CN1966130A - Film built-in type inorganic film tube and its preparation method - Google Patents
Film built-in type inorganic film tube and its preparation method Download PDFInfo
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- CN1966130A CN1966130A CN 200610037301 CN200610037301A CN1966130A CN 1966130 A CN1966130 A CN 1966130A CN 200610037301 CN200610037301 CN 200610037301 CN 200610037301 A CN200610037301 A CN 200610037301A CN 1966130 A CN1966130 A CN 1966130A
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Abstract
The invention relates to a method that arranges inorganic membrane tube in the membrane, wherein it comprises inner and outer supports, and control membrane layer; said container membrane layer is between the inner and outer supports; and the production of inorganic membrane tube comprises that preparing inorganic powder, suspension, disperser and carrier into two kinds of slurries; then eccentrically shaping them for two or three times. The inventive inorganic membrane tube can effectively control the integrity of control membrane layer, to confirm the separate accuracy of inorganic membrane and avoid the stopped pollutant to contact the separated liquid, to reduce the secondary pollution.
Description
Technical field
The present invention relates to a kind of inoranic membrane, particularly a kind of film built-in type inorganic film tube.The invention still further relates to the preparation method of described film built-in type inorganic film tube.
Background technology
Inoranic membrane has been because of its good high temperature resistant, corrosion-resistant, biologically inert, characteristics such as capable of washing have been widely used in fields such as machinery, electronics, chemistry, medical and health, biology, food, environmental protection, is used for separation, clarification, degerming of fluid etc.
The separating property of inoranic membrane depends on the structure of inoranic membrane and separation parameter such as fenestra size and pore-size distribution, membrane porosity, thickness, membrane flux, membrane resistance, film-strength etc.Fenestra size and pore-size distribution have directly determined the membrane separating effect and the application of the separating of inoranic membrane, clarification, degerming etc.Suitable membrane flux (unit interval unit are fluid is by the amount of film) can guarantee the practicality of film.And film strength has determined inoranic membrane structural stability and service life in actual use.
Interact, restrict between the said structure of inoranic membrane and the separation parameter.The separation of the inoranic membrane little as the aperture, that pore size distribution is narrow, clarification, bacteria-eliminating efficacy are good, but along with the narrowing down of the reducing of membrane aperture, pore size distribution, fluid will increase by the resistance of inoranic membrane, and the flux of film will reduce.At this moment reduce thickness, improve membrane porosity and can reduce membrane resistance, improve membrane flux, but along with thickness reduces, membrane porosity increases, inorganic film strength will decrease, and be unfavorable for the application of film.The inoranic membrane of function admirable should be to have good membrane separating effect, high film-strength and big membrane flux.The aperture is big, pore size distribution is wide, and membrane resistance is little, and membrane flux can increase, but membrane separating effect can weaken.The porosity of film is big, and membrane resistance is also little, and membrane flux can increase, but film strength can be poor.Thickness increases, and film-strength will increase, but membrane resistance can increase.Can this shows that membrane separating effect, film-strength and membrane flux influence each other and restrict, can be described as conflicting.The inoranic membrane of function admirable should be under the prerequisite that guarantees good membrane separating effect, makes film have big as far as possible flux and high film-strength.How membrane aperture and pore-size distribution, membrane porosity, film thickness organically being united in the process of inoranic membrane preparation, reach optimized coupling, is the difficult point and the key of inoranic membrane preparation.
In order to solve above-mentioned film preparation difficult point, there have been many research workers to do many work in this respect, the structure of film is also developed by the direction of initial symmetrical structure to dissymmetrical structure, gradient-structure.Because the inoranic membrane of symmetrical structure is in the membrane aperture unanimity of whole film thickness direction, if assurance membrane separating effect, just need select for use the base-material of fine particle to prepare the film of little membrane aperture, this must cause enlarging markedly of membrane resistance, membrane flux is reduced, though can reduce membrane resistance by the attenuate thickness, but will sacrifice film strength, influence the actual serviceability of film, so the inoranic membrane of symmetrical structure can't satisfy good membrane separating effect, the whole requirement of high film-strength and big membrane flux just is used for coarse filtration or this simple symmetrical structure of pre-filtered porous filter elements employing at some.
What be applied at present that the inoranic membrane of the separation, clarification, degerming etc. of field fluids such as machinery, electronics, chemistry, medical and health, biology, food, environmental protection adopts all is the asymmetric or gradient-structure of multilayer, is made up of supporter, key-course and intermediate layer.The porous layer of large aperture, number millimeters thick has certain mechanical strength as supporter, guarantees the suitable mechanical intensity of inoranic membrane.The control rete of very little, the very thin thickness in load aperture on supporter guarantees the separation accuracy of inoranic membrane.In order to improve the load effect of control rete on supporter, before the control rete is carried on carrier, earlier the aperture is littler but than the intermediate layer of big one or more layers in control rete hole, the multilayer dissymmetrical structure of this inoranic membrane can effectively solve the contradiction between membrane separating effect, film-strength and the membrane flux than supporting body opening in load on the supporter.But the asymmetric inoranic membrane of multilayer key-course or transition zone in the preparation all is on the body attached to preceding one deck macropore, because the powder granule diameter suddenlys change, following one deck powder granule will certainly stop up a part of last layer macropore, like this, will reduce the ability that sees through of inoranic membrane greatly.On the other hand, because multilayer dissymmetrical structure inoranic membrane is not one-shot forming, need repeatedly moulding and sintering process between layer and layer.At first need to prepare supporter, could descend the coating and the sintering of one deck after often needing to burn till again, the supporter behind the sintering generally can not shrink again, because the general contraction of ceramic material when sintering is all bigger, and the shrinkage factor with a last supporter of following one deck of new coating is different, so, between layer and the layer is exactly a place that is easy to generate defective most at the interface, is easy to produce peel off and shrink the crackle that causes and other defective.Influence the quality of inoranic membrane, especially long-term stability in use.
In order to address these problems, patent of invention " gradient ceramic-film tube and preparation method thereof " (ZL00117221.2) uses the method for centrifugal forming with the radially descending shaping gradually of the powder granule in the slurry, maximum particle has formed the outer surface of film pipe in the slurry, minimum particle then concentrates on the endosexine of ceramic-film tube, form the equally distributed control rete in aperture, prepared radially continually varying gradient inorganic film tube of aperture.But this forming method can only form the control rete at the inner surface of film pipe, only when advancing in by pipe, fluid just manifests its advantage, if fluid advances outside managing, the large aperture of outer tube wall, make the pollutant in the fluid enter the duct easily, cause film to stop up, easy cleaning not, at this moment the control rete of inner tubal wall is preventing that the effect aspect the film pollution such as fenestra obstruction is just not obvious.
Patent of invention " Bicontrol film layer inorganic film pipe and preparation method thereof (CN 200510033632.9) " utilizes the method for twice continuous centrifugal moulding to prepare the Bicontrol film layer inorganic film pipe that has the control rete at inside and outside tube wall simultaneously, no matter this inoranic membrane is that fluid is by advancing in the pipe or outside the pipe, can both prevent effectively that pollutant from entering in the fenestra, pollutant can only be at the surface deposition of controlling diaphragm, be easy to clean, with the usability of film is improved greatly, good use value is arranged.But this Bicontrol film layer inorganic film reduces the flux of film because the existence of dual controlling diaphragm can increase the resistance of film.And in the use of inoranic membrane, carrying out along with the film separating and filtering, have the surface that increasing pollutant is deposited on controlling diaphragm, adopt simple flushing, backwash or machinery to clean no matter be, because these controlling diaphragm layer thicknesses very thin (general＜30 microns) are along with the number of times that cleans increases, these control retes all can have damage in various degree, in case damaging appears in these control retes, will influence the separating effect of inoranic membrane to some extent.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of film built-in type inorganic film tube is provided, the control rete is built in arbitrary position of film pipe on demand, effectively prevent or slow down the damage of cleaning, reduce membrane resistance simultaneously, improve membrane flux the control rete.
The present invention also aims to provide the preparation method of described film built-in type inorganic film tube.
Film built-in type inorganic film tube of the present invention, film pipe porosity is 20～85%, diameter 5～300mm, length 10～2000mm, wall thickness is 2～15mm, is made of inner supporting body, outer support and control rete, and described control rete is between inner supporting body and outer support.
The preparation method of a kind of film built-in type inorganic film tube of the present invention comprises the steps:
(1) configuration composite mortar: with particle diameter is inorganic powder, suspending agent, dispersant and the bearer configuration form slurry A of 0.1-20 μ m, is inorganic powder, suspending agent, dispersant and the bearer configuration form slurry B of 5-30 μ m with particle diameter;
(2) twice centrifugal forming: slurry A is injected pipe die carry out centrifugal forming formation outer support and control rete, then slurry B is injected this pipe die, carry out centrifugal forming, slurry B forms inner supporting body on the control rete that slurry A forms, obtain green compact through twice centrifugal forming, carrier is sloughed in its separation, and oven dry, the demoulding, sintering can make the built-in inorganic film tube of film of the present invention.
Among the described slurry A of step (1) among the parts by weight of each component and the slurry B parts by weight of each component as follows:
Inorganic powder 30-59.9;
Carrier 69.9-40;
Suspending agent 0-0.5;
Dispersant 0-0.5;
Wherein: suspending agent and dispersant are not zero simultaneously, and each composition weight umber sum is 100;
Described inorganic powder is powder Al
2O
3, TiO
2, SiO
2, ZrO
2, one or more mixtures among the SiC, diatomite, perlite, nickel, titanium, stainless steel, bronze, copper, iron;
Described carrier is a water;
Described suspending agent and dispersant are a kind of in carboxymethyl cellulose, polyvinyl alcohol, gum arabic, polyethylene glycol, the polyacrylamide.
In the step (2), sintering temperature is 700～1850 ℃, for the first time centrifugal forming makes the largest particles among the slurry A at first attached to the moulding of pipe die inwall, increase with molding time, inorganic powder in the slurry is radially descending gradually to the poly-partially moulding of pipe die inwall, smallest particles in this slurry is finally at the inboard control rete that forms of outer support, centrifugal forming makes the bulky grain adjacent controlling diaphragm strata under centrifugal action among the slurry B amass moulding for the second time, at the certain thickness wide-aperture inner supporting body of the inboard formation of control rete.The gained film built-in type inorganic film tube, its aperture, controlling diaphragm tunic hole is 0.1 μ m～5 μ m, film pipe porosity is 20～85%, diameter 5～300mm, length 10～2000mm, wall thickness are 2～15mm.
Film built-in type inorganic film tube of the present invention can also adopt following method to prepare, and comprises the steps
(1) configuration composite mortar:, be inorganic powder, suspending agent, dispersant and the bearer configuration form slurry D of 3-40 μ m with average grain diameter with homogeneous particle diameter inorganic powder, suspending agent, dispersant and the bearer configuration form slurry C of particle diameter 0.2-1 μ m;
(2) three centrifugal formings: according to the position at the required place of controlling diaphragm, at first the amount with 1/3-2/3 slurry D joins in the pipe die, under centrifugal action, form supporter at adjacent pipe die inwall, then slurry C is injected in the pipe die, under centrifugal action, slurry C forms the uniform rete in an aperture on the supporter that slurry D forms, at last remaining slurry D is injected pipe die, carry out centrifugal forming, on the rete that slurry C forms, form an inner supporting body again, formed by three centrifugal formings and to have had interior outer support, the film built-in type inorganic film tube green compact of control rete between interior outer support separate and slough carrier, oven dry, the demoulding, sintering can make film built-in type inorganic film tube of the present invention.
In the described slurry C of step (1) among the parts by weight of each component and the slurry D parts by weight of each component as follows:
Inorganic powder 10-59.9;
Carrier 89.9-40;
Suspending agent 0-0.5;
Dispersant 0-0.5;
Wherein: suspending agent and dispersant are not zero simultaneously, and each composition weight umber sum is 100;
Described inorganic powder is powder Al
2O
3, TiO
2, SiO
2, ZrO
2, one or more mixtures among the SiC, diatomite, perlite, nickel, titanium, stainless steel, bronze, copper, iron;
Described carrier is a water;
Described suspending agent and dispersant are a kind of in carboxymethyl cellulose, polyvinyl alcohol, gum arabic, polyethylene glycol, the polyacrylamide.
Sintering temperature is 700～1850 ℃ described in the step (2), prepared film built-in type inorganic film tube, and its aperture, controlling diaphragm tunic hole is 0.1 μ m～5 μ m, film pipe porosity is 20～85%, diameter 5～300mm, length 10～2000mm, wall thickness are 2～15mm.
The inorganic film tube that obtains; its control rete can be in any position between the film pipe surfaces externally and internally; no matter fluid is by advancing in the pipe or outside the pipe; pollutant in the fluid is deposited on inner surface or outer surface; rather than be attached directly on the control rete; the protection of outer support in the control rete all is subjected in the use of film and cleaning process; be not easy to occur damaged; effectively thereby the integrality of retentive control rete guarantees the separation accuracy of inoranic membrane in whole use; prevent the fluid contact after the pollutant of holding back sees through the control rete and separates effectively; the secondary pollution of film separation process is dropped to minimum, the usability of film is improved greatly.
Compared with prior art, the present invention has following advantage:
(1) the controlling diaphragm tunic can place the arbitrary position between the inside and outside wall of film pipe;
(2) pollutant in the fluid can not be attached directly on the control rete;
(3) protection of outer support was not easy breakage to occur in the control rete all was subjected in use and the cleaning process, influenced the film separation accuracy;
(4) pollutant of holding back can not see through the control rete and separate after the fluid contact, drop to the secondary pollution of film separation process minimum;
(5) two slurries, twice or how this is continuously shaped, primary drying, sintering, operation is simple, with short production cycle.
The specific embodiment
Be described in further detail the present invention below by embodiment.
Embodiment 1
(1) configuration slurry A and slurry B:, through 4 hours mechanical agitation, make uniform slurry respectively with following recipe configuration slurry C, slurry D.
Slurry A:0.1 μ m～10 μ m alumina powder 50g; Water 80g; Polyacrylamide 0.1g.
Slurry B: average grain diameter 20 μ m alumina powder 50g; Water 60g; Polyacrylamide 0.1g.
(2) twice centrifugal forming
Slurry A is added in the pipe die of centrifugal film pipe forming machine, the pipe die rotating speed is 15000rpm, rotated 15 minutes, under action of centrifugal force, the largest particles among the slurry A is at first attached to the moulding of pipe die inwall, increase with molding time, inorganic powder among the slurry A is radially descending gradually to the poly-partially moulding of pipe die inwall, smallest particles in this slurry is finally at the inboard control rete that forms of outer support, the slurry B that will not contain the coarsegrain of smallest particles again injects, the pipe die rotating speed is 10000rpm, rotated 10 minutes, the long-pending moulding of bulky grain in this slurry adjacent controlling diaphragm strata under centrifugal action is at the certain thickness wide-aperture inner supporting body of the inboard formation of control rete.
Formed by twice centrifugal forming have interior outer support, the built-in tubular inorganic membrane green compact of the control film of rete between interior outer support.Carrier in forming process in the composite mortar separates with the green compact of being made up of inorganic powder particle, slough carrier, the film built-in type inorganic film tube green compact of making are through oven dry, the demoulding, sintering, film pipe sintering temperature is 1650 ℃, temperature retention time 2 hours promptly obtains the built-in tubular inorganic membrane of film after the cooling.Its key-course fenestra aperture is 0.04 μ m, film pipe porosity 35%, and diameter 28mm, length 250mm, the film tube thickness is 5mm, can be used for the micro-filtration of fluid, also can be used as membrane carrier, is the good carrier of inorganic ultrafiltration, NF membrane and can be used as the high temperature membrane reactor.
Embodiment 2
(1) configuration slurry A and slurry B: just following recipe configuration slurry A, slurry B, through 2 hours mechanical agitation, make uniform slurry respectively.
Slurry A:0.5 μ m～3 μ m metal Ti powder 30g; Water 40g; Polyethylene glycol 0.05g.
Slurry B: average grain diameter 5 mu-metal Ti powder 50g; Water 30g; Polyethylene glycol 0.1g.
(2) twice centrifugal forming
Slurry A is added in the pipe die of centrifugal film pipe forming machine, the mould rotating speed is 8000rpm, rotated 10 minutes, under action of centrifugal force, the largest particles among the slurry A is at first attached to the moulding of pipe die inwall, increase with molding time, Titanium powder among the slurry A is radially descending gradually to the poly-partially moulding of pipe die inwall, smallest particles in this slurry is finally at the inboard control rete that forms of outer support, the slurry B that will not contain the coarsegrain of smallest particles again injects, the pipe die rotating speed is 6000rpm, rotated 10 minutes, the long-pending moulding of bulky grain in this slurry adjacent controlling diaphragm strata under centrifugal action is at the certain thickness wide-aperture inner supporting body of the inboard formation of control rete.
Formed by twice centrifugal forming have interior outer support, the film built-in metal titanium film pipe green compact of control rete between interior outer support.Green compact are through demoulding after drying, reducing atmosphere sintering, and film pipe sintering temperature is 1050 ℃, and temperature retention time 1 hour is the Ti metal film pipe that controlled rete is in film pipe middle part after the cooling.Its key-course fenestra aperture is 0.2 μ m, film pipe porosity 40%, and diameter 20mm, length 200mm, the film tube thickness is 3mm, can be used for film catalysis, fluid purification, micro-filtration and is used as film modified carrier, and advantages such as high temperature resistant, corrosion-resistant, easy connection sealing are arranged.
Embodiment 3
(1) configuration slurry A and slurry B: just following recipe configuration slurry A, slurry B, through 4 hours mechanical agitation, make uniform slurry respectively.
Slurry A:0.5 μ m～20 μ m diatomite in powder 50g; Water 60g; Carboxymethyl cellulose 0.1g.
Slurry B: average grain diameter 30 μ m diatomite in powder 50g; Water 50g; Carboxymethyl cellulose 0.1g.
(2) twice centrifugal forming
Slurry A is added in the pipe die of centrifugal film pipe forming machine, the pipe die rotating speed is 10000rpm, rotated 15 minutes, under action of centrifugal force, the largest particles among the slurry A is at first attached to the moulding of pipe die inwall, increase with molding time, inorganic powder among the slurry A is radially descending gradually to the poly-partially moulding of pipe die inwall, smallest particles in this slurry is finally at the inboard control rete that forms of outer support, the slurry B that will not contain the coarsegrain of smallest particles again injects, the pipe die rotating speed is 8000rpm, rotated 10 minutes, the long-pending moulding of bulky grain in this slurry adjacent controlling diaphragm strata under centrifugal action is at the certain thickness wide-aperture inner supporting body of the inboard formation of control rete.
Formed by twice centrifugal forming have interior outer support, the built-in diatomaceous earth membrane pipe of the control film of rete between interior outer support green compact.Carrier in forming process in the composite mortar separates with the green compact of being made up of inorganic powder particle, slough carrier, the film built-in type inorganic film tube green compact of making are through oven dry, the demoulding, sintering, film pipe sintering temperature is 1200 ℃, temperature retention time 2 hours promptly obtains the built-in diatomaceous earth membrane pipe of film after the cooling.Its key-course fenestra aperture is 0.2 μ m, film pipe porosity 68%, and diameter 48mm, length 250mm, the film tube thickness is 8mm, can be used for the purification of compressed-air actuated purification, drinking water of rural area, dedusting, degerming, the air and the drinking water of acquisition cleaning sterile.
Embodiment 4
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 8 hours mechanical agitation, make uniform slurry respectively.
Slurry C: 0.5 μ m metal Ni powder 10g; Water 40g; Polyethylene glycol 0.05g.
Slurry D: average grain diameter 3 mu-metal Ni powder 90g; Water 30g; Polyethylene glycol 0.1g.
(2) three centrifugal formings
1/2 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the cast rotating speed is 3000rpm, pass through centrifugal forming, rotate dehydration after 5 minutes, the slurry C of reinjecting, rotating speed 10000rpm rotated 3 minutes down, dehydration, to remain 1/2 slurry D again and inject in the pipe die, the built-in metal Ni film pipe green compact of film are made in 3000rpm rotation dehydration after 5 minutes, green compact are through demoulding after drying, reducing atmosphere sintering, film pipe sintering temperature is 950 ℃, and temperature retention time 1 hour is the Ni metal film pipe that controlled rete is in film pipe middle part after the cooling.Its key-course fenestra aperture is 0.1 μ m, film pipe porosity 38%, and diameter 25mm, length 250mm, the film tube thickness is 3mm; Its mechanical strength height can use under high temperature and higher operating pressure, and can not cause the distortion and the damage of membrane module and membrane material, can excellent sealing performance be arranged by connections such as welding.The serviceability temperature scope is big, clean (can carry out chemistry, machinery or heated wash and backwash) easily, the life-span is long, and favorable actual application value is arranged.
Embodiment 5
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 10 hours mechanical agitation, make uniform slurry respectively.
Slurry C: 0.2 μ m alumina powder 5g; Water 10g; Gum arabic 0.02g.
Slurry D:10 μ m alumina powder 100g; Water 100g; Polyvinyl alcohol 0.3g.
(2) three centrifugal formings
1/3 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the pipe die rotating speed is 5000rpm, pass through centrifugal forming, dehydration, rotate after 10 minutes, the slurry C of reinjecting, rotating speed 10000rpm rotated 6 minutes down, and dehydration will remain 2/3 slurry D again and be injected in the aluminium alloy pipe die of rotation at a high speed, the pipe die rotating speed is 5000rpm, pass through centrifugal forming, dehydration was rotated after 15 minutes, made the built-in tubular inorganic membrane green compact of film, the tubular inorganic membrane green compact of making are through demoulding after drying, sintering, film pipe sintering temperature is 1600 ℃, and temperature retention time 2 hours promptly obtains the built-in tubular inorganic membrane of film after the cooling.Its key-course fenestra aperture is 0.05 μ m, film pipe porosity 48%, and diameter 60mm, length 1000mm, the film tube thickness is 6mm; It can be used for drink water purifying, but harmful substances such as the algae in harmful pathogenic bacteria such as Escherichia coli, golden staphylococci, salmonella and the water, suspended contaminant in the filtering water, and the running water after the built-in tubular inorganic membrane of this film is filtered is capable of direct drinking.Can adopt the method for backwash to clean this film pipe,, can effectively prevent the destruction of cleaning process, increase wash number and backwash hydraulic pressure, effectively prolong the service life of film pipe the control rete because controlling diaphragm is built-in.
Embodiment 6
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 4 hours mechanical agitation, make uniform slurry respectively.
Slurry C: the ultra-fine diatomite in powder 15g of average grain diameter 0.5 μ m; Water 50g; Carboxymethyl cellulose 0.1g.
Slurry D: average grain diameter 5 μ m diatomite in powder 100g; Water 150g; Carboxymethyl cellulose 0.2g.
(2) three centrifugal formings
2/3 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the pipe die rotating speed is 8000rpm, rotated 15 minutes, under action of centrifugal force, diatomite in powder in the slurry is attached to the inwall of pipe die, form the lateral branch support body, after the dehydration, slurry C is injected in the stainless steel tube pipe die of rotation at a high speed, the pipe die rotating speed is 12000rpm, rotated 10 minutes, ultra-fine diatomite in powder under action of centrifugal force in the slurry C loads on the in type supporter, forms the control rete, dehydration, remaining slurry D reinjects, the cast rotating speed is 8000rpm, rotates 10 minutes, under action of centrifugal force, diatomite in powder among the slurry D forms the built-in diatomaceous earth membrane pipe of the control film of rete between interior outer support green compact in the inboard moulding of control rete.Green compact are through demoulding after drying, sintering, and film pipe sintering temperature is 1200 ℃, and temperature retention time 2 hours promptly obtains the built-in diatomaceous earth membrane pipe of film after the cooling.Its key-course fenestra aperture is 0.2 μ m, film pipe porosity 65%, and diameter 58mm, length 500mm, the film tube thickness is 8mm; It can be used for purification, clarification and the degerming of liquid such as beverage, fruit juice.
Embodiment 7
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 3 hours mechanical agitation, make uniform slurry respectively.
Slurry C: average grain diameter 0.2 μ m superfine silicon dioxide powder 20g; Water 30g; Polyvinyl alcohol 0.1g.
Slurry D: average grain diameter 10 μ m silicon dioxide powder 100g; Water 100g; Polyvinyl alcohol 0.3g.
(2) three centrifugal formings
1/2 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the cast rotating speed is 5000rpm, rotated 15 minutes, under action of centrifugal force, inorganic powder particle among the slurry D is made travel motion, silica dioxide granule in the slurry is attached to the inwall of pipe die, again slurry C is injected in the pipe die of rotation at a high speed, the cast rotating speed is 7000rpm, rotated 5 minutes, de-watering of slurries under action of centrifugal force, the superfine silicon dioxide powder in the slurry is attached to the inwall of lateral branch support body, form a control rete, again remaining slurry D is injected pipe die, the periosteum rotating speed is 5000rpm, rotates 15 minutes, under action of centrifugal force, silicon dioxide powder among the slurry D is made travel motion, and next-door neighbour's controlling diaphragm formable layer is close to the long-pending moulding of controlling diaphragm strata, formed the internal layer supporter of control rete, by the be under control film pipe green compact of rete between interior outer support of three continuous centrifugal moulding.The built-in silicon dioxide film pipe of the film of making green compact are through demoulding after drying, sintering, and film pipe sintering temperature is 1200 ℃, and temperature retention time 2 hours promptly obtains the built-in silicon dioxide film pipe of film after the cooling.
The built-in silicon dioxide film pipe of prepared film, its key-course fenestra aperture is 0.05 μ m, film pipe porosity 40%, diameter 25mm, length 500mm, the film tube thickness is 6mm, it can be used for filtering mature vinegar, can remove the suspensions such as yeast, bacterium and vinegar mud in the mature vinegar, and the mature vinegar color and luster after the filter is old black, aseptic, improved the biology and the abiotic stability of mature vinegar.Thoroughly solved mature vinegar and placed the problem that precipitation appears in the back, so not only simplified the mature vinegar production technology, can make aseptic mature vinegar, improved the quality of mature vinegar, solved mature vinegar can't enter the international market because of sedimentation problem a difficult problem once going on foot.
Embodiment 8
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 4 hours mechanical agitation, make uniform slurry respectively.
Slurry C: average grain diameter 1 μ m superfine zirconia powder 5g; Water 6g; Gum arabic 0.01g.
Slurry D: average grain diameter 40 μ m zirconia powder 100g; Water 100g; Gum arabic 0.3g.
(2) three centrifugal formings
1/2 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the pipe die rotating speed is 6000rpm, rotated 10 minutes, under action of centrifugal force, zirconia powder among the slurry D is attached to the inwall of pipe die, form outer support, again slurry C is injected in the stainless steel tube pipe die of rotation at a high speed, the pipe die rotating speed is 8000rpm, rotates de-watering of slurries under action of centrifugal force 5 minutes, superfine zirconia particle in the slurry is attached to the inwall of outer support, form the control rete, the remaining slurry D that reinjects, the cast rotating speed is 6000rpm, rotated 10 minutes, under action of centrifugal force, the zirconia powder among the slurry D is poly-in the interior lateral deviation of control rete, has formed inner supporting body, this have an interior outer support, the built-in zirconium oxide film pipe of the control film of rete between interior outer support green compact are through demoulding after drying, sintering, film pipe sintering temperature is 1700C, and temperature retention time 3 hours promptly obtains the built-in zirconium oxide film pipe of film after the cooling.Its key-course fenestra aperture is 0.3 μ m, film pipe porosity 54%, and diameter 45mm, length 250mm, the film tube thickness is 5mm; It can be used for air cleaning, removes floating dusts such as airborne bacterium, dust, obtains the air of aseptic cleaning.
Embodiment 9
(1) configuration slurry C and slurry D: just following recipe configuration slurry C, slurry D, through 2 hours mechanical agitation, make uniform slurry respectively.
Slurry C: average grain diameter 0.5 μ m metallic titanium powder 5g; Water 10g; Gum arabic 0.02g.
Slurry D: average grain diameter 10 μ m metallic titanium powder 100g; Water 90g; Gum arabic 0.3g.
(2) three centrifugal formings
1/3 slurry D is injected in the stainless steel pipe die of the centrifugal film pipe forming machine that rotates at a high speed, the cast rotating speed is 6000rpm, rotated 8 minutes, under action of centrifugal force, metallic titanium powder among the slurry D is attached to the inwall of pipe die, form outer support, again slurry C is injected in the stainless steel tube pipe die of rotation at a high speed, the pipe die rotating speed is 8000rpm, rotated 6 minutes, de-watering of slurries under action of centrifugal force, the superfine metal titanium valve in the slurry forms a control rete at the inwall of outer support, remaining slurry D reinjects, the pipe die rotating speed is 6000rpm, rotates 15 minutes, under action of centrifugal force, metallic titanium powder among the slurry D has formed inner supporting body at the inwall of control rete, and this have an interior outer support, the film built-in metal titanium film pipe green compact of control rete between interior outer support.Through demoulding after drying, drying, the reducing atmosphere sintering, film pipe sintering temperature is 1000 ℃, temperature retention time 2 hours promptly obtains the built-in metal titanium membrane pipe of film after the cooling.Key-course rete aperture is 0.1 μ m, film pipe porosity 45%, and diameter 50mm, length 500mm, the film tube thickness is 3mm.The built-in metal titanium membrane pipe of the film of making can be used for separation such as the fluid purification, degerming, clarification of water, air etc.
Claims (5)
1. a film built-in type inorganic film tube is characterized in that film pipe porosity is 20～85%, diameter 5～300mm, length 10～2000mm, wall thickness is 2～15mm, is made of inner supporting body, outer support and control rete, and described control rete is between inner supporting body and outer support.
2. the preparation method of the described film built-in type inorganic film tube of claim 1 is characterized in that comprising the steps:
(1) configuration composite mortar: with particle diameter is inorganic powder and suspending agent, dispersant and the bearer configuration form slurry A of 0.1～20 μ m, is inorganic powder and suspending agent, dispersant and the bearer configuration form slurry B of 5～30 μ m with particle diameter;
(2) twice centrifugal forming: slurry A is injected pipe die carry out centrifugal forming formation outer support and control rete, then slurry B is injected this pipe die, carry out centrifugal forming, slurry B forms inner supporting body on the control rete that slurry A forms, obtain green compact through twice centrifugal forming, carrier is sloughed in its separation, oven dry, the demoulding, at 700～1850 ℃ of following sintering.
3. method according to claim 2 is characterized in that the parts by weight of each component among the parts by weight of each component among the described slurry A of step (1) and the slurry B are as follows:
Inorganic powder 30～59.9;
Carrier 69.9～40;
Suspending agent 0～0.5;
Dispersant 0～0.5;
Wherein: suspending agent and dispersant are not zero simultaneously, and each composition weight umber sum is 100;
Described inorganic powder is powder Al
2O
3, TiO
2, SiO
2, ZrO
2, one or more mixtures among the SiC, diatomite, perlite, nickel, titanium, stainless steel, bronze, copper, iron;
Described carrier is a water;
Described suspending agent and dispersant are a kind of in carboxymethyl cellulose, polyvinyl alcohol, gum arabic, polyethylene glycol, the polyacrylamide.
4. the preparation method of the described film built-in type inorganic film tube of claim 1 is characterized in that comprising the steps:
(1) configuration composite mortar: with average grain diameter is inorganic powder and suspending agent, dispersant and the bearer configuration form slurry C of 0.2～1 μ m, is inorganic powder and suspending agent, dispersant and the bearer configuration form slurry D of 3～40 μ m with average grain diameter;
(2) three centrifugal formings: according to the position at the required place of controlling diaphragm, at first the amount with 1/3～2/3 slurry D joins in the pipe die, under centrifugal action, form supporter at adjacent pipe die inwall, then slurry C is injected in the pipe die, under centrifugal action, slurry C forms the uniform rete in an aperture on the supporter that slurry D forms, at last remaining slurry D is injected pipe die, under centrifugal action, on the rete that slurry C forms, form an inner supporting body again, formed by three centrifugal formings and to have had interior outer support, the film built-in type inorganic film tube green compact of control rete between interior outer support separate and slough carrier, oven dry, the demoulding, at 700～1850 ℃ of following sintering.
5. method according to claim 4 is characterized in that the parts by weight of each component among the parts by weight of each component in the described slurry C of step (1) and the slurry D are as follows:
Inorganic powder 10～59.9;
Carrier 89.9～40;
Suspending agent 0～0.5;
Dispersant 0～0.5;
Wherein: suspending agent and dispersant are not zero simultaneously, and each composition weight umber sum is 100;
Described inorganic powder is powder Al
2O
3, TiO
2, SiO
2, ZrO
2, one or more mixtures among the SiC, diatomite, perlite, nickel, titanium, stainless steel, bronze, copper, iron;
Described carrier is a water;
Described suspending agent and dispersant are a kind of in carboxymethyl cellulose, polyvinyl alcohol, gum arabic, polyethylene glycol, the polyacrylamide.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100373017A CN100415351C (en) | 2006-08-25 | 2006-08-25 | Film built-in type inorganic film tube and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100373017A CN100415351C (en) | 2006-08-25 | 2006-08-25 | Film built-in type inorganic film tube and its preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1966130A true CN1966130A (en) | 2007-05-23 |
| CN100415351C CN100415351C (en) | 2008-09-03 |
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ID=38075212
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009012706A1 (en) * | 2007-07-23 | 2009-01-29 | Guangzhen Meng | Internally-supported capillary filter membrane |
| CN107551826A (en) * | 2017-07-31 | 2018-01-09 | 成都易态科技有限公司 | The manufacturing equipment of asymmetric tubular filter element base substrate |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1543404A (en) * | 1975-04-04 | 1979-04-04 | Millipore Corp | Tubular filtration element and method of making it |
| FR2693921B1 (en) * | 1992-07-24 | 1994-09-30 | Tech Sep | Monolithic ceramic support for tangential filtration membrane. |
| CN1299808C (en) * | 2005-03-03 | 2007-02-14 | 上海一鸣过滤技术有限公司 | Tubular reducing stainlss steel micro porous film and its preparing method |
| CN100471546C (en) * | 2005-03-18 | 2009-03-25 | 广州净易环保科技有限公司 | Bicontrol film layer inorganic film pipe and its preparation method |
-
2006
- 2006-08-25 CN CNB2006100373017A patent/CN100415351C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009012706A1 (en) * | 2007-07-23 | 2009-01-29 | Guangzhen Meng | Internally-supported capillary filter membrane |
| CN107551826A (en) * | 2017-07-31 | 2018-01-09 | 成都易态科技有限公司 | The manufacturing equipment of asymmetric tubular filter element base substrate |
| CN107551826B (en) * | 2017-07-31 | 2023-11-14 | 成都易态科技有限公司 | Apparatus for manufacturing an asymmetrical tubular filter element blank |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100415351C (en) | 2008-09-03 |
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