parts of butter of tin, 3 parts of potassium acetate, 2 parts of titanium tetrachloride, 2 parts of acetic acid, vinegar
Sour 3 parts of zinc, 2 parts of cobalt acetate, 25 parts of ethyl alcohol, isopropyl three (dioctyl phosphoric acid acyloxy) 3 parts of titanate esters.
The preparation method of above-mentioned electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, acetic acid, zinc acetate, acetic acid
Cobalt, isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters are added in ethyl alcohol, are heated to 70 DEG C, are stirred with 300 revs/min of rotating speed
It mixes 3 hours and is uniformly mixed, be cooled to room temperature after 20 DEG C to get electrothermal film sol.
Embodiment 4
Electrothermal film sol raw material (parts by weight)：50 parts of butter of tin, 3 parts of potassium acetate, 2 parts of titanium tetrachloride, 2 parts of acetic acid, vinegar
Sour 3 parts of zinc, 2 parts of cobaltous dichloride, 25 parts of ethyl alcohol, modified isopropyl three (dioctyl phosphoric acid acyloxy) 3 parts of titanate esters.
The preparation method of modified isopropyl three (the dioctyl phosphoric acid acyloxy) titanate esters is：By isopropyl three, (two is pungent
Base phosphoric acid acyloxy) titanate esters and ceria be 5.5 in molar ratio：1 mixing, using rotating speed as 150r/ at being 120 DEG C in temperature
Min is stirred to react 3 hours, obtains reactant；By reactant temperature be 80 DEG C, vacuum degree be 0.07MPa dry 7 hours to obtain the final product
Modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters.
The preparation method of above-mentioned electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, acetic acid, zinc acetate, dichloro
Change in cobalt, modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters addition ethyl alcohol, 70 DEG C are heated to, with 300 revs/min
Rotating speed is stirred 3 hours and is uniformly mixed, and is cooled to room temperature after 20 DEG C to get electrothermal film sol.
Embodiment 5
Electrothermal film sol raw material (parts by weight)：50 parts of butter of tin, 3 parts of potassium acetate, 2 parts of titanium tetrachloride, 2 parts of acetic acid, vinegar
Sour 3 parts of zinc, 1.4 parts of cobalt acetate, 0.6 part of cobaltous dichloride, 25 parts of ethyl alcohol, modified isopropyl three (dioctyl phosphoric acid acyloxy) metatitanic acid
3 parts of ester.
The preparation method of modified isopropyl three (the dioctyl phosphoric acid acyloxy) titanate esters is：By isopropyl three, (two is pungent
Base phosphoric acid acyloxy) titanate esters and ceria be 5.5 in molar ratio：1 mixing, using rotating speed as 150r/ at being 120 DEG C in temperature
Min is stirred to react 3 hours, obtains reactant；By reactant temperature be 80 DEG C, vacuum degree be 0.07MPa dry 7 hours to obtain the final product
Modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters.
The preparation method of above-mentioned electrothermal film sol, by butter of tin, potassium acetate, titanium tetrachloride, acetic acid, zinc acetate, dichloro
Change cobalt, cobalt acetate, modified isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters to add in ethyl alcohol, 70 DEG C are heated to, with 300
Rev/min rotating speed stir 3 hours be uniformly mixed, be cooled to room temperature after 20 DEG C to get electrothermal film sol.By electrothermal film sol system
It into heating element, is then tested for the property, resistance change rate test result is：A=0.71%, B=0.82%；Adhesion property
Test result is：Adhesive force is 228N.
Test case 1
The electrothermal film sol of embodiment 1-4 is respectively adopted heating element is made, is then tested for the property.Specific test
It the results are shown in Table 1.
Table 1：Performance test table
Electrothermal film sol of the present invention and preparation method thereof, solution component is simple, and it is convenient to prepare, no discharging of waste liquid, Electric radiant Heating Film
The colloidal sol uniformity is high, and homogeney is good, thus the structural compactness of Electric radiant Heating Film prepared by colloidal sol, and extend Electric radiant Heating Film uses the longevity
It orders, bear that voltage is high, power is big, there is good performance.
Claims (10)
1. a kind of electrothermal film sol, which is characterized in that be prepared by following raw materials：Butter of tin, potassium acetate, titanium tetrachloride,
Cosolvent, zinc acetate, cobalt salt additive, ethyl alcohol, coupling agent.
2. a kind of electrothermal film sol, which is characterized in that be prepared by the raw material of following weight parts：40-60 parts of butter of tin, vinegar
Sour potassium 2-5 parts, 1-3 parts of titanium tetrachloride, 1-5 parts of cosolvent, 2-5 parts of zinc acetate, 1-3 parts of cobalt salt additive, 20-30 parts of ethyl alcohol,
2-5 parts of coupling agent.
3. electrothermal film sol according to claim 2, it is characterised in that：The cosolvent is acetic acid or hydrochloric acid.
4. electrothermal film sol according to claim 2, it is characterised in that：The cobalt salt additive is cobaltous dichloride and/or second
Sour cobalt.
5. electrothermal film sol according to claim 2, it is characterised in that：The coupling agent is (the dioctyl phosphoric acid of isopropyl three
Acyloxy) titanate esters.
6. electrothermal film sol according to claim 2, it is characterised in that：The coupling agent is three (dioctyl of modified isopropyl
Phosphoric acid acyloxy) titanate esters.
7. electrothermal film sol according to claim 6, it is characterised in that：(the dioctyl phosphoric acid acyl-oxygen of modified isopropyl three
Base) preparation methods of titanate esters is：It is in molar ratio with ceria by isopropyl three (dioctyl phosphoric acid acyloxy) titanate esters
(3-7)：1 mixing is stirred to react 2-4 hours at being 115-125 DEG C in temperature, obtains reactant；Reactants dry 5-10 is small
When to obtain the final product.
8. electrothermal film sol according to claim 7, it is characterised in that：The rotating speed of the stirring is 100-300r/min.
9. electrothermal film sol according to claim 7, it is characterised in that：The temperature of the drying is 70-90 DEG C, vacuum degree is
0.04-0.08MPa。
10. according to the preparation method of any one of the claim 1-9 electrothermal film sols, it is characterised in that：By butter of tin,
Potassium acetate, titanium tetrachloride, cosolvent, zinc acetate, cobalt salt additive, coupling agent are added in ethyl alcohol, are heated to 60-80 DEG C, with
100-500 revs/min of rotating speed stir 2-5 hour it is uniformly mixed, after being cooled to room temperature to get.
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Cited By (1)
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