CN113896545A - Ceramic envelope for ceramic membrane and 3D printing forming method thereof - Google Patents
Ceramic envelope for ceramic membrane and 3D printing forming method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of ceramic membrane components, and particularly discloses a ceramic envelope for a ceramic membrane and a 3D printing forming method thereof, wherein the ceramic envelope comprises the following steps: preparing ceramic slurry; injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body; drying, removing the glue and sintering at high temperature on the ceramic envelope green body to obtain a finished product; the ceramic slurry comprises the following components in parts by weight: 75-80 parts of ceramic powder, 20-25 parts of photosensitive resin prepolymer, 0.2-0.5 part of first dispersing agent and 0.2-0.5 part of photoinitiator. The preparation method provided by the invention has the advantages of simple process and accurate size, and the obtained ceramic envelope can be suitable for severe working conditions such as strong corrosivity, high temperature, organic solvent and the like, and overcomes the defects of the conventional ceramic membrane component.
Description
Technical Field
The invention relates to the technical field of ceramic membrane components, in particular to a ceramic envelope for a ceramic membrane and a 3D printing forming method thereof.
Background
As a novel separation material, the ceramic membrane has obvious advantages of easy cleaning, corrosion resistance, high temperature resistance, long service life and the like, is suitable for separation and filtration treatment in environments with strong acid-base property, high temperature, strong oxidizability and the like, and has the advantages which are incomparable with filtration material membranes of metals, macromolecules and the like. Therefore, the ceramic membrane has significant development potential in the fields of chemical industry, electric power, biological medicine, industrial sewage purification and the like.
However, in practical applications, the ceramic membrane is still difficult to operate and serve for a long time under severe conditions of strong corrosion, high temperature, strong oxidation and the like. The flat ceramic membrane with a wide application range is taken as an example, and the main reasons for the failure of the flat ceramic membrane under severe working conditions are as follows: 1. in a strong corrosive environment, the diaphragm of the flat ceramic membrane is made of a ceramic-based material, and the main material is generally alumina, titanium oxide or silicon carbide. And the packaging structure material such as envelope, end socket, etc. of the component is one of ABS resin, PP or PVC, and organic adhesive such as epoxy resin or polyurethane. Although the diaphragm is made of ceramic material and has good acid and alkali corrosion resistance, the packaging material in the module is made of specific organic material and does not have sufficient acid and alkali corrosion resistance. Therefore, in the service process of the whole ceramic membrane module, the organic material is often the first factor of failure, and usually causes the leakage at the sealing position of the ceramic membrane module to cause the sealing failure, thereby directly influencing the operation and filtration performance of the module. 2. Under high temperature environment, the organic materials used in the ceramic membrane module generally cannot be used for a long time at high temperature (T >60 ℃), because the organic material module generates softening deformation at high temperature, which also causes peeling between the organic materials and the ceramic membrane, and leads to damage of the sealing structure. Meanwhile, because the difference between the thermal expansion coefficients of the organic material and the ceramic material is large, the organic material assembly can generate a large thermal expansion phenomenon under a high-temperature and large-temperature difference use environment, so that a large stress is generated between the ceramic membrane and the organic material assembly, the peeling phenomenon between the membrane and the envelope is caused, and even the ceramic membrane or the organic assembly is damaged. In short, in order to ensure the operational stability of the assembly as a whole, it is necessary that the components of the assembly as a whole meet the performance requirements of the actual application.
Therefore, in order to prolong the service time of the flat-plate ceramic membrane under severe conditions, the envelope or the end socket needs to be in service for a long time under severe conditions such as strong corrosion, high temperature, strong oxidation and the like.
Among the prior art, can adopt 3D printing technique preparation dysmorphism ceramic element, adopt 3D printing technique preparation ceramic envelope alright solve above-mentioned problem, the ceramic 3D printing technique commonly used has: the method comprises an ink-jet printing technology, a melting deposition molding technology and a photocuring molding technology, wherein the photocuring molding technology is a principle of curing photosensitive resin mixed with ceramic powder by using ultraviolet rays, and a blank at a printing position has the advantages of high surface quality, good mechanical property, high dimensional precision and the like, and has advantages in preparing complex ceramic parts or high-precision parts. However, the stereolithography technique also has significant disadvantages, such as: the blank is easy to damage in the post-treatment process, the proportion of the photosensitive resin and the ceramic powder is not easy to master, the mixed slurry is an irritant material with toxicity and must be stored away from light, the working environment has strict requirements, and the air circulation and the light ray are required to be ensured.
Furthermore, the photo-curing molding technology requires the ceramic slurry to have appropriate rheological characteristics, including appropriate viscosity and long-term dispersion stability. The ceramic particles must be uniformly and efficiently dispersed in the photosensitive solution, and a good ceramic paste should also maintain a suitable viscosity during printing to ensure fluidity and remain stable for a reasonable period of time without significant particle precipitation.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a 3D printing and forming method of a ceramic envelope for a ceramic membrane, wherein the ceramic slurry has good rheological property, the prepared ceramic envelope has high mechanical strength, and the preparation process is simple, the size is accurate and the industrialization is easy to realize.
The technical problem to be solved by the invention is to provide a ceramic envelope for a ceramic membrane, which can be suitable for severe working conditions such as strong corrosivity, high temperature, organic solvent and the like, has long service life and makes up the defects of the existing ceramic membrane component.
In order to solve the technical problem, the invention provides a 3D printing forming method of a ceramic envelope for a ceramic membrane, which comprises the following steps:
preparing ceramic slurry;
injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
drying, removing the glue and sintering at high temperature on the ceramic envelope green body to obtain a finished product;
the ceramic slurry comprises the following components in parts by weight: 75-80 parts of ceramic powder, 20-25 parts of photosensitive resin prepolymer, 0.2-0.5 part of first dispersing agent and 0.2-0.5 part of photoinitiator.
Preferably, the preparing of the ceramic slurry comprises the steps of:
preparing ceramic powder;
mixing the ceramic powder with the photosensitive resin prepolymer, the first dispersant and the photoinitiator, grinding and sieving to obtain ceramic slurry;
preferably, in the grinding treatment, the rotating speed is 400-500 r/min, and the grinding time is 2-5 h;
in the sieving treatment, the mesh number of the sieve is 80-200 meshes;
the viscosity of the ceramic slurry is 1-2 Pas.
Preferably, the preparing the ceramic powder comprises the following steps:
mixing alumina, kaolin, titanium oxide and a second dispersing agent in proportion to obtain first powder;
mixing the first powder with water, grinding, sieving and drying to obtain ceramic powder;
the ceramic powder comprises the following components in parts by weight: 82-97 parts of aluminum oxide, 1-15 parts of kaolin, 1-5 parts of titanium oxide and 0.2-0.5 part of second dispersing agent;
the second dispersing agent comprises one or a combination of polyethylene glycol, sodium polycarboxylate and carboxymethyl cellulose.
Preferably, the alumina comprises a first alumina, a second alumina and a third alumina, wherein the first alumina is 8-12 μm alumina, the second alumina is 4-7 μm alumina, the third alumina is 1-3 μm alumina, and the mass ratio of the first alumina to the second alumina to the third alumina is (5-6): (1-2): (3-4).
Preferably, the adding amount of the first powder is as follows: the addition amount of water = (5-7): (3-5);
mixing the first powder with water, grinding, sieving and drying to obtain ceramic powder, wherein in the grinding treatment, the rotating speed is 400-500 r/min, and the grinding time is 2-5 h;
in the sieving treatment, the mesh number of the sieve is 80-200 meshes;
the drying treatment is carried out by adopting a spray dryer, the inlet hot air temperature of the spray dryer is 150-200 ℃, the atomization pressure is 0.5-1 MPa,
the water content of the ceramic powder is 3-5%.
Preferably, the photosensitive resin prepolymer comprises acrylate and/or polyurethane;
the first dispersant comprises polyvinylpyrrolidone and/or sodium polyacrylate;
the photoinitiator comprises one or a combination of benzoin and derivatives thereof, acetophenone derivatives and triarylsulfur salts.
Preferably, the drying process of the ceramic envelope green body is as follows: drying for 3-5 h at 80-120 ℃;
the glue discharging process comprises the following steps: heating to 600-800 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-5 h;
the high-temperature firing process comprises the following steps: heating to 1300-1600 ℃ at the speed of 2-5 ℃/min, and preserving heat for 1-2 h.
The invention also provides a ceramic envelope for the ceramic membrane, which is prepared by the preparation method;
preferably, the ceramic envelope is provided with an opening surface, the opening surface is inwards recessed to form a clamping groove for accommodating the edge of the ceramic diaphragm, and the shape of the clamping groove is matched with that of the edge of the ceramic diaphragm;
one end of the clamping groove is provided with a water collecting cavity, and the water collecting cavity is far away from the opening surface and is communicated with the clamping groove;
and glue pouring grooves are formed in two sides of the clamping groove, are formed along two sides of the clamping groove and are communicated with the clamping groove.
Preferably, the glue pouring groove is V-shaped, a chamfer angle is arranged at the joint of the glue pouring groove and the clamping groove, and a chamfer angle is arranged at the joint of the glue pouring groove and the opening surface;
the inner surface of the glue pouring groove is provided with a concave-convex structure.
The implementation of the invention has the following beneficial effects:
according to the 3D printing forming method for the ceramic envelope for the ceramic membrane, the ceramic slurry is used as the raw material, the 3D printing technology is adopted to prepare the special-shaped ceramic envelope, the ceramic envelope has the characteristics of excellent corrosion resistance, high temperature resistance and the like, and the thermal expansion coefficients of the ceramic envelope and the ceramic membrane are basically consistent, so that the stability influence of severe environments such as acid-base corrosion, high temperature and the like on the ceramic membrane component can be effectively avoided, and the integrated ceramic membrane component can be stably suitable for the separation and filtration process in a specific environment for a long time.
According to the invention, the ceramic slurry suitable for the photocuring molding technology is prepared by adopting a specific ceramic slurry formula, and the ceramic slurry has good rheological property, good fluidity and good stability. Moreover, the ceramic envelope finally obtained by the invention has high mechanical strength and long service life.
Drawings
Fig. 1 is a schematic structural view of a ceramic envelope for a ceramic membrane according to the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below.
Among the prior art, can adopt 3D printing technique preparation dysmorphism ceramic element, adopt 3D printing technique preparation ceramic envelope alright solve above-mentioned problem, the ceramic 3D printing technique commonly used has: the method comprises an ink-jet printing technology, a melting deposition molding technology and a photocuring molding technology, wherein the photocuring molding technology is a principle of curing photosensitive resin mixed with ceramic powder by using ultraviolet rays, and a blank at a printing position has the advantages of high surface quality, good mechanical property, high dimensional precision and the like, and has advantages in preparing complex ceramic parts or high-precision parts. However, the stereolithography technique also has significant disadvantages, such as: the blank is easy to damage in the post-treatment process, the proportion of the photosensitive resin and the ceramic powder is not easy to master, the mixed slurry is an irritant material with toxicity and must be stored away from light, the working environment has strict requirements, and the air circulation and the light ray are required to be ensured.
Furthermore, the photo-curing molding technology requires the ceramic slurry to have appropriate rheological characteristics, including appropriate viscosity and long-term dispersion stability. The ceramic particles must be uniformly and efficiently dispersed in the photosensitive solution, and a good ceramic paste should also maintain a suitable viscosity during printing to ensure fluidity and remain stable for a reasonable period of time without significant particle precipitation.
In order to solve the above problems, the present invention provides a 3D printing forming method of a ceramic envelope for a ceramic membrane, comprising the steps of:
s1, preparing ceramic slurry;
s2, injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
s3, drying, binder removal and high-temperature sintering of the ceramic envelope green body to obtain a finished product;
the ceramic slurry comprises the following components in parts by weight: 75-80 parts of ceramic powder, 20-25 parts of photosensitive resin prepolymer, 0.2-0.5 part of first dispersing agent and 0.2-0.5 part of photoinitiator.
The invention takes ceramic slurry as a raw material and adopts a 3D printing technology to prepare the special-shaped ceramic envelope. It should be noted that the envelope with the special-shaped structure can be accurately and quickly prepared by adopting the 3D printing technology, and the preparation problem of the ceramic envelope is solved. The traditional ceramic material forming process can be divided into compression forming, plastic forming and slip casting forming, but for the ceramic product with a complex structure of a ceramic envelope, the traditional ceramic forming technology can not be sufficient, and the ceramic product with a special-shaped structure can be obtained only by later processing. But the cost of the later processing of the ceramics is extremely high and the yield is lower, which is not beneficial to the industrialized production. The special-shaped ceramic piece can be flexibly prepared by adopting the 3D printing method, and meanwhile, aiming at the ceramic envelope, the designed envelope structure does not need to adopt extremely high preparation precision, so that the problem that the 3D printing molding consumes too long time is solved.
The prepared ceramic envelope has the characteristics of excellent corrosion resistance, high temperature resistance and the like, and the thermal expansion coefficients of the ceramic envelope and the ceramic membrane are basically consistent, so that the influence of acid-base corrosion, high temperature and other severe environments on the stability of the ceramic membrane assembly can be effectively avoided, and the integrated ceramic membrane assembly can be stably suitable for the separation and filtration process in a specific environment for a long time.
According to the invention, the ceramic slurry suitable for the photocuring molding technology is prepared by adopting a specific ceramic slurry formula, and the ceramic slurry has good rheological property, good fluidity and good stability. Moreover, the ceramic envelope finally obtained by the invention has high mechanical strength and long service life.
The preparation method comprises the following specific steps:
s1, preparing ceramic slurry;
in order to meet the requirements of 3D printing on formula and raw materials, the invention provides a ceramic slurry system, and preferably, the preparation of the ceramic slurry comprises the following steps:
preparing ceramic powder;
and mixing 75-80 parts of ceramic powder, 20-25 parts of photosensitive resin prepolymer, 0.2-0.5 part of first dispersant and 0.2-0.5 part of photoinitiator, grinding and sieving to obtain the ceramic slurry.
It should be noted that the proportion of the ceramic powder not only affects the roughness of the appearance of the finally obtained ceramic envelope, but more importantly, the proportion of the ceramic powder affects the mechanical strength of the finally obtained ceramic envelope.
The inventors have found that when the ceramic powder is present in an amount of 75 to 80 parts by weight, the resulting ceramic envelope can have a good mechanical strength. When the weight part of the ceramic powder is less than 75 parts, Al in a resin system2O3The particle content is too small, the density of the sintered ceramic is not enough, the combination of the ceramic particles is poor, and the Vickers hardness of the obtained ceramic envelope is reduced.
When the ceramic powder is present in an amount of more than 80 parts by weight, the ceramic envelope may have poor flexural strength and fracture toughness, and although the hardness of the ceramic envelope is increased, the ceramic itself may have increased brittleness, resulting in a great decrease in flexural strength and fracture toughness.
According to the invention, the ceramic powder with a self-made formula is adopted, and the ceramic envelope can meet the subsequent severe use environment and the requirements of a 3D printing process. Preferably, the ceramic powder of the present invention is prepared by the following steps:
mixing alumina, kaolin, titanium oxide and a second dispersing agent in proportion to obtain first powder;
mixing the first powder with water, grinding, sieving and drying to obtain ceramic powder;
the ceramic powder comprises the following components in parts by weight: 82-97 parts of aluminum oxide, 1-15 parts of kaolin, 1-5 parts of titanium oxide and 0.2-0.5 part of second dispersing agent.
The main raw material of the ceramic powder is alumina, and the alumina finally forms the base material of the ceramic envelope, which is consistent with the material of the mainstream commercial flat ceramic film. Moreover, alumina has good corrosion resistance and excellent mechanical properties, and is a raw material suitable for 3D printing. Preferably, the alumina comprises a first alumina, a second alumina and a third alumina, wherein the first alumina is 8-12 μm alumina, the second alumina is 4-7 μm alumina, the third alumina is 1-3 μm alumina, and the mass ratio of the first alumina to the second alumina to the third alumina is (5-6): (1-2): (3-4).
It should be noted that, alumina is used as an aggregate in the ceramic powder, which determines the flow property of the finally obtained ceramic slurry to a certain extent, in the prior art, alumina with a single particle size is often used, the particle size of the alumina is generally 10 to 20 μm, but flocculation is likely to occur between alumina powders with single particle sizes, and the slurry viscosity is increased by larger coarse alumina particles, which is not favorable for 3D printing of alumina ceramics. The invention adopts alumina particles with different sizes, and mixes the alumina particles according to a specific proportion, and the alumina particles with larger particle size are added in a proper amount to reduce the weaker interaction among the alumina particles in the slurry, so that the slurry has small viscosity and good fluidity, and the ceramic slurry prepared by the method has better fluidity.
In addition, the aluminum oxide particles with smaller particle size can be distributed among the aluminum oxide particles with larger particle size by adopting the aluminum oxide particles with different sizes, gaps among the aluminum oxide particles are filled, the effective bonding area among the aluminum oxide particles is increased in the sintering process, the bonding among the aluminum oxide powder is firmer, the mechanical strength of a finished product is increased finally, and the obtained ceramic envelope has better bending resistance and higher density.
The ceramic powder formula also comprises kaolin, titanium oxide and other raw materials, wherein the kaolin is used as a plasticizer, the titanium oxide is used as a sintering aid, and a second dispersing agent is added to ensure the uniformity of the components. Preferably, the second dispersant comprises one or a combination of polyethylene glycol, sodium polycarboxylate and carboxymethyl cellulose.
The ceramic powder preparation process needs wet grinding, and preferably, the addition amount of the first powder is as follows: the addition amount of water = (5-7): (3-5); more preferably, the addition amount of the first powder is as follows: water addition = 6: 4. the milling apparatus comprises a planetary ball mill or a nano mill, preferably the resulting milling apparatus is a planetary ball mill. In the grinding treatment, the rotation speed is preferably 400-500 r/min, and the grinding time is preferably 2-5 h. And (4) sieving after grinding is finished, preferably, in the sieving treatment, the mesh number of a sieve is 80-200 meshes. And finally, drying the uniform suspension without agglomeration in drying equipment, preferably, the drying equipment is a spray dryer, the inlet hot air temperature of the spray dryer is 150-200 ℃, and the atomization pressure is 0.5-1 MPa. The water content of the finally obtained ceramic powder is 3-5%.
In addition, ceramic pastes for 3D printing are required to satisfy good dispersibility, suspensibility, and rheological properties and to have good photocurability. Therefore, the ceramic slurry also comprises a photosensitive resin prepolymer, a first dispersing agent and a photoinitiator.
Preferably, the photosensitive resin prepolymer comprises acrylate and/or polyurethane; more preferably, the photosensitive resin prepolymer is composed of two resin monomers, namely the photosensitive resin prepolymer is dipentaerythritol penta/hexaacrylate (DPHA) and 1, 6 hexanediol diacrylate, and the mass ratio of the dipentaerythritol penta/hexaacrylate (DPHA) to the 1, 6 hexanediol diacrylate is 1: 1.
Preferably, the first dispersing agent comprises polyvinylpyrrolidone and/or sodium polyacrylate, and the first dispersing agent ensures that the ceramic slurry has good powder dispersibility, avoids the phenomenon that flocculation and the like occurs in the ceramic slurry to influence the component uniformity, improves the fluidity of the ceramic slurry, improves the solid content, and reduces the difficulty of subsequent processes such as drying and the like.
The photoinitiator accelerates the crosslinking and curing of the resin under the induction of ultraviolet light. Preferably, the photoinitiator comprises one or a combination of benzoin and derivatives thereof, acetophenone derivatives, triarylsulfonium salts.
The raw materials are mixed with ceramic powder, ground and sieved to obtain ceramic slurry. Preferably, in the grinding treatment, the grinding rotating speed is 400-500 r/min, and the grinding time is 2-5 h. The milling apparatus comprises a planetary ball mill or a nano mill, preferably the resulting milling apparatus is a planetary ball mill. After grinding, sieving, preferably, in the sieving, the mesh number of a sieve is 80-200 meshes; the viscosity of the finally obtained ceramic slurry is 1-2 Pas. The ceramic slurry obtained by the preparation grinding and process treatment methods has no impurities and hard blocks, and is fine and smooth and good in fluidity. The ceramic slurry is stored for standby, and can be reprocessed before being used, preferably, the reprocessing method comprises the steps of mechanically stirring and vibrating the ceramic slurry in an ultrasonic processing mode, wherein the stirring speed is 50-100 r/min, the stirring time is 0.5-2 h, and the ceramic slurry is in a state of good suspension property and fluidity when being used.
S2, injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
in this process, the three-dimensional model of the ceramic envelope structure that has been designed is imported into a 3D printer and sliced to obtain an executable program. Preferably, the light source of the 3D printer is 350-360 nm, and the light source intensity is 8000 mu W/cm2The slice thickness is 20-150 μm, the exposure time is 8-12 s, and the printing speed is controlled at 0.1-100 mm/s. And injecting the prepared ceramic slurry into a bin of a 3D printer, conveying the ceramic slurry to a workbench through a peristaltic pump, and performing layer-by-layer stacking according to a program to finally obtain a ceramic envelope green body. Because residual slurry exists on the surface of the obtained ceramic envelope green body, the ceramic envelope green body still needs to be soaked in alcohol, assisted with ultrasonic treatment and cleaned.
S3, drying, binder removal and high-temperature sintering of the ceramic envelope green body to obtain a finished product;
specifically, the ceramic envelope green body needs to be dried first, and preferably, the drying process of the ceramic envelope green body is as follows: drying for 3-5 h at 80-120 ℃. Secondly, a large amount of organic matters exist in the ceramic envelope green body, degreasing and glue discharging treatment is needed, and preferably, the glue discharging process comprises the following steps: heating to 600-800 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-5 h, so that organic matter components in the blank can be removed under the condition. And finally, transferring the ceramic envelope green body subjected to the glue discharging into a high-temperature box type furnace, and carrying out high-temperature burning according to a temperature system to finally obtain a ceramic envelope finished product. Preferably, the high-temperature firing process is as follows: heating to 1300-1600 ℃ at the speed of 2-5 ℃/min, and preserving heat for 1-2 h.
The invention also provides a ceramic envelope for the ceramic membrane, which is prepared by the preparation method, as shown in figure 1, the ceramic envelope is provided with an opening surface, the opening surface is inwards sunken to form a clamping groove 1 for accommodating the edge of the ceramic membrane 4, and the shape of the clamping groove 1 is matched with the shape of the edge of the ceramic membrane 4;
one end of the clamping groove 1 is provided with a water collecting cavity 2, and the water collecting cavity 2 is far away from the opening surface and is communicated with the clamping groove 1;
and glue pouring grooves 3 are formed in two sides of the clamping groove 1, and the glue pouring grooves 3 are formed along two sides of the clamping groove 1 and are communicated with the clamping groove 1.
The ceramic envelope provided by the invention comprises a clamping groove 1, a water collecting cavity 2 and a glue pouring groove 3. The clamping groove 1 is used for installing and positioning the ceramic diaphragm 4, so that the ceramic diaphragm 4 is stably positioned in the ceramic envelope, and the phenomenon of dislocation or slippage and the like is prevented from causing poor adhesion. The water collecting cavity 2 is used for collecting penetrating fluid and is beneficial to water drainage of a water outlet channel. A certain gap is formed between the glue pouring groove 3 and the clamping groove 1, and the glue pouring groove can be used for pouring glue.
Preferably, the glue pouring groove 3 is V-shaped, a chamfer is arranged at the joint of the glue pouring groove 3 and the clamping groove 1, and a chamfer is arranged at the joint of the glue pouring groove 3 and the opening surface. The inner surface of the glue pouring groove 3 is provided with a concave-convex structure. More preferably, the chamfer dimension is 1-2 mm. The V-shaped shape and the concave-convex surface of the glue pouring groove 3 are beneficial to the inorganic adhesive to flow into the glue pouring groove 3, the phenomenon that the inorganic adhesive is not fully contacted with the inner surfaces of the ceramic membrane 4 and the ceramic envelope or bubbles exist inside the inorganic adhesive is avoided, the contact area between the inorganic adhesive and the inner wall of the glue pouring groove 3 is increased by the concave-convex surface, and the combination degree between the inorganic adhesive and the glue pouring groove is improved.
Taking a flat ceramic membrane with the specification of 250mm in width, 1000mm in length and 6mm in thickness as an example, the outer dimension of the ceramic envelope matched with the flat ceramic membrane is preferably 20-25mm in height and 257-262mm in length, and it should be noted that the outer dimension and shape of the ceramic envelope are not limited by the present invention.
In the internal structure of the ceramic envelope, preferably, the water collecting cavity 2 is located at the innermost side of the ceramic envelope, and has a rectangular cross section, and more preferably, the water collecting cavity 2 has a width of 2-4mm, a height of 2-4mm, and a length of 255-260 mm.
The water collecting cavity 2 is communicated with the clamping groove 1, preferably, the width of the clamping groove 1 is 6.0-6.5mm, the size of the clamping groove is matched with the thickness of the ceramic diaphragm 4, and a gap between the ceramic diaphragm 4 and the clamping groove 1 can be used for entering an adhesive to realize the insertion positioning of the ceramic diaphragm 4 and simultaneously used for stabilizing the mechanical fixation of the envelope and the diaphragm and avoiding the slippage phenomenon in the subsequent process.
Two sides of the clamping groove 1 are provided with glue pouring grooves 3, preferably, the width between the glue pouring grooves 3 and the installed ceramic diaphragm 4 is 0.1-1mm, and the length of the glue pouring grooves 3 is smaller than that of the clamping groove 1.
The invention is further illustrated by the following specific examples:
example 1
A method of making a ceramic envelope comprising the steps of:
s1, preparing ceramic slurry;
1.1 preparing ceramic powder;
mixing 82 parts of alumina, 13 parts of kaolin, 4.5 parts of titanium oxide and 0.5 part of polyethylene glycol to obtain first powder, wherein the alumina comprises 60% of first alumina with the average particle size of 10 microns, 10 parts of second alumina with the average particle size of 5 microns and 30% of third alumina with the average particle size of 2 microns;
mixing the first powder and water according to a mass ratio of 6:4, grinding the mixture in a ball mill at a rotating speed of 400r/min for 3 hours, then sieving the mixture by a 120-mesh sieve, and then drying the mixture in a spray dryer with inlet hot air temperature of 200 ℃ and atomization pressure of 0.8MPa to obtain ceramic powder;
1.2 mixing 79 parts of the ceramic powder, 10 parts of dipentaerythritol penta/hexaacrylate, 10 parts of 1, 6 hexanediol diacrylate, 0.5 part of polyvinylpyrrolidone and 0.5 part of benzoin, grinding and sieving to obtain ceramic slurry with the viscosity of 1.5 Pas;
in the grinding treatment, the rotating speed is 500r/min, and the grinding time is 3 h; in the screening treatment, the mesh number of the screen is 120 meshes.
S2, injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
adopts SLA ceramic 3D printer with ultraviolet laser 355nm light source of 8000 μ W/cm intensity2The slice thickness was set to 100 μm, the exposure time was 10s, and the printing speed was controlled in the range of 50mm/s for printing.
S3, drying, binder removal and high-temperature sintering of the ceramic envelope green body to obtain a finished product;
the drying process of the ceramic envelope green body comprises the following steps: drying at 100 deg.C for 4 h;
the glue discharging process comprises the following steps: heating to 800 ℃ at the speed of 8 ℃/min, and preserving heat for 3 h;
the high-temperature firing process comprises the following steps: heating to 1500 deg.C at a speed of 5 deg.C/min, and maintaining for 1.5 h.
The ceramic envelope with ceramic membrane prepared by the method is used for the flat ceramic membrane with the specification of 250mm in width and 1000mm in length and 6mm in thickness.
The ceramic envelope is provided with an opening surface, the opening surface is inwards sunken to form a clamping groove for containing the edge of the ceramic diaphragm, and the shape of the clamping groove is matched with that of the edge of the ceramic diaphragm;
one end of the clamping groove is provided with a water collecting cavity, and the water collecting cavity is far away from the opening surface and is communicated with the clamping groove;
and glue pouring grooves are formed in two sides of the clamping groove, are formed along two sides of the clamping groove and are communicated with the clamping groove.
The ceramic envelope was matched to a flat ceramic membrane of width 250mm and length 1000mm and thickness 6mm, with the outside dimensions of the ceramic envelope being 20mm in height and 257mm in length. The water collecting cavity is rectangular in cross section, 2mm in width, 2mm in height and 255mm in length. The width of draw-in groove is 6.1mm, and the height is 10mm, and length is 255 mm. The width between the glue pouring groove and the installed ceramic membrane is 0.5mm, the height is 5mm, and the length is 255 mm.
Example 2
A3D printing forming method of a ceramic envelope for a ceramic membrane comprises the following steps:
s1, preparing ceramic slurry;
1.1 preparing ceramic powder;
mixing 97 parts of alumina, 1.5 parts of kaolin, 1.3 parts of titanium oxide and 0.2 part of sodium polycarboxylate to obtain first powder, wherein the alumina comprises 50% of first alumina with the average particle size of 11 mu m, 20% of second alumina with the average particle size of 6 mu m and 30% of third alumina with the average particle size of 3 mu m;
mixing the first powder and water according to a mass ratio of 5:5, grinding for 4h in a ball mill at a rotating speed of 500r/min, then passing through a 200-mesh screen, and then drying in a spray dryer with an inlet hot air temperature of 200 ℃ and an atomization pressure of 1MPa to obtain ceramic powder;
1.2 mixing 75 parts of the ceramic powder, 10 parts of dipentaerythritol penta/hexaacrylate, 10 parts of 1, 6 hexanediol diacrylate, 0.5 part of sodium polyacrylate and 0.5 part of triaryl sulfide salt, grinding and sieving to obtain ceramic slurry with the viscosity of 1 Pas;
in the grinding treatment, the rotating speed is 450r/min, and the grinding time is 5 h; in the screening treatment, the mesh number of the screen is 150.
S2, injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
adopts SLA ceramic 3D printer with ultraviolet laser 355nm light source of 8000 μ W/cm intensity2The slice thickness was set to 150 μm, the exposure time was set to 10s, and the printing speed was controlled to be in the range of 80mm/s for printing.
S3, drying, binder removal and high-temperature sintering of the ceramic envelope green body to obtain a finished product;
the drying process of the ceramic envelope green body comprises the following steps: drying at 120 deg.C for 3 h;
the glue discharging process comprises the following steps: heating to 600 ℃ at the speed of 10 ℃/min, and preserving heat for 5 h;
the high-temperature firing process comprises the following steps: heating to 1300 ℃ at the speed of 2 ℃/min, and preserving heat for 1 h.
The ceramic envelope with ceramic membrane prepared by the method is used for flat ceramic membrane with the specification of 150mm in width and 800mm in length and 3mm in thickness.
The ceramic envelope is provided with an opening surface, the opening surface is inwards sunken to form a clamping groove for containing the edge of the ceramic diaphragm, and the shape of the clamping groove is matched with that of the edge of the ceramic diaphragm;
one end of the clamping groove is provided with a water collecting cavity, and the water collecting cavity is far away from the opening surface and is communicated with the clamping groove;
and glue pouring grooves are formed in two sides of the clamping groove, are formed along two sides of the clamping groove and are communicated with the clamping groove.
The ceramic envelope is matched with a flat ceramic membrane with the specification of 150mm in width, 800mm in length and 3mm in thickness, and the outer side of the ceramic envelope is 8mm in height and 155mm in length. The water collecting cavity is rectangular in cross section, 1mm in width, 1mm in height and 152mm in length. The width of draw-in groove is 3.2mm, and highly is 5mm, and length is 152 mm. The width between the glue pouring groove and the installed ceramic membrane is 0.1mm, the height is 3mm, and the length is 152 mm.
Example 3
A3D printing forming method of a ceramic envelope for a ceramic membrane comprises the following steps:
s1, preparing ceramic slurry;
1.1 preparing ceramic powder;
mixing 92 parts of alumina, 14 parts of kaolin, 3.6 parts of titanium oxide and 0.4 part of polyethylene glycol to obtain first powder, wherein the alumina comprises 60% of first alumina with the average particle size of 8 microns, 20% of second alumina with the average particle size of 4 microns and 20% of third alumina with the average particle size of 1 micron;
mixing the first powder and water according to a mass ratio of 7:3, grinding for 4 hours in a ball mill at a rotating speed of 450r/min, then passing through a 150-mesh screen, and then drying in a spray dryer with an inlet hot air temperature of 180 ℃ and an atomization pressure of 0.6MPa to obtain ceramic powder;
1.2 mixing 77 parts of the ceramic powder, 22.4 parts of epoxy acrylate resin, 0.3 part of polyvinylpyrrolidone and 0.3 part of benzoin, grinding and sieving to obtain ceramic slurry with the viscosity of 1.5 Pas;
in the grinding treatment, the rotating speed is 450r/min, and the grinding time is 4 h; in the screening treatment, the mesh number of the screen is 150 meshes; the ceramic slurry.
S2, injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
adopts SLA ceramic 3D printer with ultraviolet laser 355nm light source of 8000 μ W/cm intensity2The slice thickness was set to 150 μm, the exposure time was set to 10s, and the printing speed was controlled in the range of 100mm/s for printing.
S3, drying, binder removal and high-temperature sintering of the ceramic envelope green body to obtain a finished product;
the drying process of the ceramic envelope green body comprises the following steps: drying at 80 deg.C for 5 h;
the glue discharging process comprises the following steps: heating to 600 ℃ at the speed of 5 ℃/min, and preserving heat for 5 h;
the high-temperature firing process comprises the following steps: heating to 1300 ℃ at the speed of 2 ℃/min, and preserving heat for 2 h.
The ceramic envelope with ceramic membrane prepared by the above method is used for flat ceramic membrane with width of 500mm and length of 2000mm and thickness of 15 mm.
The ceramic envelope is provided with an opening surface, the opening surface is inwards sunken to form a clamping groove for containing the edge of the ceramic diaphragm, and the shape of the clamping groove is matched with that of the edge of the ceramic diaphragm;
one end of the clamping groove is provided with a water collecting cavity, and the water collecting cavity is far away from the opening surface and is communicated with the clamping groove;
and glue pouring grooves are formed in two sides of the clamping groove, are formed along two sides of the clamping groove and are communicated with the clamping groove.
The ceramic envelope is matched with a flat ceramic membrane with the specification of 500mm in width, 2000mm in length and 15mm in thickness, and the outer side of the ceramic envelope is 40mm in height and 510mm in length. The water collecting cavity is rectangular in cross section, 5mm in width, 5mm in height and 505mm in length. The width of draw-in groove is 15.5mm, and the height is 20mm, and length is 505 mm. The width between the glue pouring groove and the installed ceramic membrane is 1mm, the height is 10mm, and the length is 505 mm.
Comparative example 1
The difference from example 1 is that:
1.1 preparing ceramic powder;
mixing 82 parts of alumina, 13 parts of kaolin, 4.5 parts of titanium oxide and 0.5 part of polyethylene glycol to obtain first powder, wherein the alumina is 100% alumina with the average particle size of 10 mu m;
mixing the first powder and water according to a mass ratio of 6:4, grinding the mixture in a ball mill at a rotating speed of 400r/min for 3 hours, then sieving the mixture by a 120-mesh sieve, and then drying the mixture in a spray dryer with inlet hot air temperature of 200 ℃ and atomization pressure of 0.8MPa to obtain ceramic powder;
1.2, 70 parts of ceramic powder, 14 parts of dipentaerythritol penta/hexaacrylate, 14 parts of 1, 6 hexanediol diacrylate, 1 part of polyvinylpyrrolidone and 1 part of benzoin are mixed, ground and sieved to obtain ceramic slurry;
the rest is the same as in example 1.
Table 1 is a comparison table of the mechanical strength of the ceramic envelopes obtained in examples 1 to 3 and comparative example 1, and it can be seen from table 1 that the ceramic envelopes obtained by the present invention have good mechanical properties.
Table 1 is a table comparing the mechanical strengths of the ceramic envelopes obtained in examples 1 to 3 and comparative example 1
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (11)
1. A3D printing forming method of a ceramic envelope for a ceramic membrane is characterized by comprising the following steps:
preparing ceramic slurry;
injecting the ceramic slurry into 3D printing equipment, and printing to obtain a ceramic envelope green body;
drying, removing the glue and sintering at high temperature on the ceramic envelope green body to obtain a finished product;
the ceramic slurry comprises the following components in parts by weight: 75-80 parts of ceramic powder, 20-25 parts of photosensitive resin prepolymer, 0.2-0.5 part of first dispersing agent and 0.2-0.5 part of photoinitiator.
2. The 3D print forming method of ceramic envelopes for ceramic membranes as claimed in claim 1, wherein the preparation of ceramic slurry comprises the steps of:
preparing ceramic powder;
and mixing the ceramic powder with the photosensitive resin prepolymer, the first dispersant and the photoinitiator, grinding and sieving to obtain the ceramic slurry.
3. The 3D printing forming method of ceramic envelope for ceramic membrane according to claim 2, wherein in the grinding treatment, the rotating speed is 400-500 r/min, and the grinding time is 2-5 h;
in the sieving treatment, the mesh number of the sieve is 80-200 meshes;
the viscosity of the ceramic slurry is 1-2 Pas.
4. The 3D printing forming method of ceramic envelope for ceramic membrane according to claim 2, wherein said preparing ceramic powder comprises the steps of:
mixing 82-97 parts of alumina, 1-15 parts of kaolin, 1-5 parts of titanium oxide and 0.2-0.5 part of second dispersing agent according to a mass ratio to obtain first powder;
mixing the first powder with water, grinding, sieving and drying to obtain ceramic powder;
wherein the second dispersing agent comprises one or a combination of polyethylene glycol, sodium polycarboxylate and carboxymethyl cellulose.
5. The 3D printing forming method of ceramic envelope for ceramic membrane according to claim 4, wherein the alumina comprises a first alumina, a second alumina and a third alumina, the first alumina is alumina with particle size of 8-12 μm, the second alumina is alumina with particle size of 4-7 μm, the third alumina is alumina with particle size of 1-3 μm, the mass ratio of the first alumina, the second alumina and the third alumina is (5-6): (1-2): (3-4).
6. The 3D printing and forming method of ceramic envelope for ceramic membrane according to claim 4, wherein the adding amount of the first powder is: the addition amount of water = (5-7): (3-5);
mixing the first powder with water, grinding, sieving and drying to obtain ceramic powder, wherein in the grinding treatment, the rotating speed is 400-500 r/min, and the grinding time is 2-5 h;
in the sieving treatment, the mesh number of the sieve is 80-200 meshes;
a spray dryer is adopted for drying in the drying treatment, the inlet hot air temperature of the spray dryer is 150-200 ℃, and the atomization pressure is 0.5-1 MPa;
the water content of the ceramic powder is 3-5%.
7. The 3D printing method of ceramic envelope for ceramic membrane according to claim 1, wherein the photosensitive resin pre-polymer comprises acrylate and/or polyurethane;
the first dispersant comprises polyvinylpyrrolidone and/or sodium polyacrylate;
the photoinitiator comprises one or a combination of benzoin and derivatives thereof, acetophenone derivatives and triarylsulfur salts.
8. The 3D printing method of ceramic envelopes for ceramic membranes as claimed in claim 1, wherein the drying process of the ceramic envelope green body is: drying for 3-5 h at 80-120 ℃;
the glue discharging process comprises the following steps: heating to 600-800 ℃ at the speed of 5-10 ℃/min, and preserving heat for 2-5 h;
the high-temperature firing process comprises the following steps: heating to 1300-1600 ℃ at the speed of 2-5 ℃/min, and preserving heat for 1-2 h.
9. A ceramic envelope for ceramic membrane, which is prepared by the 3D printing forming method of ceramic envelope for ceramic membrane according to any one of claims 1 to 8.
10. A ceramic envelope for a ceramic membrane according to claim 9, wherein the ceramic envelope is provided with an open face which is recessed inwardly to form a slot for receiving an edge of the ceramic membrane, the slot being shaped to conform to the shape of the edge of the ceramic membrane;
one end of the clamping groove is provided with a water collecting cavity, and the water collecting cavity is far away from the opening surface and is communicated with the clamping groove;
and glue pouring grooves are formed in two sides of the clamping groove, are formed along two sides of the clamping groove and are communicated with the clamping groove.
11. A ceramic envelope for a ceramic membrane as claimed in claim 10, wherein the potting groove is V-shaped, a chamfer is provided at a junction of the potting groove and the neck, and a chamfer is provided at a junction of the potting groove and the opening surface;
the inner surface of the glue pouring groove is provided with a concave-convex structure.
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