CN102945974B - Method for preparing sealing pad of solid oxide fuel cell and waste material recovery process - Google Patents
Method for preparing sealing pad of solid oxide fuel cell and waste material recovery process Download PDFInfo
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- CN102945974B CN102945974B CN201210469835.2A CN201210469835A CN102945974B CN 102945974 B CN102945974 B CN 102945974B CN 201210469835 A CN201210469835 A CN 201210469835A CN 102945974 B CN102945974 B CN 102945974B
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention provides a method for preparing a sealing pad of a solid oxide fuel cell and a recovery and utilization method of waste materials generated in the method. Powder of sealing materials are subjected to ball grinding and mixing after being matched with dispersing agents, bonding agents, plasticizing agents and solvents, casting and drying are carried out after the screen net filtering and the vacuum defoamation, blanks are cut according to the overall dimension requirement of the sealing pad, multiple layers are stacked and aligned, then, PET (polyethylene terephthalate) films and stainless steel plates are sequentially padded at two sides, the materials are filled into a plastic package bag for vacuum pumping and plastic package and are then placed on a hot pressing machine for hot pressing, and the materials are taken out to be cut into the sealing pad in specified sizes. Waste materials after cutting are collected, are subjected to ball grinding and mixing after being matched with the solvents and can be continuously used for preparing the sealing pad.
Description
Technical field
The present invention relates to the preparation method of sealing gasket for a kind of solid fuel cell, relate in particular to the recycling method of the waste material producing in a kind of method of preparing described sealing gasket and described production method.
Background technology
Solid Oxide Fuel Cell (SOFC) is chemical energy to be converted into all solid state Blast Furnace Top Gas Recovery Turbine Unit (TRT) of electric energy.The advantages such as the energy conversion efficiency that has based on it is high, environmentally friendly, wide to fuel tolerance, long service life, SOFC is a kind of energy utilization patterns with broad prospect of application.
The common structure of SOFC has tubular type and flat, and other structures that derived by these two kinds of basic structures.Wherein planar SOFC is simple with its preparation technology, production cost is low, assemble the advantages such as time-histories order in heaps is simple, is the study hotspot of SOFC.For planar SOFC, the sealing of battery is a key technology.When SOFC normally works, the Main Function of encapsulant has: 1) isolated fuel gas and air; 2) assemblies such as connecting plate and monocell are linked together formation pile; 3) guarantee the electrical insulating property between connecting plate, prevent connecting plate short circuit current.
Therefore the requirement that, encapsulant must meet has: 1) under oxidation and reducing atmosphere, all have higher chemical stability; 2) and between seal, sealing materials, had good chemical compatibility; 3) with by the matched coefficients of thermal expansion of seal, sealing materials; 4) with by the wettability of seal, sealing materials better and stronger adhesion; 5), under the working temperature of SOFC, there is higher long-term thermal stability.Except this thinks, encapsulant also necessary production cost is low, is applicable to batch production, and steady quality is reliable.
At present the research of SOFC Sealing Technology is mainly contained to means of press seals and hard sealing.Means of press seals is to adopt the concept of " sealing ring " to realize sealing, and the encapsulant (as mica, flexible graphite etc.) that is filled in SOFC inter-module by compacting reaches sealing purpose.Hard sealing refers to that between encapsulant and SOFC assembly be hard connection, does not produce plastic deformation, the sealing that can not do relative motion after sealing-in.The seal, sealing materials that hard sealing adopts mainly contains glass, devitrified glass, glass ceramics etc.
The method of forming materials that the current common hard method for sealing of employing carries out sealing-in mainly contains: die casting (as CN1812159A, CN101651188A, CN1494176A), curtain coating (as CN102386345A, CN101079476A, CN101174677A), roll forming (as CN1465647A, CN1599092A, CN1884423A), slurry coating method (as CN1234617A, CN101075665A, CN101174677A), and spraying etc.These forming methods respectively have pluses and minuses.For example, slurry coating method is also not suitable for large area batch production, and thickness evenness when reason is large area coating coating slurry is wayward.For die casting method, because needs customize specific mould in advance according to size, dimension modifying generally must change mould, has improved cost.For the tape casting, production technology is simple, with low cost, is applicable to batch production.But when preparing planar SOFC sealing gasket, the waste of raw material is more serious.Reason is, when reality is used, sealing area is general only need to be at the periphery of battery, and the shape of sealing gasket is mostly ring-type, and when the dried biscuit of curtain coating is carried out to cutting, core region can be scratched and remove, and this just causes raw material to be greatly wasted.In addition, rolling film, the methods such as roll forming also can run into analogue.Up to now, not yet find to carry out for the waste material after cutting the patent report of recycling.When waste material is reclaimed, the problem that may occur is: compare with original powder, the powder in waste material has passed through ball milling dispersion, hot pressing, and after the steps such as curtain coating oven dry, its diameter of particle distributes and great changes have occurred accumulation situation.Consistency while how to guarantee to use waste material to prepare sealing gasket and use original powder to prepare sealing gasket, control through strict.Otherwise in sealing-in process, the intensification retractable property of sealing gasket can great changes will take place, easily cause sealing-in failure.
After having assembled by sealing gasket with by the battery component of sealing-in, through heat treatment step, carry out sealing-in.In temperature-rise period, because the organic additive in sealing gasket is burned, sealing matrix itself also has sintering shrinkage.When shrinkage is excessive, sealing gasket easily shrinks fracture, causes sealing-in failure.Patent CN101079476A mentions, and before assembling, sealing gasket is carried out to precompressed, improves the bulk density of powder, can improve sealing-in success rate.But mention equally, excessive preload pressure may cause sealing gasket to take off from press the problem encountering difficulties.
In addition, for reaching good sealing effectiveness, sealing gasket need to possess certain thickness, simultaneously even thickness.In flow casting molding, when curtain coating thickness surpasses certain limit, the thickness evenness of biscuit is wayward.Must adopt the sealing gasket biscuit of curtain coating suitable thickness, then use the hot pressing of multilayer biscuit lamination, and then obtain the method for the thick biscuit of desired thickness, just can evade above problem.
Summary of the invention
The problems referred to above that exist based on existing technology, the invention provides the preparation technology of sealing gasket for a kind of planar SOFC, and object is to solve the tape casting while preparing sealing gasket, and raw material availability is too low, wastes serious problem; Solution sealing gasket is because the restriction of drying time causes production efficiency to be limited by the problem of curtain coating table top length; Solve the excessive too low problem of sealing-in success rate that causes of sealing gasket shrinkage in heat treatment process; Inhomogeneity problem when solving thick sealing gasket and preparing.
In order to realize above object, the present invention is achieved through the following technical solutions: select suitable solvent, dispersant, organic binder bond and plasticiser to mix with encapsulant powder successively and ball milling, after filtration and vacuum defoamation, obtain the high stable slurry of solid content; When casting slurry, slurry is poured over to PET counterdie surface, along with the drive of PET counterdie forward, be equipped with heating steps, dry completely when guaranteeing that slurry arrives curtain coating table top end, then roll together with PET counterdie; First according to the Outside Dimensions of sealed battery component, curtain coating biscuit is cut, biscuit multiple-layer stacked is alignd, PET film and corrosion resistant plate on the pad of biscuit both sides, then put into plastic packaging bag and vacuumize processing, be placed on again on hot press, under certain temperature and pressure, carry out hot pressing pressurize a period of time; After taking-up, according to the concrete size of seal request, carry out again cutting, can obtain for actual sealing gasket.
First aspect of the present invention is to provide a kind of method of sealing gasket for Solid Oxide Fuel Cell (SOFC) of preparing, and described method comprises the steps:
Step 1, by ball milling after encapsulant powder and A/B mixed solvent, dispersant, obtains slurry;
Step 2, ball milling after slurry described in step 1 is mixed with binding agent and plasticiser;
Step 3, by gained slurry in step 2 through 60 ~ 200 eye mesh screens sieve, vacuum defoamation, be poured over and on PET counterdie, carry out curtain coating, and driven forward by PET counterdie, wherein in curtain coating process, slurry thickness is controlled at 0.1 ~ 0.3mm, and curtain coating table top is heated to 45 ~ 85 ℃, removes PET counterdie and obtains biscuit;
Step 4, at least one deck biscuit stack alignment, carries out hot pressing, and wherein, hot pressing pressure is 10 ~ 50MPa, and temperature is 50 ~ 90 ℃, and the dwell time is 10 ~ 20min.
Step 5, carries out cutting by the biscuit after hot pressing according to the concrete size of seal request, and obtaining can the actual sealing gasket using.
In step 1, A is aromatic hydrocarbon solvent, is preferably any one or a few in benzene, alkyl benzene, halogeno-benzene, as toluene, dimethylbenzene, chlorobenzene etc., most preferably is dimethylbenzene.
B is the represented ester of R1-C (O)-O-R2, wherein, R1 and R2 can be identical or different, and respectively independently selected from the alkyl of C1 ~ C5, described alkyl can be straight or branched alkyl, as methyl, ethyl, n-pro-pyl, isopropyl, normal-butyl, isobutyl group, the tert-butyl group, n-pentyl, the concrete example of B, as ethyl acetate, butyl acetate, most preferably is butyl acetate.
Wherein, the mass ratio of A and B is 1
:0.5 ~ 2.
In step 1, described dispersant can be inorganic dispersant, but be preferably organic dispersing agent, as lauryl sodium sulfate, cellulose derivative (methylcellulose, ethyl cellulose, carboxymethyl cellulose), fatty acid polyglycol ethylene glycol, tristerin, polyethylene glycol etc.
In step 1, in the mixture of encapsulant powder and A/B mixed solvent, dispersant, A/B mixed solvent percentage by weight is preferably 10 ~ 40wt%, and dispersant percentage by weight is preferably 1 ~ 10wt%.
In step 1, described ball milling is preferably selects roller milling machine, and in mechanical milling process, rotating speed is preferably 60～200rpm, and Ball-milling Time is 2 ~ 12h.
In step 2, binding agent is selected from any one or a few in cellulose derivative (as sodium carboxymethylcellulose, hydroxypropyl cellulose, methylcellulose and cellulose), animal glue (as gelatin), araldite (as acrylic resin, epoxy resin, polyvinyl acetate).
In step 2, described plasticiser can be any one or a few in phthalic acid ester (as DBP, DOP, DIDP), aliphatic dicarboxylic acid ester (as dioctyl adipate, dioctyl sebacate), epoxy compounds (as epoxidized soybean oil, epoxyoleic acid butyl ester), synthetic resin plasticizer (as PPA), chlorinated paraffin wax.
In step 2, in described slurry, binding agent, elasticizer mixture, weight of binder percentage is preferably 1 ~ 10wt%, and plasticiser percentage by weight is preferably 1 ~ 10wt%.
In step 2, described ball milling is preferably selects roller milling machine, and in mechanical milling process, rotating speed is preferably 20 ~ 100rpm, and Ball-milling Time is 2 ~ 12h.
In step 4, more preferably, after described at least one laminin base stack, carry out vacuum treatment, to remove the air between each laminin base, then carry out hot pressing.In a kind of preferred embodiment of the present invention, biscuit is inserted in variable airtight container (as plastic packaging bag), vacuumizes, and then the biscuit in the airtight container of vacuum carries out hot pressing.
In addition, the present invention during for cutting sealing gasket remaining waste material carry out centralized recovery, after adding a certain proportion of solvent, carry out ball milling at a slow speed, can guarantee that significant change does not occur again the consoluet while diameter of particle of waste material, thereby obtain the stable slurry of the continued on for curtain coating that consistency is high.
Therefore,, according to a kind of preferred implementation of the method for the invention, step also comprises:
Step 6, reclaims waste material unnecessary after cutting biscuit, mixes with A/B mixed solvent, with roller milling machine ball milling 2 ~ 12h under 20 ~ 100rpm rotating speed, obtains being recycled and reused for the stable slurry of curtain coating, repeats above-mentioned steps 3 ~ step 5.
In step 6, A/B mixed solvent is identical with step 1, and its consumption accounts for the 10 ~ 50wt% that reclaims waste material and mixed solvent total weight.
The invention has the advantages that:
1) the present invention is not limited by the restriction of curtain coating table top length, can realize in batches and producing continuously, thereby greatly improve productive rate.
2) the present invention, by the recycling to biscuit waste material, has improved the utilance of sealing raw material, has significantly reduced cost.
3) the present invention adopts the method for multilayer biscuit lamination hot pressing, has improved the bulk density of solid particle in sealing gasket, has significantly reduced the shrinkage of sealing gasket in high-temperature process, thereby has greatly improved sealing-in success rate.
4) the present invention adopts the method for multilayer biscuit lamination hot pressing, has evaded direct curtain coating uppity problem of thickness evenness while preparing thick sealing gasket.
Accompanying drawing explanation
Fig. 1 be embodiment of the present invention sealing bag to 10 battery pile sealing-ins before photo;
Fig. 2 be embodiment of the present invention sealing bag to 10 battery pile sealing-ins after photo.
Embodiment
The invention provides a kind of method of the waste recovery recycling producing in the method for sealing gasket and the method for Solid Oxide Fuel Cell of preparing.The powder of encapsulant is mixed after dispersant, binding agent, plasticiser and the mixing of solvent ball milling, through screen filtration and vacuum defoamation, carry out curtain coating and dry, according to the requirement of sealing gasket Outside Dimensions, biscuit is carried out to cutting, to after multilayer biscuit stack alignment, in both sides, pad successively PET film and corrosion resistant plate, pack plastic packaging bag into and vacuumize plastic packaging, be then placed on hot press and carry out hot pressing, after taking-up, be cut into the sealing gasket of given size.Waste material after cutting is collected, carried out ball milling mixing after mixing solvent, can continue on for the preparation of sealing gasket.
The present invention is described in more detail with reference to following examples, but following embodiment should not be interpreted as limitation of the scope of the invention.
embodiment 1
the tape casting is prepared sealing gasket biscuit
Take 120g encapsulant powder, join 25g dimethylbenzene and butyl acetate (by 1
:1 mass ratio) in mixed solvent, then add 6g dispersant, with tumbling ball mill ball milling under 125rpm rotating speed, within 8 hours, mix.
Add again 4g binding agent and 4g plasticiser, with tumbling ball mill ball milling under 80rpm rotating speed, within 8 hours, mix, obtain the stable slurry of modest viscosity.
Slurry sieves and after vacuum defoamation processes through 190 eye mesh screens, be poured on PET counterdie, along with the drive of counterdie forward, after the scraper that is 0.3mm through knife up, obtain the biscuit of even thickness, curtain coating table top is heated to 50 ℃ simultaneously, when biscuit arrives curtain coating table top end along with PET counterdie is rolled-up together.
the preparation of sealing gasket
Biscuit is taken off from PET counterdie, by 6 laminin base lamination alignment, in both sides, respectively padded one deck PET film and corrosion resistant plate.Put into plastic packaging bag and vacuumize processing, object is air remaining between shielding layer.
Be placed under hot press and carry out hot pressing, wherein hot press pressure is 20MPa, and the dwell time is 10min, and temperature is 75 ℃.
After taking out from plastic packaging bag, the biscuit according to the concrete size of seal request after to hot pressing carries out cutting, can obtain the sealing gasket of actual use.
Advantage of the present invention has, and the sealing gasket sealing-in success rate of preparing is high, and raw material availability is high, is applicable to producing continuously in batches.
embodiment 2
the recovery of sealing gasket biscuit waste material
Remaining biscuit waste material after cutting in recovery embodiment 1.
Take 80g sealing gasket biscuit waste material, mix 30g dimethylbenzene and butyl acetate (by 1
:1 mass ratio) mixed solvent, mixes with tumbling ball mill ball milling under 80rpm rotating speed for 8 hours; Method described in repetition embodiment 1 is prepared the subsequent step of sealing gasket biscuit.
After tested, sealing gasket prepared by the waste material utilize reclaiming, does not have difference with the performance such as the thermal endurance of the sealing gasket of preparation in embodiment 1, resistance to morphotropism.
embodiment 3
the tape casting is prepared sealing gasket biscuit
Take 120g encapsulant powder, join 40g dimethylbenzene and butyl acetate (by 1
:2 mass ratioes) in mixed solvent, then add 10g dispersant, with tumbling ball mill ball milling under 125rpm rotating speed, within 8 hours, mix.
Add again 6g binding agent and 10g plasticiser, with tumbling ball mill ball milling under 80rpm rotating speed, within 8 hours, mix, obtain the stable slurry of modest viscosity.
Slurry sieves and after vacuum defoamation processes through 190 eye mesh screens, be poured on PET counterdie, along with the drive of counterdie forward, after the scraper that is 0.3mm through knife up, obtain the biscuit of even thickness, curtain coating table top is heated to 50 ℃ simultaneously, when biscuit arrives curtain coating table top end along with PET counterdie is rolled-up together.
the preparation of sealing gasket
Biscuit is taken off from PET counterdie, by 6 laminin base lamination alignment, in both sides, respectively padded one deck PET film and corrosion resistant plate.Put into plastic packaging bag and vacuumize processing, object is air remaining between shielding layer.
Be placed under hot press and carry out hot pressing, wherein hot press pressure is 20MPa, and the dwell time is 10min, and temperature is 75 ℃.
After taking out, according to the concrete size of seal request, biscuit is carried out to cutting from plastic packaging bag, can obtain the sealing gasket of actual use.
sealing gasket heats up and shrinks test:
The sealing gaskets of embodiment 1 and 2 preparations of take are example, and sealing gasket is carried out to cutting according to the size of 2cm * 2cm, apply the pressure of 10kPa, are placed in Muffle furnace and heat up, and be warming up to 810 ℃ of insulation 40min, then naturally lower the temperature with the speed of 3 ℃/min.As shown in table 1, compare with the method for the thick sealing gasket biscuit of direct curtain coating, the sealing gasket of preparing for the method adopting after the present invention improves, the shrinkage in the intensification sealing-in stage is obviously reduced, and this is very favorable for sealing-in success rate.
The shrinkage ratio that table 1 distinct methods is prepared sealing gasket
the application of sealing gasket in pile
By the sealing gasket that adopts the method to prepare, the size needing according to sealing is carried out cutting, then with battery, receive each of the pile that electric material, connecting plate etc. are assembled into 3,5,10,15, Fig. 1 and Fig. 2 are respectively the pictures before and after 10 battery pile sealing-ins.Experiment finds that the pile sealing-in success rate of these different sizes has reached 100%, has ensured the successful sealing-in of all size pile.
Above specific embodiments of the invention be have been described in detail, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and alternative also all among category of the present invention.Therefore, equalization conversion and the modification done without departing from the spirit and scope of the invention, all should contain within the scope of the invention.
Claims (9)
1. prepare the method for sealing gasket for Solid Oxide Fuel Cell, it is characterized in that, described method comprises: step 1, by ball milling after encapsulant powder and A/B mixed solvent, dispersant, obtains slurry; Wherein, A is aromatic hydrocarbon solvent, and B is
represented ester, R1 and R2 are respectively independently selected from the alkyl of C1～C5;
Step 2, ball milling after slurry described in step 1 is mixed with binding agent and plasticiser;
Step 3, by gained slurry in step 2 through 60～200 eye mesh screens sieve, vacuum defoamation, be poured over and on PET counterdie, carry out curtain coating, and driven forward by PET counterdie, wherein in curtain coating process, slurry thickness is controlled at 0.1～0.3mm, curtain coating table top is heated to 45～85 ℃, removes PET counterdie and obtains biscuit;
Step 4, at least one deck biscuit stack alignment, carries out hot pressing, and wherein, hot pressing pressure is 10～50MPa, and temperature is 50～90 ℃, and the dwell time is 10～20min;
Step 5, carries out cutting by the biscuit after hot pressing according to the concrete size of seal request, and obtaining can the actual sealing gasket using;
Step 6, reclaims waste material unnecessary after cutting biscuit, mixes with A/B mixed solvent, with roller milling machine ball milling 2～12h under 20～100rpm rotating speed, obtains being recycled and reused for the stable slurry of curtain coating, repeats above-mentioned steps 3～step 5.
2. method according to claim 1, is characterized in that, A is any one or a few in benzene, alkyl benzene, halogeno-benzene.
3. method according to claim 1, is characterized in that, A/B mixed solvent is dimethylbenzene/butyl acetate.
4. method according to claim 1, is characterized in that, in the mixture of encapsulant powder and A/B mixed solvent, dispersant, A/B mixed solvent percentage by weight is 10～40wt%, and dispersant percentage by weight is 1～10wt%.
5. according to the method described in any one in claim 1～4, it is characterized in that, the mass ratio of A and B is 1: (0.5～2).
6. method according to claim 1, is characterized in that, in step 1 and/or 2, described ball milling is selected roller milling machine, and in mechanical milling process, rotating speed is 60～200rpm, and Ball-milling Time is 2～12h.
7. method according to claim 1, is characterized in that, in described slurry, binding agent, elasticizer mixture, weight of binder percentage is 1～10wt%, and plasticiser percentage by weight is 1～10wt%.
8. method according to claim 1, is characterized in that, in step 4, after described at least one laminin base stack, carries out vacuum treatment, to remove the air between each laminin base, then carries out hot pressing.
9. method according to claim 1, is characterized in that, in step 6, A/B mixed solvent accounts for the 10～50wt% that reclaims waste material and mixed solvent total weight.
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108110277A (en) * | 2016-11-25 | 2018-06-01 | 中国科学院大连化学物理研究所 | A kind of preparation method of solid oxide fuel cell seal pad |
| CN112225492B (en) * | 2020-10-15 | 2022-04-19 | 合肥市盛文信息技术有限公司 | Preparation method of solid oxide fuel cell sealing material |
| CN113224340B (en) * | 2021-04-29 | 2022-11-15 | 华能国际电力股份有限公司 | Molten carbonate fuel cell diaphragm and preparation method thereof |
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