CN104658722A - Preparation method of polyimide insulation particles - Google Patents
Preparation method of polyimide insulation particles Download PDFInfo
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- CN104658722A CN104658722A CN201410744361.7A CN201410744361A CN104658722A CN 104658722 A CN104658722 A CN 104658722A CN 201410744361 A CN201410744361 A CN 201410744361A CN 104658722 A CN104658722 A CN 104658722A
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Abstract
The invention discloses a preparation method of polyimide insulation particles, and belongs to the field of material preparation. The preparation method comprises the following steps: dipping cylindrical activated carbon in distilled water, washing the dipped cylindrical activated carbon, placing the washed cylindrical activated carbon in a beaker, boiling the cylindrical activated carbon placed in the beaker, standing and cooling the boiled cylindrical activated carbon, filtering the cooled cylindrical activated carbon so as to remove the water, putting the dewatered cylindrical activated carbon into a dryer, and drying the cylindrical activated carbon for standby; macerating the pretreated activated carbon in a polyamic acid solution, after slightly stirring, taking out the activated carbon, spreading the activated carbon on a glass plate so that a polyamic acid film is formed on the surface of the activated carbon, placing into a vacuum dryer, warming so as to remove a solvent, and performing thermal imidization so as to form a PI film; taking out the coated insulation particles, and naturally cooling to an indoor temperature so as to obtain the insulation particles. Through the improvement of a technology, dip coating and cyclodehydration are performed to prepare the PI insulation particles, so that the prepared particles have an excellent electrical insulation property, a short-circuit current is effectively reduced, the current efficiency is improved, and an electrolysis effect on dyestuff wastewater by a three-dimensional electrode reactor is improved; the preparation method disclosed by the invention is simple in technology, easy to operate and suitable for popularization.
Description
Technical field
the invention belongs to field of material preparation, particularly relate to a kind of preparation method of polyimide insulative particle.
Background technology
Along with the development of science and technology, many new materials are applied to the every aspect of living.Three-diemsnional electrode catalytic oxidation is a kind of novel high-level oxidation technology, have operating condition gentleness, non-secondary pollution, generation OH can by advantages such as persistent organic pollutants mineralisings.Mostly select quartz sand, bead, plastic or other material as insulating particle in bipolar three-dimensional electrode reactor, and as bed filler after mixing with granule electrode by certain volume ratio or mass ratio, but because the material of the insulating particles such as quartz sand, bead, plastics, density, geomery differ very large with granule electrode, be difficult to make it to be evenly distributed in granule electrode, effectively can not reduce short circuit current, the phenomenon of electrode material and insulating material layering is produced in operation, even cause failure of insulation, cause short circuit current.
Summary of the invention
The present invention is intended to solve the problem, and provides a kind of preparation method of polyimide insulative particle.
A preparation method for polyimide insulative particle, is characterized in that comprising the steps:
(1) by column type active carbon distilled water immersion, rinse and be placed in beaker, boil and boil elimination moisture after rear standing cooling, put into baking oven dry after stand-by;
(2) pretreated active carbon is immersed in polyamic acid solution, take out after mild agitation, divide and make activated carbon surface form Polyamic Acid Film on glass plate, insert in vacuum drying oven, be warming up to 110 DEG C and be incubated 50min desolvation, continue to be warming up to 310 DEG C and after being incubated 60min, hot imidization forms PI film;
(3) taking-up of film insulating particle is naturally cooled to room temperature, repeat the insulating particle that above-mentioned steps (2) once can be prepared into the PI film of Surface coating even compact.
The preparation method of a kind of polyimide insulative particle of the present invention, is characterized in that described in step (1), column type active carbon is 4mm.
The preparation method of a kind of polyimide insulative particle of the present invention, is characterized in that described in step (1), soak time is 8 ~ 12h.
The preparation method of a kind of polyimide insulative particle of the present invention, the time of boiling that it is characterized in that boiling described in step (1) is 10 ~ 15min.
The preparation method of a kind of polyimide insulative particle of the present invention, is characterized in that described in step (1), washing time is 3 times.
The preparation method of a kind of polyimide insulative particle of the present invention, by the improvement to technique, dipping film, cyclodehydration have prepared PI insulating particle, prepared particle is made to have excellent electrical insulation capability, effectively reduce short circuit current, improve current efficiency, improve the electrolysis effectiveness of 3 D electrode reactor to waste water from dyestuff.Present invention process is simple, is easy to operation, is applicable to promoting.
Embodiment
A preparation method for polyimide insulative particle, comprises the steps:
(1) by column type active carbon distilled water immersion, rinse and be placed in beaker, boil and boil elimination moisture after rear standing cooling, put into baking oven dry after stand-by;
(2) pretreated active carbon is immersed in polyamic acid solution, take out after mild agitation, divide and make activated carbon surface form Polyamic Acid Film on glass plate, insert in vacuum drying oven, be warming up to 110 DEG C and be incubated 50min desolvation, continue to be warming up to 310 DEG C and after being incubated 60min, hot imidization forms PI film;
(3) taking-up of film insulating particle is naturally cooled to room temperature, repeat the insulating particle that above-mentioned steps (2) once can be prepared into the PI film of Surface coating even compact.
The preparation method of a kind of polyimide insulative particle of the present invention, described in step (1), column type active carbon is 4mm.Described in step (1), soak time is 8 ~ 12h.Time of boiling of boiling described in step (1) is 10 ~ 15min.Described in step (1), washing time is 3 times.By changing the different volumes ratio of PI insulating particle and activated carbon particles in bed filler, investigate its impact on Electrocatalysis Degradation effect, to determine the optimum volume ratio of insulating particle and activated carbon particles in bed filler.When insulating particle content in bed filler is less, active carbon is excessive, active carbon directly contacts and causes short circuit, makes the ratio that in bed, activated carbon particles becomes granule electrode by electrostatic induction low, and thus the degradation efficiency of system is low.Along with the increase of insulating particle and activated carbon particles volume ratio, percent of decolourization and COD clearance improve constantly, when insulating particle and active carbon volume ratio reach 1/3, percent of decolourization and COD clearance the highest, what PI insulating particle was described adds the short circuit current effectively reduced in bed filler between granule electrode, improves the degradation efficiency of using three-dimensional electrodes system to waste water from dyestuff.After this, continue to increase insulating particle, percent of decolourization and COD clearance decline on the contrary.This is because the function of insulating particle is the short circuit current stoping the direct contact in bed between granule electrode and cause, insulating particle itself can not play the effect of micro cell, therefore, along with the increase of insulating particle and active carbon volume ratio, insulation effect improves, but activated carbon particles ratio is more and more less.Within the scope of 15 ~ 25 V, percent of decolourization and COD clearance all improve with the increasing of voltage, and when voltage reaches 25V, COD clearance reaches the highest.This is the increase due to applied voltage, make the ratio of the number of particles becoming granule electrode in bed because of electrostatic induction, namely the multipole rate of granule electrode improves, the increase of applied voltage simultaneously adds the power of electrochemical reaction, if when continuing high voltage to 30 V, although percent of decolourization still improves, but the amplitude improved is very little, and COD clearance declines slightly, this may be because too high voltage exacerbates the hydrolysis on activated carbon surface or occurs caused by other side reaction, therefore, decomposition voltage with 25 V for the best., in the scope that pH value is 2 ~ 5, waste water from dyestuff colourity and COD all can be removed preferably, and best initial pH value is 4.Solution pH value not only affects main electrode and granule electrode to the absorption of dyestuff, also affects the electric charge on main electrode and granule electrode surface, thus affects the catalytic oxidation efficiency of whole system; The reduction of oxygen evolution potential, adds side reaction in the basic conditions, reduces current efficiency, thus affects electrolysis effectiveness.And in sour environment, the intermediate product in dye oxidation process is easier to be degraded further, promotes that electrode transfers the water electrolysis catalyst on its surface to hydrogen peroxide, accelerate the oxidative degradation of dye molecule.In addition, the hydroxyl radical free radical under acid condition has stronger oxidizability, and dyestuff is more easily oxidized.But pH value is lower, is more conducive to H
+h is reduced at the cathode terminal of minus plate and granule electrode
2, decrease hydrogen peroxide productive rate thus decrease the productive rate of hydroxyl radical free radical.Excessive aeration rate reduces the absorption of dyestuff at electrode surface, and makes the hydrogen peroxide that produces in electro-catalysis process and hydroxyl radical free radical cancellation, thus reduces degradation efficiency.When pH value is greater than 13, PI film starts to occur dissolving, and strengthens with the increasing of pH value.But the acid-alkali-corrosive-resisting performance of PI insulating particle has been much better than cellulose acetate Coated Activated Carbon, thus as the insulating particle of bipolar three-dimensional electrode reactor, its scope of application will be more wide.
Claims (5)
1. a preparation method for polyimide insulative particle, is characterized in that comprising the steps:
(1) by column type active carbon distilled water immersion, rinse and be placed in beaker, boil and boil elimination moisture after rear standing cooling, put into baking oven dry after stand-by;
(2) pretreated active carbon is immersed in polyamic acid solution, take out after mild agitation, divide and make activated carbon surface form Polyamic Acid Film on glass plate, insert in vacuum drying oven, be warming up to 110 DEG C and be incubated 50min desolvation, continue to be warming up to 310 DEG C and after being incubated 60min, hot imidization forms PI film;
(3) taking-up of film insulating particle is naturally cooled to room temperature, repeat the insulating particle that above-mentioned steps (2) once can be prepared into the PI film of Surface coating even compact.
2. the preparation method of a kind of polyimide insulative particle as claimed in claim 1, is characterized in that described in step (1), column type active carbon is 4mm.
3. the preparation method of a kind of polyimide insulative particle as claimed in claim 1, is characterized in that described in step (1), soak time is 8 ~ 12h.
4. the preparation method of a kind of polyimide insulative particle as claimed in claim 1, the time of boiling that it is characterized in that boiling described in step (1) is 10 ~ 15min.
5. the preparation method of a kind of polyimide insulative particle as claimed in claim 1, is characterized in that described in step (1), washing time is 3 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410744361.7A CN104658722A (en) | 2014-12-09 | 2014-12-09 | Preparation method of polyimide insulation particles |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410744361.7A CN104658722A (en) | 2014-12-09 | 2014-12-09 | Preparation method of polyimide insulation particles |
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| CN104658722A true CN104658722A (en) | 2015-05-27 |
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| CN201410744361.7A Pending CN104658722A (en) | 2014-12-09 | 2014-12-09 | Preparation method of polyimide insulation particles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386132A (en) * | 2022-08-12 | 2022-11-25 | 华南理工大学 | Low dielectric polyimide film with electrostatic spinning high molecular organic porous film as pore-forming sacrificial template and preparation method thereof |
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2014
- 2014-12-09 CN CN201410744361.7A patent/CN104658722A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115386132A (en) * | 2022-08-12 | 2022-11-25 | 华南理工大学 | Low dielectric polyimide film with electrostatic spinning high molecular organic porous film as pore-forming sacrificial template and preparation method thereof |
| CN115386132B (en) * | 2022-08-12 | 2023-06-20 | 华南理工大学 | Low dielectric polyimide film taking electrostatic spinning high molecular organic porous film as pore-forming sacrificial template and preparation method thereof |
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Application publication date: 20150527 |