CN105503232A - Preparation of wall-flow SiC honeycomb ceramic filter - Google Patents
Preparation of wall-flow SiC honeycomb ceramic filter Download PDFInfo
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- CN105503232A CN105503232A CN201510866313.XA CN201510866313A CN105503232A CN 105503232 A CN105503232 A CN 105503232A CN 201510866313 A CN201510866313 A CN 201510866313A CN 105503232 A CN105503232 A CN 105503232A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/0006—Honeycomb structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
- B01D46/0001—Making filtering elements
Abstract
Preparation of a wall-flow SiC honeycomb ceramic filter used for filtering particles in diesel vehicle smoke comprises the following step: preparation of plastic pug, wherein the pug comprises the following raw materials by mass: 80 to 90 parts of recrystallized SiC aggregate of which the particle diameters range from 10 to 20 [mu]m, 12 to 19 parts of a SiC sintering additive of which the particle diameters range from 10 to 50 [mu]m, 15 to 23 parts of a pore-forming agent of which the particle diameters range from 10 to 50 [mu]m, and 2 to 7 parts of a water-soluble organic binder, and is prepared according to the steps of mixing the micron-sized recrystallized SiC aggregate, sintering additive and pore-forming agent uniformly, adding the binder, a composite additive and water for kneading, and carrying out vacuum refining, aging and plasticizing; mold extrusion, microwave drying, crossed hole plugging and sintering: the plastic pug is extruded with a square mold of which the cross section is relatively small, the extruded material is cut to obtain cuboid wet green bodies, microwave drying, crossed hole plugging and drying are carried out in sequence, temperature rises in a programmed manner to 2100 to 2300 DEG C via heating in a subpressure gas and a protection gas in sequence, and sintering is carried out.
Description
Technical field
The present invention relates to a kind of filter plant, relate to for wall-flow type SiC ceramic honey comb trapping diesel vehicle flue gas particles and preparation method thereof, belong to porous ceramics trap and manufacture field.
Technical background
It is large that diesel engine has power, and the life-span is long, and dynamic performance is good, discharges low feature, is a development trend of automobile, particularly diesel oil car from now on.But the flue gas of emission of diesel engine contains more particulate matter, it is one of source of topsoil.It is " diesel particulate trap " (being called for short DPF) that current exhaust gas from diesel vehicle administers conventional method, especially adopts honeycomb ceramic filter as strainer.Its principle utilizes before and after the duct import of strainer and adjacent outlets to replace blocking technology, makes exhaust pass from wall and reach the object of filtering particle.Current trichroite is the most frequently used making material of DPF, but the shortcoming of product to be physical strength lower, resistance toheat and resistance to chemical corrosion are also poor, can not adapt to more and more higher emission standard requirement.In recent years, be that the DPF that material makes obtains and develops rapidly with SiC, its physical strength and use temperature, excellent resistance to chemical attack is far above trichroite DPF, and the gap structure of SiC has better adjustability, more high porosity and evenly the strainer of pore size distribution can be prepared, therefore just progressively replace the trichroite DPF of current widespread use.Relevant research and development situation is as follows:
CN101747078A discloses a kind of manufacture method of high purity silicon carbide honeycomb ceramic body using nanometer silicon carbide as sintering adjuvant, the feature of this invention is: (1) selects pure silicon carbide as porous ceramics aggregate, take nanometer silicon carbide as sintering aid, allocate as bonding agent and plastic forming agent and suitable quantity of water using methylcellulose gum and tung oil organism auxiliary agent; (2) extruding-out process is adopted to obtain the biscuit extruded, by regulating proportioning and the consumption of bonding agent and forming agent in organism auxiliary agent; (3) adopt the moisture in low power microwave heating eliminating biscuit body, then adopt oven drying to get rid of the remaining moisture of biscuit body, hocket therebetween; (4) employing conventional heating mode gets rid of the organism auxiliary component in biscuit; (5) sintering with pressure is adopted, by change micro-size particles mean sizes and select to have different mean sizes SiC powder product, change sintering of nano-material additive dosage, select different firing temperatures, realize the object regulating and change porous ceramic film material void content and average pore size and distribution thereof.
CN201310024015.7 discloses a kind of manufacture method of resistant to elevated temperatures silicon carbide soot filters, and the feature of this invention is: this preparation method comprises the following steps: (1) prepares 70 ~ 95 weight parts and median size is the talcum that silicon carbide, 13 ~ 18 weight parts and the median size of 20 μm ~ 30 μm is less than 10 μm; The silicon powder that kaolin, 0 ~ 5 weight part and median size that 0 ~ 10 weight part and median size are less than 2 μm are less than 5 μm; (2) first above-mentioned silicon carbide, talcum, kaolin, silicon powder are mixed into powder mixture, then add pore-forming material, binding agent, lubricant, water mediate plastify into pug, again mix; Powder mixture 100 weight part in this pug, pore-forming material 10 ~ 25 weight part, binding agent 3 ~ 6 weight part, lubricant 0.5 ~ 2 weight part, water 20 ~ 30 weight part; (3) above-mentioned pug is become pane green compact by extrusion moulding; (4) by after the drying of above-mentioned pane green compact through 1430 ~ 1450 DEG C of high-temperature calcinations, be incubated and form the rectangular base substrate of sintered silicon carbon after 6 ~ 10 hours, the ceramic fiber of preparation 10 ~ 25 weight parts, the colloided silica of 15 ~ 20 weight parts, the water of 10 ~ 20 weight parts are mixed into splicing agent, the rectangular base substrate of several sintered silicon carbons of 100 weight parts and splicing agent bonds and forms ceramic honey comb, and be less than 1000 DEG C temperature sinter acquisition silicon carbide carbon smoke particle trap.
CN200910155765 discloses a kind of manufacturing process of wall-flow type honeycomb ceramic carrier, and the feature of this invention is: the manufacturing process relating to a kind of wall flow type honeycomb ceramic carrier blank for traps diesel exhaust micro particle.Mix pure silicon carbide and methylcellulose gum mixed powder thoroughly, be that methylcellulose gum is poured into after inside stirrer and stirred by pure silicon carbide and weight, silicon carbide powder and methylcellulose powder can be mixed; To pour into while stirring inside stirrer after the flour aqueous solution of flour and water mixing is mixed thoroughly and pug is fully mixed thoroughly; In the pug mixed, add tung oil and stirred for several minute, make pug have stickiness, easily be bonded together and be put into by pug in a container and load, seal it off, guarantee that the moisture in pug can not evaporate, old 1 day; Then dry with microwave oven after mud refining, extrusion molding, last plug-hole dried, dry, fire and get final product.
CN200610106784 discloses a kind of sintering method of wall-flow type honeycomb ceramic carrier; this invention is mainly used in the trapping of diesel engine vent gas particulate; wall flow type honeycomb ceramic carrier blank is put into stove; vacuumize; be incubated after kiln temperature is increased to set(ting)value, insulation after being filled with protective gas sintering in stove, continuation raise furnace temperature and sinter to set(ting)value, are then incubated; continue to raise furnace temperature to set(ting)value, be incubated, lower the temperature, come out of the stove.Advantage: one is that stove intensification combines with insulation, not only guarantees the sinter molding quality of green honeycomb body, and ensure that the ceramics strength after blank sintering; Two is that stove adopts protective gas protection sintering technology; both the melt temperature needed for silicon carbide recrystallization had been met; silicon carbide recrystallization can be made again to be incubated in the molten state, to smelt, and final formation has the recrystallized silicon carbide ceramic honeycomb trap of high strength.
Physical strength, the porosity of current domestic SiC honeycomb ceramic filter DPF also have larger gap with pore size distribution compared with same kind of products at abroad, still have necessity of improvement.
Summary of the invention
The object of the invention is: be mostly cordierite for current exhaust gas from diesel vehicle particulate filter, the defect of its physical strength, high temperature resistant and poor corrosion resistance, the present invention adopts recrystallization SiC to be aggregate and corresponding preparation technology, be intended to manufacture that a kind of physical strength is good, high temperature resistant, anticorrosive, porosity is high, micropore is even and the wall-flow honeycomb ceramic filter that distribution good, soot filterability is high, to adapt to the requirement that exhaust gas from diesel vehicle discharges more strict standard.
The object of the present invention is achieved like this: the step preparing wall-flow type SiC honeycomb ceramic filtering bodies is as follows:
(1) plastic mud material is prepared
Raw material forms: particle diameter is recrystallization SiC aggregate 80 ~ 90 parts of (mass fractions of 10 ~ 20 μm, lower same), particle diameter is the SiC sintering aid 12 ~ 19 parts of 10 ~ 50nm, particle diameter is that (pore-forming material used is polymethylmethacrylate for the pore-forming material 15 ~ 23 parts of 10 ~ 50 μm, or acrylic acid esters co-polymer, or micronized polystyrene, or powdered carbon etc.), soluble organic adhesive is 2 ~ 7 parts, and (water-soluble binder is conventional Walocel MT 20.000PV, or Natvosol, or Vltra tears, or polyvinyl alcohol etc.); After raw material Homogeneous phase mixing, add Water Soluble Compound additive 9 ~ 15 parts (composite additive is two kinds of combinations in the materials such as polyoxyethylene glycol, stearic acid, glycerine, tung oil and ethanol, and the mass ratio of two kinds of materials is 1:1) and 21 ~ 26 parts, water; Mediate, system 2 ~ 3 times (vacuum tightness is below 90KPa) is practiced in vacuum outgas, and old 24 ± 8h, plastifies into plastic mud material.
(2) mould extrude, microwave drying, intersection plug-hole (namely intersect shutoff honeycomb hole) and burn till
Extruded after plastic mud material by honeycomb die by extrusion machine, mould (self-control) sectional dimension adopted is the square of 30 ~ 40mm × 30 ~ 40mm, honeycomb die hole density is 100 ~ 300 holes/square inch, pug cuts into the wet base substrate of certain length after extruding, obtain dry body body after 8 ~ 12Kw microwave drying;
Again to dry body body intersection plug-hole.First use film applying on the cross section at dry body body two ends, the outlet in ceramic honey comb duct is closed.Then submit fork hole at the cross section film at two ends respectively with laser beam drilling device, the one end in same duct is got through, and the other end is still closed, mutual not conducting between Kong Yukong.Then be laid on the cross section at base substrate two ends by the plastic mud material (not adding the composition of pore-forming material) of claim 1, thickness is 5 ~ 9mm.Be pressed in perforate with extrusion machine by pug again, hole blocking layer thickness is 3 ~ 7mm, microwave drying;
Then dry body body is placed in kiln kiln roasting.First vacuumize and make vacuum tightness 50 ~ 90KPa, be warming up to 1000 DEG C with 10 ~ 20 DEG C/min simultaneously, then be warming up to 1700 DEG C with 5 ~ 10 DEG C/min.Stopping vacuumizes, with 2 ~ 6cm
3/ min speed is filled with rare gas element or nitrogen in stove, and is warming up to 2100 ~ 2300 DEG C with 2 ~ 5 DEG C/min, and insulation 3 ~ 6h, then naturally cools to less than 100 DEG C, closes protection gas, kiln discharge.
(3) cross section is the shaping and roasting of square or rectangle SiC honeycomb ceramic strainer
Be that the little rectangular base substrate that 30 ~ 40mm × 30 ~ 40mm sinters is bonded to the larger base substrate of volume by 9 ~ 25 sectional areas, its sectional dimension is square or the rectangle of 100 ~ 250mm × 100 ~ 250mm.Binding agent used is mixed by ceramic fiber 5 ~ 10 parts, colloided silica 25 ~ 35 parts, 10 ~ 15 parts, water, and during bonding, the thickness of binding agent is 1 ~ 3mm, microwave drying after base substrate placement 8 ~ 10h after bonding.Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 1 ~ 4h, naturally cools to less than 100 DEG C, obtains the product needed.
(4) cross section is the shaping and roasting of circle, oval and special-shaped SiC honeycomb ceramic strainer
As mentioned above, be that the rectangular base substrate of 30 ~ 40mm × 30 ~ 40mm sintering is bonded to the larger base substrate of volume by 9 ~ 25 sectional areas, its sectional dimension is square or the rectangle of 100 ~ 250mm × 100 ~ 250mm.Cut with lathe car limit after placing 8 ~ 10h, its circular diameter is 100 ~ 250mm, and oval semi-major axis is 15 ~ 25mm, minor semi-axis 8 ~ 20mm, and guarantees that roundness deviation is less than 0.5mm.Then the outer wall of car limit base substrate is made skin graft, namely first one deck binder liquid is applied at base substrate outer wall, then described subsides mechanically closely, equably containing the plastic mud material of pore-forming material be loaded on base substrate outer wall, making to bear layer thickness is 1 ~ 2.5mm, and base substrate is microwave drying again.Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 1 ~ 4h, naturally cooling, obtains the product needed.
Beneficial effect of the present invention: adopt honeycomb ceramic filter as crossing flue gas particle filter, its exhaust is passed from wall, and therefore removal efficiency is high, and settling easily processes; Honeycomb ceramic filter is aggregate with micron order recrystallization SiC, is successively vacuumizing and temperature programming high temperature sintering under nitrogen protection with nano grade Sic sintering aid, ensure that the tool intensity of product is good, high temperature resistant and corrosion resistant characteristic; The skin-grafting of dry body body adopted and deburring can guarantee the roundness of base substrate, simultaneously outer wall materials due to do not strengthen containing pore-forming material filtering bodies intensity, also can prevent from filtering time particulate matter reveal; Product is not directly be crushed to integral honeycomb formula structure, but first makes small rectangular block, then with there being certain elastic ceramic fiber to be bonded to entirety (as shown in Figure 1), this partition type structure can significantly improve the thermal-shock resistance of product.After measured, its ultimate compression strength is greater than 50MPa to obtained wall-flow type SiC honeycomb ceramic sample, and porosity is 53% ~ 58%, and micropore mean pore size is 11 ~ 13 μm, and in flue gas, the clearance of particulate matter is greater than 95%, and thermal expansivity is less than 1.5 × 10
-6/ DEG C (room temperature ~ 800 DEG C), heat-shock resistance is greater than 500 DEG C.
Accompanying drawing explanation
Fig. 1 is used for the photo (cross section is circle) of the SiC honeycomb ceramic that diesel vehicle flue gas particles filters, Φ 143.8mm × 152.4mm.
Embodiment
Embodiment comprises: proportioning raw materials and process, small rectangular block blank forming, drying, intersection plug-hole and burn till, and small rectangular block base substrate bonding, shape process and roasting, physicochemical property detects.
Proportioning raw materials and process: recrystallization SiC major ingredient 80 ~ 90 parts of (mass fractions by particle diameter being first 10 ~ 20 μm, lower with), particle diameter is the SiC sintering aid 12 ~ 19 parts of 10 ~ 50nm, particle diameter is that (pore-forming material comprises polymethylmethacrylate for the pore-forming material 15 ~ 23 parts of 10 ~ 50 μm, or acrylic acid esters co-polymer, or micronized polystyrene, or powdered carbon etc.), water-soluble binder 2 ~ 7 parts (comprises Walocel MT 20.000PV, or Natvosol, or Vltra tears, or polyvinyl alcohol etc.).After raw material Homogeneous phase mixing, add Water Soluble Compound additive 9 ~ 15 parts (comprising more than two kinds of the materials such as polyoxyethylene glycol, stearic acid, glycerine, tung oil and ethanol), 21 ~ 26 parts, water.Mediate, system 2 ~ 3 times (vacuum tightness is below 90KPa) is practiced in vacuum outgas, and old 24 ± 8h, plastifies into plastic mud material again.。
Small rectangular block blank forming, drying, intersection plug-hole and burn till: the honeycomb die (self-control) of plastic mud material by extrusion machine extruded, mold sections is the square of 30 ~ 40mm × 30 ~ 40mm, and hole density is 100 ~ 300 holes/square inch.Pug cuts into the wet base substrate of certain length after extruding, to dry body body intersection plug-hole, again microwave drying after 8 ~ 12Kw microwave drying.Then dry body body is placed in kiln, vacuumizes and make vacuum tightness 50 ~ 90KPa, be warming up to 1000 DEG C with 10 ~ 20 DEG C/min simultaneously, then be warming up to 1700 DEG C with 5 ~ 10 DEG C/min.Stopping vacuumizes, with 2 ~ 6cm
3/ min speed is filled with rare gas element or nitrogen in stove, and is warming up to 2100 ~ 2300 DEG C with 2 ~ 5 DEG C/min, and insulation 3 ~ 6h, then naturally cools to less than 100 DEG C, closes protection gas, kiln discharge.
Small rectangular block base substrate bonding, shape process and roasting: the SiC honeycomb ceramic strainer that cross section is square, rectangle as prepared, as long as be that the little rectangular base substrate that 30 ~ 40mm × 30 ~ 40mm square sinters is bonded to the larger base substrate of volume by 9 ~ 25 sectional areas, its sectional dimension is square or the rectangle of 100 ~ 250mm × 100 ~ 250mm.Binding agent used is by ceramic fiber 5 ~ 10 parts of (mass fractions, down together), colloided silica 25 ~ 35 parts, 10 ~ 15 parts, water mix, and at 800 ~ 1000 DEG C of aging 8h, during bonding, the thickness of binding agent is 1 ~ 3mm, microwave drying after base substrate placement 8 ~ 10h after bonding.Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 2h, naturally cools to less than 100 DEG C, obtains the product needed.
Be circle, oval and special-shaped SiC honeycomb ceramic strainer as cross section will be prepared, will be first that the rectangular base substrate that 30 ~ 40mm × 30 ~ 40mm sinters is bonded to the larger base substrate of volume by part sectional area, its sectional dimension be square or the rectangle of 100 ~ 250mm × 100 ~ 250mm.Then with the cutting of lathe car limit, its circular diameter is 100 ~ 250mm, and oval semi-major axis is 15 ~ 25mm, minor semi-axis 8 ~ 20mm, and guarantees that roundness deviation is less than 0.5mm.The outer wall of car limit base substrate is made skin graft, namely first one deck binder liquid is applied at base substrate outer wall, above-mentioned subsides mechanically closely, equably containing the plastic mud material of pore-forming material be loaded on base substrate outer wall, making to bear layer thickness is 1 ~ 2.5mm, and base substrate is microwave drying again again.Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 2h, naturally cools to less than 100 DEG C, obtains the product needed.
Physicochemical property detects: ultimate compression strength adopts YA-300 type electric-liquid type pressure testing machine to measure, and aperture and porosity adopt mercury penetration method to measure; Efficiency of dust collection test performs with reference to standard GB/T/T13931-2002 " electric precipitator performance testing method "; Thermal expansivity adopts NETZSCH ⊕ D11-402PC type thermal expansivity detector to measure, and heat shock resistance utilizes retort furnace to measure, sample appearance size, wall thickness vernier caliper measurement.
Embodiment 1 cross section is the preparation of square wall-flow type SiC honeycomb ceramic filtering bodies, obtained 40, sample, and the parameter that making method and sample record is as follows:
Proportioning raw materials and process: the recrystallization SiC major ingredient 85 parts of (mass fractions by particle diameter being first 15 μm, lower with), after the particle diameter SiC sintering aid 15 parts that is 30nm, the particle diameter raw material Homogeneous phase mixing such as pore-forming material polymethylmethacrylate 2 parts, water-soluble binder Vltra tears 5 parts that is 30 μm, add the polyoxyethylene glycol as Water Soluble Compound additive and tung oil (1:1) 12 parts, 24 parts, water, mediate in kneader again, then degassed experienced system 3 times under vacuum tightness is 92KPa, old 24h, obtains plastification pug.
Small rectangular block blank forming and drying: the mould (self-control) of plastic mud material by extrusion machine is extruded, the cross section of mould is the square of 36mm × 36mm, hole density is 300 holes/square inch, pug cuts into length after extruding be that the small rectangular block of 155mm wets base substrate, obtains dry body body after 10Kw microwave drying.
Small rectangular block base substrate intersection plug-hole and drying: with film applying on the cross section at dry body body two ends, then (namely the neighbours in a hole all close to submit fork hole at the cross section film at two ends respectively with laser beam drilling device, the structure that one neighbours closed all open, other end therewith end face perforate mode is similar, but one end perforate in same duct, the other end is closed), the one end in same duct is got through, the other end is closed, then be not laid on the cross section at base substrate two ends containing the plastic mud material layer of pore-forming material with above-mentioned, thickness 5mm, with extrusion machine, pug is pressed in perforate again, strike off, hole blocking layer thickness is about 4mm, microwave drying.
Small rectangular block base substrate burns till: dry body body is placed in kiln, vacuumizes and make vacuum tightness 90KPa, is warming up to 1000 DEG C simultaneously, then is warming up to 1700 DEG C with 5 DEG C/min with 15 DEG C/min.Stopping vacuumizes, with 4cm
3/ min speed is filled with nitrogen in stove, and is warming up to 2150 DEG C with 3 DEG C/min, and insulation 4h, then naturally cools to less than 100 DEG C, closes protection gas, kiln discharge.
Small rectangular block base substrate bonding and roasting: the small rectangular block base substrate bonding that above-mentioned 16 are burnt till, obtaining sectional dimension is 144mm × 144mm, the high base substrate for 153mm, binding agent used is mixed by ceramic fiber 8 parts, colloided silica 30, water 13, during bonding, the thickness of binding agent is 2mm, microwave drying after base substrate placement 8h after bonding.Finally be placed in roasting at kiln 900 DEG C, 2h is held in insulation, naturally cools to less than 100 DEG C, obtains product.
Product performance detect: sample in cross section size 144mm × 144mm, high 153mm, ultimate compression strength 55MPa, porosity is 53%, and micropore mean pore size is 12 μm, the clearance 98% of particulate matter in flue gas, thermal expansivity (room temperature ~ 800 DEG C) 1.5 × 10
-6/ DEG C, heat shock resistance 500 DEG C.
Result shows: the product performance that the present invention obtains are all more excellent.
Embodiment 2 cross section is the preparation of circle wall-flow type SiC matter honeycomb pottery filtering bodies, obtained 40, sample, and the parameter that making method and sample record is as follows:
Raw materials proportioning and process, small rectangular block blank forming and drying, small rectangular block base substrate intersect plug-hole and drying, small rectangular block base substrate burn till and the operation steps such as bonding is all same as embodiment 1, bonding being obtained sectional dimension is that 144mm × 144mm, height are for cutting on the base substrate lathe car limit of 153mm again, its circular diameter is 144mm, and guarantees that roundness deviation is less than 0.5mm.Then the outer wall of car limit base substrate is made skin graft, namely first one deck binder liquid is applied at base substrate outer wall, above-mentioned subsides mechanically closely, equably containing the plastic mud material of pore-forming material be loaded on base substrate outer wall, making to bear layer thickness is 1.5mm, and base substrate is microwave drying again again.Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 2h, naturally cools to less than 100 DEG C, obtain product.
Product performance detect: sample in cross section diameter of phi is 143.8mm, high 152.4mm, the cross section that other number of times is all same as embodiment 1 as the clearance of particulate matter in ultimate compression strength, porosity, micropore mean pore size, flue gas, the index such as thermal expansivity and heat shock resistance is square SiC matter wall-flow honeycomb ceramic filter.
Result shows: the face shaping (cross section is circle or square) of SiC matter wall-flow honeycomb pottery filtering bodies does not affect its location parameter.
Embodiment 3 feed change composition and calcining system, preparation cross section is square wall-flow type SiC honeycomb ceramic filtering bodies, obtained 40, sample, and the parameter that making method and sample record is as follows:
Proportioning raw materials and process: the pure SiC major ingredient 85 parts of (mass fractions by particle diameter being first 30 μm, lower with), particle diameter be 30 μm (close particle diameter also can, indistinction) the raw material Homogeneous phase mixing such as pore-forming material polymethylmethacrylate 2 parts, water-soluble binder Vltra tears 5 parts after, add the polyoxyethylene glycol as Water Soluble Compound additive and tung oil (1:1) 12 parts, 24 parts, water, mediate in kneader again, then degassed experienced system 3 times under vacuum tightness is 92KPa, old 24h, obtains plastification pug.
Small rectangular block blank forming and drying, small rectangular block base substrate intersection plug-hole and drying: operation steps is with embodiment 1.
Small rectangular block base substrate burns till: dry body body is placed in kiln, is warming up to 1000 DEG C at ambient pressure with 15 DEG C/min, then is warming up to 1450 DEG C with 5 DEG C/min, and insulation 4h, then naturally cools to less than 100 DEG C, obtain product.
Small rectangular block base substrate bonding and roasting: operation steps is with embodiment 1.
Product performance detect: sample in cross section size 144mm × 144mm, high 153mm, ultimate compression strength 17MPa, porosity is 48%, and micropore mean pore size is 14 μm, the clearance 90% of particulate matter in flue gas, thermal expansivity (room temperature ~ 800 DEG C) 1.5 × 10
-6/ DEG C, heat shock resistance 450 DEG C.
Result shows: the reduction of the reduction of SiC raw materials quality and product firing temperature, makes the ultimate compression strength of product and thermal shock resistance all have and decline in various degree.
Embodiment 4 adopts plastic mud material monolithic extruded shaping, but not small rectangular block splicing, preparation cross section is square wall-flow type SiC matter honeycomb ceramic filter, obtained 40, sample, and the parameter that making method and sample record is as follows:
Proportioning raw materials and process: operate same embodiment 1.
Blank forming and drying: the mould (self-control) of plastic mud material by extrusion machine is extruded, the cross section of mould is the square of 144mm × 144mm, hole density is 300 holes/square inch, pug cuts into length after extruding be that the small rectangular block of 155mm wets base substrate, obtains dry body body after 10Kw microwave drying.
Dry body body burns till: dry body body is placed in kiln, vacuumizes and make vacuum tightness 90KPa, is warming up to 1000 DEG C simultaneously, then is warming up to 1700 DEG C with 5 DEG C/min with 15 DEG C/min; Stopping vacuumizes, with 4cm
3/ min speed is filled with nitrogen in stove, and is warming up to 2150 DEG C with 3 DEG C/min, and insulation 4h, then naturally cools to less than 100 DEG C, closes protection gas, obtains product.
Product performance detect: sample in cross section size 144mm × 144mm, high 153mm, ultimate compression strength 50MPa, porosity is 53%, and micropore mean pore size is 12 μm, the clearance 98% of particulate matter in flue gas, thermal expansivity (room temperature ~ 800 DEG C) 1.5 × 10
-6/ DEG C, heat shock resistance 400 DEG C.
Result shows: adopt the monolithic extruded shaping but not small rectangular block splicing of plastic mud material, and the thermal shock resistance of obtained SiC matter wall-flow honeycomb pottery filtering bodies has and significantly declines, and some other indexs reduce also has reduction.
The above is only the preferred embodiment of the present invention; be noted that for those skilled in the art; under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (7)
1. a preparation for wall-flow type SiC honeycomb ceramic filtering bodies, its characterization step is as follows:
Prepare plastic mud material: pug raw materials quality number consists of 80 ~ 90 parts, the recrystallization SiC aggregate that particle diameter is 10 ~ 20 μm, particle diameter is the SiC sintering aid 12 ~ 19 parts of 10 ~ 50nm, particle diameter is the pore-forming material 15 ~ 23 parts of 10 ~ 50 μm, and soluble organic adhesive is 2 ~ 7 parts; After raw material Homogeneous phase mixing, add Water Soluble Compound additive 9 ~ 15 parts and 21 ~ 26 parts, water, mediate, vacuum tightness is that the vacuum outgas of more than 90KPa practices system 2 ~ 3 times, and old 24 ± 8h, plastifies into plastic mud material;
Mould is extruded, microwave drying, intersection plug-hole and burn till: extruded after plastic mud material by honeycomb die by extrusion machine, the hole density of mould is 100 ~ 300 holes/square inch, and pug cuts into the wet base substrate of certain length after extruding; Dry body body is obtained, again through 8 ~ 12Kw microwave drying after making the one end open one end in same duct close to dry body body intersection plug-hole after 8 ~ 12Kw microwave drying; Then dry body body is placed in kiln, vacuumizes and make vacuum tightness 50 ~ 90KPa, be warming up to 1000 DEG C with 10 ~ 20 DEG C/min simultaneously, then be warming up to 1700 DEG C with 5 ~ 10 DEG C/min; Stopping vacuumizes, with 2 ~ 6cm
3/ min speed is filled with rare gas element or nitrogen as protection gas in stove, and is warming up to 2100 ~ 2300 DEG C with 2 ~ 5 DEG C/min, and insulation 3 ~ 6h, then naturally cools to less than 100 DEG C, closes protection gas, kiln discharge.
2. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to claim 1, it is characterized in that cross section is the shaping and roasting of square or rectangle SiC honeycomb ceramic strainer: be that the little rectangular base substrate that 30 ~ 40mm × 30 ~ 40mm sinters is bonded to bulky base substrate by 9 ~ 25 sectional areas, the sectional dimension of large base substrate is square or the rectangle of 100 ~ 250mm × 100 ~ 250mm; The binding agent used that bonds is mixed by ceramic fiber 5 ~ 10 mass parts, colloided silica 25 ~ 35 mass parts, water 10 ~ 15 mass parts, and during bonding, the thickness of binding agent is 1 ~ 3mm, microwave drying after base substrate placement 8 ~ 10h after bonding; Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 1 ~ 4h, naturally cooling.
3. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to claim 1, it is characterized in that cross section is circle, the shaping and roasting of oval or special-shaped SiC honeycomb ceramic strainer: be that the rectangular base substrate that 30 ~ 40mm × 30 ~ 40mm sinters is bonded to bulky base substrate by 9 ~ 25 sectional areas, its sectional dimension is square or the rectangle of 100 ~ 250mm × 100 ~ 250mm; Cut with lathe car limit after placing 8 ~ 10h, its circular diameter is 100 ~ 250mm, and oval semi-major axis is 15 ~ 25mm, minor semi-axis 8 ~ 20mm, and guarantees that roundness deviation is less than 0.5mm; Then the outer wall of car limit base substrate is made skin graft, namely first one deck binder liquid is applied at base substrate outer wall, then described subsides mechanically closely, equably containing the plastic mud material of pore-forming material be loaded on base substrate outer wall, making to bear layer thickness is 1 ~ 2.5mm, and base substrate is microwave drying again; Finally be placed in kiln kiln roasting, temperature is 800 ~ 1000 DEG C, keeps 1 ~ 4h, naturally cooling.
4. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to Claims 2 or 3, it is characterized in that the mold sections adopted is of a size of the square of 30 ~ 40mm × 30 ~ 40mm, hole density is 100 ~ 300 holes/square inch, pug cuts into the wet base substrate of certain length after extruding, again through 8 ~ 12Kw microwave drying, obtain dried rectangular base substrate.
5. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to Claims 2 or 3, is characterized in that pore-forming material used is polymethylmethacrylate, or acrylic acid esters co-polymer, or micronized polystyrene, or powdered carbon etc.; Water-soluble binder is conventional Walocel MT 20.000PV, or Natvosol, or Vltra tears or polyvinyl alcohol.
6. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to Claims 2 or 3, it is characterized in that composite additive is the combination of two kinds of materials in the materials such as polyoxyethylene glycol, stearic acid, glycerine, tung oil and ethanol, the mass ratio of two kinds of materials is 1:1.
7. the preparation of wall-flow type SiC honeycomb ceramic filtering bodies according to Claims 2 or 3, is characterized in that the rectangular base substrate after by microwave drying carries out intersecting plug-hole: first use film applying on the cross section at dry body body two ends, and the outlet in ceramic honey comb duct is closed; Then submit fork hole at the cross section film at two ends respectively with laser beam drilling device, the one end in same duct is got through, and the other end is still closed, mutual not conducting between Kong Yukong; Then be laid on the cross section at base substrate two ends by the composition plastic mud material not adding pore-forming material, tiling plastic mud material thickness is 5 ~ 9mm; Be pressed in perforate with extrusion machine by pug again, hole blocking layer thickness is 3 ~ 7mm, microwave drying.
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