CN114920564A - Preparation method of high-purity boron carbide tubular ceramic filtering membrane - Google Patents
Preparation method of high-purity boron carbide tubular ceramic filtering membrane Download PDFInfo
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- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 98
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 239000012528 membrane Substances 0.000 title claims abstract description 92
- 239000000919 ceramic Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000001914 filtration Methods 0.000 title claims abstract description 16
- 239000002002 slurry Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000011248 coating agent Substances 0.000 claims abstract description 6
- 238000000576 coating method Methods 0.000 claims abstract description 6
- 239000000843 powder Substances 0.000 claims description 75
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 75
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 75
- KBPLFHHGFOOTCA-UHFFFAOYSA-N caprylic alcohol Natural products CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 claims description 28
- 239000011812 mixed powder Substances 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- 239000011259 mixed solution Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 25
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 24
- 239000004327 boric acid Substances 0.000 claims description 24
- 238000000227 grinding Methods 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 15
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 15
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 15
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 15
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 14
- 239000005011 phenolic resin Substances 0.000 claims description 14
- 229920001568 phenolic resin Polymers 0.000 claims description 14
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 2
- 230000005855 radiation Effects 0.000 abstract description 12
- 239000007788 liquid Substances 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 8
- 239000003292 glue Substances 0.000 abstract description 3
- 229920002521 macromolecule Polymers 0.000 abstract description 3
- 244000005700 microbiome Species 0.000 abstract description 3
- 239000000941 radioactive substance Substances 0.000 abstract description 3
- 239000007769 metal material Substances 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 6
- 238000005457 optimization Methods 0.000 description 6
- 230000002285 radioactive effect Effects 0.000 description 6
- 239000002253 acid Substances 0.000 description 4
- 239000003513 alkali Substances 0.000 description 4
- 238000003801 milling Methods 0.000 description 4
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
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- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
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- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
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- 229910052878 cordierite Inorganic materials 0.000 description 1
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
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- 229910052863 mullite Inorganic materials 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
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- 229910052722 tritium Inorganic materials 0.000 description 1
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- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/563—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on boron carbide
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0041—Inorganic membrane manufacture by agglomeration of particles in the dry state
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Abstract
The invention relates to the technical field of inorganic non-metallic materials, in particular to a preparation method of a high-purity boron carbide tubular ceramic filter membrane. A preparation method of a high-purity boron carbide tubular ceramic filter membrane comprises the following steps: s1, preparing a support voxel blank; s2, preparing membrane layer slurry; s3, coating a film layer; and S4, sintering. The high-purity boron carbide ceramic filter membrane can be used as a ceramic membrane for filtering macromolecular substances such as suspended matters, glue, microorganisms and the like in liquid, and simultaneously absorbs neutron radiation of radioactive substances in the liquid, so that the neutron radiation hazard of nuclear-polluted liquid is reduced, and the high-purity boron carbide ceramic filter membrane is the capability which is not possessed by ceramic membranes made of other materials.
Description
Technical Field
The invention relates to the technical field of inorganic non-metallic materials, in particular to a preparation method of a high-purity boron carbide tubular ceramic filter membrane.
Background
The ceramic membrane is an asymmetric membrane formed by preparing an inorganic ceramic material through a special process and is divided into a tubular ceramic membrane and a flat ceramic membrane. The tube wall of the tubular ceramic membrane is densely distributed with micropores, under the action of pressure, the raw material liquid flows in the membrane tube or outside the membrane, small molecular substances (or liquid) permeate the membrane, and large molecular substances (or solid) are intercepted by the membrane, so that the purposes of separation, concentration, purification, environmental protection and the like are achieved. According to a certain membrane aperture range, the pressure difference between two sides of the membrane is used as a driving force, the membrane is used as a filtering medium, and under the action of a certain pressure, when feed liquid flows through the surface of the membrane, only water, inorganic salt and small molecular substances are allowed to permeate through the membrane, and macromolecular substances such as suspended matters, glue, microorganisms and the like in the water are prevented from passing through the membrane. The ceramic membrane has the advantages of high separation efficiency, stable effect, good chemical stability, acid and alkali resistance, organic solvent resistance, bacteria resistance, high temperature resistance, pollution resistance, high mechanical strength, good regeneration performance, simple separation process, low energy consumption, simple and convenient operation and maintenance, long service life and the like, is successfully applied to various fields of deep processing of foods, beverages, plants (medicines), biological medicines, fermentation, fine chemical engineering and the like, and can be used for separation, clarification, purification, concentration, oil removal, sterilization and the like in the technical process.
The ceramic membrane materials on the market at present mainly comprise mullite, cordierite, alumina, silicon carbide and the like, and compared with an organic membrane, the ceramic membrane made of the materials has the performance advantages of long service life, strong environmental adaptability, stable water production quality and the like in a plurality of water treatment scenes.
Natural boron B has two stable isotopes, 10B and 11B. The thermal neutron absorption capacity of 10B is extremely high, the cross section is as high as 3837 targets, the absorption energy spectrum is wide, strong secondary radiation is not generated after neutrons are absorbed, and the post-treatment is easy. The method has the advantages of high-efficiency stable absorption of neutron radiation, no secondary radiation release and the like in the nuclear industry. The boron carbide ceramic material has the advantages of high hardness, high temperature resistance, radiation resistance and the like on the premise of ensuring the neutron absorption capacity of boron element, and is widely applied to the nuclear power field at present as a neutron absorption material.
The treatment of nuclear polluted water is a common problem in the field of nuclear power and water treatment at present, and the traditional method for treating the nuclear polluted water is a precipitation method, namely a method for carrying out coprecipitation on a precipitator and trace radioactive nuclide in wastewater. Most of the compounds in the wastewater, such as hydroxides, carbonates, and phosphates of radioactive nuclides, are insoluble and can be removed during the treatment. However, the precipitation method cannot completely precipitate the radioactive elements, and part of the radioactive elements exist in the form of suspended matters, so that a filter membrane with fine filter pore size is required for filtration treatment. The neutron radiation of radioactive elements such as deuterium, tritium and the like cannot be solved by using the traditional water treatment process, and if the high-purity boron carbide ceramic filtering membrane is manufactured by combining the ceramic membrane manufacturing process, the neutron radiation in nuclear polluted water is absorbed while suspended radioactive solids are filtered, so that a solution can be provided for the technical problem of nuclear polluted water treatment.
Disclosure of Invention
In order to solve the problem of the high-purity boron carbide ceramic filtering membrane, the invention provides a preparation method of a high-purity boron carbide tubular ceramic filtering membrane.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a high-purity boron carbide tubular ceramic filter membrane comprises the following steps:
s1, preparation of a support voxel blank: fully mixing boron carbide micro powder, boric acid, hydroxypropyl methyl cellulose and silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder A, mixing deionized water, polyethylene glycol, phenolic resin and n-octanol according to a certain mass ratio to obtain 25 parts of mixed solution B, adding the mixed powder A and the mixed solution B into a conical mixer, adding 50 parts of silicon carbide grinding balls into the conical mixer, fully mixing for 10 hours to obtain a uniformly mixed mixture C, transferring the mixture C to an extrusion molding machine for extrusion to obtain a supporting voxel blank of the multichannel tubular boron carbide ceramic membrane;
s2, preparing membrane layer slurry: fully mixing boron carbide micro powder, hydroxypropyl methyl cellulose and silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder D, mixing deionized water, polyethylene glycol, phenolic resin and n-octanol according to a certain mass ratio to obtain 150 parts of mixed solution E, adding the mixed powder D and the mixed solution E into a conical mixer, adding 100 parts of silicon carbide grinding media balls into the conical mixer, and fully mixing for 10 hours to obtain uniformly mixed film slurry F;
s3, coating a film layer: grouting the membrane layer slurry F obtained in the step S2 into each channel of the support voxel blank obtained in the step S1 for 30-40S, and then placing the slurry in an oven for drying for 8h to obtain a boron carbide ceramic membrane blank;
s4, sintering: and (5) placing the dried boron carbide ceramic membrane blank obtained in the step (S3) in a vacuum sintering furnace for sintering, keeping the temperature for 3-5 hours after the temperature in the furnace rises, and then cooling the furnace to room temperature to obtain the high-purity boron carbide tubular ceramic filtering membrane.
As an optimization, the powder mixture A in the step S1 comprises the following components: the boron carbide micro powder is 90-95 parts by mass, the boric acid is 1 part by mass, the hydroxypropyl methyl cellulose is 2 parts by mass, and the silicon carbide micro powder is 2-7 parts by mass.
As an optimization, the mixed solution B described in step S2 includes the following components in percentage by mass: 16-18 parts of ionized water, 4-5 parts of polyvinyl alcohol, 3 parts of phenolic resin and 0.5 part of n-octanol. .
For optimization, the mixed powder D in the step S2 comprises the following components in percentage by mass: 90-95 parts of boron carbide micro powder, 2 parts of boric acid and 3-8 parts of silicon carbide micro powder.
As an optimization, the mixed solution E described in step S2 includes the following components in percentage by mass: 115-120 parts of ionized water, 20 parts of polyvinyl alcohol, 10 parts of phenolic resin and 1 part of n-octanol.
As optimization, in the step S1, the particle size D50 of the boron carbide micro powder ranges from 50 to 70 μm, the purity of the boron carbide micro powder is greater than 98%, the purity of the boric acid is greater than 99.9%, the purity of the hydroxypropyl methyl cellulose is greater than 97.8%, the particle size D50 of the silicon carbide micro powder ranges from 50 to 70 μm, the purity of the silicon carbide micro powder is greater than 99%, the content of silicon carbide in the silicon carbide milling ball is greater than 95%, and the size of the silicon carbide milling ball is a column ball with a diameter of 12 mm;
in the step S2, the particle size D50 of the boron carbide micro powder ranges from 1 to 2 microns, the purity of the boron carbide micro powder is greater than 98%, the purity of the boric acid is greater than 99.9%, the particle size D50 of the silicon carbide micro powder ranges from 1 to 2 microns, the purity of the silicon carbide micro powder is greater than 98%, the content of silicon carbide in the silicon carbide milling balls is greater than 95%, and the size of the silicon carbide milling balls is phi 12mm column balls.
And optimally, removing bubbles by using ultrasonic vibration before grouting the membrane layer slurry F obtained in the step S2, wherein the ultrasonic vibration lasts for 1 min.
As an optimization, the furnace temperature increasing process of the vacuum sintering furnace in step S4 is as follows: when the temperature is between room temperature and 1000 ℃, the heating rate is 7-8 ℃/min; keeping the temperature for 1 hour after the temperature reaches 1000 ℃, keeping the temperature for 3-5 hours after the temperature rises to 2100 ℃ at the temperature rising rate of 5 ℃/min when the temperature reaches 1000-2100 ℃, and then slowly cooling the furnace body to the room temperature;
when the temperature in the furnace is below 1000 ℃, the furnace is in a vacuum state, the vacuum degree is less than 20KPa, when the temperature in the furnace is above 1000 ℃, argon is filled for protection, and the furnace is in a normal pressure state.
The beneficial effect of this scheme is: the preparation method of the high-purity boron carbide tubular ceramic filtering membrane has the following beneficial effects:
the high-purity boron carbide ceramic filter membrane can be used as a ceramic membrane for filtering macromolecular substances such as suspended matters, glue, microorganisms and the like in liquid, and simultaneously absorbs neutron radiation of radioactive substances in the liquid, so that the neutron radiation hazard of nuclear-polluted liquid is reduced, which is the capability that ceramic membranes made of other materials do not have;
boron carbide is one of the three hardest known materials, the Mohs hardness of the boron carbide is 9.3, and the Vickers hardness of a high-purity boron carbide ceramic filter membrane material reaches 1800kgf/mm 2 Therefore, the film body has the advantages of being firmer and more durable in the using process;
the mixed powder A and the mixed powder D adopt boron carbide micro powder, the particles of the boron carbide micro powder are bonded at 2100 ℃, a small amount of silicon carbide micro powder is used as a bonding agent, a recrystallization process is carried out at 2100 ℃, the boron carbide micro powder is bonded together better, the toughness of the whole material is enhanced, and the characteristics of high hardness, high temperature resistance, acid and alkali resistance and the like of the silicon carbide are similar to those of the boron carbide on the other hand, and the characteristics of high hardness, high temperature resistance, acid and alkali resistance of the boron carbide ceramic membrane cannot be influenced by using the boron carbide micro powder as the bonding agent;
hydroxypropyl methyl cellulose in the support is used as a support layer pore-forming agent and volatilizes in the high-temperature sintering process, so that a plurality of channels are left for the support, and the water flux of the boron carbide ceramic membrane is improved;
the boric acid can react with a small amount of free carbon impurities in the boron carbide micro powder in the high-temperature sintering process to generate boron carbide, and the purity and the boron content of the boron carbide ceramic membrane can be further improved by adding a small amount of boric acid.
The proportion of the mixed powder A to the mixed solution B is 4:1, and the mixture C obtained in the proportion has moderate wettability, so that the smooth extrusion of an extrusion forming machine is facilitated to obtain the supporting voxel blank of the boron carbide ceramic membrane.
The temperature rise process and the heat preservation time length during sintering can ensure that the ceramic membrane can not crack due to too fast temperature rise while ensuring the production efficiency.
Drawings
FIG. 1 is an electron micrograph of a supporting voxel embryo according to example 3 of the present invention.
FIG. 2 is an electron micrograph of a film layer according to example 3 of the present invention. .
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined or explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Example 1:
a preparation method of a high-purity boron carbide tubular ceramic filter membrane comprises the following steps:
s1, preparation of a support voxel blank:
according to the mass fraction, fully mixing 90 parts of boron carbide micro powder, 1 part of boric acid, 2 parts of hydroxypropyl methyl cellulose and 7 parts of silicon carbide micro powder to obtain 100 parts of mixed powder A;
mixing 16.5 parts of ionized water, 5 parts of polyvinyl alcohol, 3 parts of phenolic resin and 0.5 part of n-octanol according to mass fraction to obtain 25 parts of a mixed solution B;
adding the mixed powder A and the mixed solution B into a conical mixer, adding 50 parts by mass of silicon carbide grinding medium balls into the conical mixer, fully mixing for 10 hours to obtain a uniformly mixed mixture C, transferring the mixture C to an extrusion molding machine, and extruding to obtain a support voxel blank of the multi-channel tubular boron carbide ceramic membrane;
the particle size D50 value of boron carbide micro powder is 55 mu m, the purity of the boron carbide micro powder is 98.7%, the purity of boric acid is 99.97%, the purity of hydroxypropyl methyl cellulose is 98.8%, the particle size D50 value of the silicon carbide micro powder is 60 mu m, the purity of the silicon carbide micro powder is 99.2%, the content of silicon carbide in the silicon carbide grinding ball is 96.2%, and the size of the silicon carbide grinding ball is phi 12 mm;
s2, preparing membrane layer slurry: fully mixing 90 parts by mass of boron carbide micro powder, 2 parts by mass of boric acid and 8 parts by mass of silicon carbide micro powder to obtain 100 parts by mass of mixed powder D;
119 parts of ionized water, 20 parts of polyvinyl alcohol, 10 parts of phenolic resin and 1 part of n-octanol according to a certain mass ratio are mixed to obtain 150 parts of a mass mixed solution E;
adding the mixed powder D and the mixed solution E into a conical mixer, adding 100 parts by mass of silicon carbide grinding medium balls into the conical mixer, and fully mixing for 10 hours to prepare uniformly mixed film slurry F;
the particle size D50 of the boron carbide micro powder is 2 microns, the purity of the boron carbide micro powder is 98.7 percent, the purity of the boric acid is more than 99.9 percent, the particle size D50 of the silicon carbide micro powder is 1.7 microns, the purity of the silicon carbide micro powder is 98.2 percent, the content of silicon carbide in the silicon carbide grinding media ball is 95.5 percent, and the size of the silicon carbide grinding media ball is phi 12 mm.
S3, coating a film layer: removing bubbles from the membrane layer slurry F obtained in the step S2 through ultrasonic vibration for 1min, grouting the membrane layer slurry F after the bubbles are removed into each channel of the support voxel blank obtained in the step S1, wherein the flowing time of the slurry is 30S, and then placing the slurry in an oven to dry for 8h to obtain a boron carbide ceramic membrane blank;
s4, sintering: placing the dried boron carbide ceramic film blank obtained in the step S3 in a vacuum sintering furnace for sintering, wherein the heating rate is 7.2 ℃/min when the temperature is between room temperature and 1000 ℃; keeping the temperature for 1 hour after the temperature reaches 1000 ℃, keeping the temperature for 3 hours after the temperature reaches 2100 ℃ at the temperature of 1000-2100 ℃, keeping the temperature in the furnace in a vacuum state and the vacuum degree of 16KPa when the temperature in the furnace is below 1000 ℃, and filling argon for protection when the temperature in the furnace is above 1000 ℃, wherein the temperature in the furnace is in a normal pressure state;
and then cooling the furnace to room temperature to obtain the high-purity boron carbide tubular ceramic filter membrane.
Example 2:
a preparation method of a high-purity boron carbide tubular ceramic filter membrane comprises the following steps:
s1, preparation of a support voxel blank:
according to the mass fraction, 92.5 parts of boron carbide micro powder, 1 part of boric acid, 2 parts of hydroxypropyl methyl cellulose and 4.5 parts of silicon carbide micro powder are fully mixed to obtain 100 parts of mixed powder A;
mixing 17 parts of ionized water, 4.5 parts of polyvinyl alcohol, 3 parts of phenolic resin and 0.5 part of n-octanol by mass percent to obtain 25 parts of mixed solution B;
adding the mixed powder A and the mixed solution B into a conical mixer, adding 50 parts by mass of silicon carbide grinding medium balls into the conical mixer, fully mixing for 10 hours to obtain a uniformly mixed mixture C, transferring the mixture C to an extrusion molding machine, and extruding to obtain a support voxel blank of the multi-channel tubular boron carbide ceramic membrane;
the particle size D50 of the boron carbide micro powder is 55 microns, the purity of the boron carbide micro powder is 98.7 percent, the purity of the boric acid is 99.97 percent, the purity of the hydroxypropyl methyl cellulose is 98.8 percent, the particle size D50 of the silicon carbide micro powder is 60 microns, the purity of the silicon carbide micro powder is 99.2 percent, the content of the silicon carbide in the silicon carbide grinding ball is 96.2 percent, and the size of the column ball is phi 12 mm;
s2, preparing membrane layer slurry: fully mixing 92.5 parts of boron carbide micro powder, 2 parts of boric acid and 5.5 parts of silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder D;
119 parts of ionized water, 20 parts of polyvinyl alcohol, 10 parts of phenolic resin and 1 part of n-octanol according to a certain mass ratio are mixed to obtain 150 parts of a mass mixed solution E;
adding the mixed powder D and the mixed solution E into a conical mixer, adding 100 parts by mass of silicon carbide grinding medium balls into the conical mixer, and fully mixing for 10 hours to prepare uniformly mixed film slurry F;
the particle size D50 of the boron carbide micro powder is 2 microns, the purity of the boron carbide micro powder is 98.7 percent, the purity of the boric acid is more than 99.9 percent, the particle size D50 of the silicon carbide micro powder is 1.7 microns, the purity of the silicon carbide micro powder is 98.2 percent, the content of silicon carbide in the silicon carbide grinding media ball is 95.5 percent, and the size of the silicon carbide grinding media ball is phi 12 mm.
S3, coating a film layer: removing bubbles from the membrane layer slurry F obtained in the step S2 through ultrasonic vibration for 1min, grouting the membrane layer slurry F after the bubbles are removed into each channel of the support voxel blank obtained in the step S1, wherein the flowing time of the slurry is 35S, and then placing the slurry in an oven to dry for 8h to obtain a boron carbide ceramic membrane blank;
s4, sintering: placing the dried boron carbide ceramic film blank obtained in the step S3 in a vacuum sintering furnace for sintering, wherein the heating rate is 7.5 ℃/min when the temperature is between room temperature and 1000 ℃; keeping the temperature for 1 hour after the temperature reaches 1000 ℃, keeping the temperature for 4 hours after the temperature reaches 2100 ℃ at a heating rate of 5 ℃/min and keeping the temperature for 4 hours when the temperature in the furnace is below 1000 ℃, wherein the furnace is in a vacuum state and a vacuum degree of 18KPa, and the temperature in the furnace is above 1000 ℃, and is in a normal pressure state;
and then cooling the furnace to room temperature to obtain the high-purity boron carbide tubular ceramic filter membrane.
Example 3:
a preparation method of a high-purity boron carbide tubular ceramic filter membrane comprises the following steps:
s1, preparation of a support voxel blank:
according to the mass fraction, 95 parts of boron carbide micro powder, 1 part of boric acid, 2 parts of hydroxypropyl methyl cellulose and 2 parts of silicon carbide micro powder are fully mixed to obtain 100 parts of mixed powder A;
mixing 17.5 parts of ionized water, 4 parts of polyvinyl alcohol, 3 parts of phenolic resin and 0.5 part of n-octanol by mass percent to obtain 25 parts of mixed solution B;
adding the mixed powder A and the mixed solution B into a conical mixer, adding 50 parts by mass of silicon carbide grinding medium balls into the conical mixer, fully mixing for 10 hours to obtain a uniformly mixed mixture C, and transferring the mixture C to an extrusion molding machine for extrusion to obtain a support voxel blank of the multichannel tubular boron carbide ceramic membrane;
the particle size D50 of the boron carbide micro powder is 55 microns, the purity of the boron carbide micro powder is 98.7 percent, the purity of the boric acid is 99.97 percent, the purity of the hydroxypropyl methyl cellulose is 98.8 percent, the particle size D50 of the silicon carbide micro powder is 60 microns, the purity of the silicon carbide micro powder is 99.2 percent, the content of the silicon carbide in the silicon carbide grinding ball is 96.2 percent, and the size of the column ball is phi 12 mm;
s2, preparing membrane layer slurry: fully mixing 95 parts of boron carbide micro powder, 2 parts of boric acid and 3 parts of silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder D;
119 parts of ionized water, 20 parts of polyvinyl alcohol, 10 parts of phenolic resin and 1 part of n-octanol according to a certain mass ratio are mixed to obtain 150 parts of a mass mixed solution E;
adding the mixed powder D and the mixed solution E into a conical mixer, adding 100 parts by mass of silicon carbide grinding medium balls into the conical mixer, and fully mixing for 10 hours to prepare uniformly mixed film slurry F;
the particle size D50 value of boron carbide micro powder is 2 mu m, the purity of the boron carbide micro powder is 98.7%, the purity of boric acid is more than 99.9%, the particle size D50 value of silicon carbide micro powder is 1.7 mu m, the purity of the silicon carbide micro powder is 98.2%, the content of silicon carbide in the silicon carbide grinding medium ball is 95.5%, and the size of the silicon carbide grinding medium ball is phi 12 mm.
S3, coating a film layer: removing bubbles from the membrane layer slurry F obtained in the step S2 through ultrasonic vibration for 1min, grouting the membrane layer slurry F after the bubbles are removed into each channel of the support voxel blank obtained in the step S1, wherein the flowing time of the slurry is 30-40S, and then placing the slurry in an oven to dry for 8h to obtain a boron carbide ceramic membrane blank;
s4, sintering: placing the dried boron carbide ceramic film blank obtained in the step S3 in a vacuum sintering furnace for sintering, wherein the heating rate is 7.1 ℃/min when the temperature is between room temperature and 1000 ℃; keeping the temperature for 1 hour after the temperature reaches 1000 ℃, keeping the temperature for 5 hours after the temperature reaches 1000-2100 ℃, keeping the temperature for 5 hours after the temperature reaches 2100 ℃, keeping the temperature in the furnace in a vacuum state and a vacuum degree of 19KPa when the temperature in the furnace is below 1000 ℃, filling argon for protection when the temperature in the furnace is above 1000 ℃, and keeping the temperature in the furnace in a normal pressure state;
and then cooling the furnace to room temperature to obtain the high-purity boron carbide tubular ceramic filter membrane.
The test data of the high-purity boron carbide tubular ceramic filtering membrane obtained in the embodiment 1-3 are as follows:
the high-purity boron carbide tubular ceramic filter membrane obtained by the preparation method of the high-purity boron carbide tubular ceramic filter membrane has the characteristics of high Vickers hardness, high bending strength and acid and alkali resistance, and has the advantages of large water flow capacity, high filtering efficiency, high boron carbide purity, strong neutron radiation absorption capacity and capability of absorbing radioactive substances in nuclear waste liquid and neutron radiation.
The above embodiments are only specific cases of the present invention, and the protection scope of the present invention includes but is not limited to the product form and style of the above embodiments, and any method for preparing a high purity boron carbide tubular ceramic filter membrane according to the claims of the present invention and any suitable changes or modifications thereof by those skilled in the art shall fall within the protection scope of the present invention.
Claims (8)
1. A preparation method of a high-purity boron carbide tubular ceramic filter membrane is characterized by comprising the following steps: the method comprises the following steps:
s1, preparation of a support voxel blank: fully mixing boron carbide micro powder, boric acid, hydroxypropyl methyl cellulose and silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder A, mixing deionized water, polyethylene glycol, phenolic resin and n-octanol according to a certain mass ratio to obtain 25 parts of mixed solution B, adding the mixed powder A and the mixed solution B into a conical mixer, adding 50 parts of silicon carbide grinding balls into the conical mixer, fully mixing for 10 hours to obtain a uniformly mixed mixture C, transferring the mixture C to an extrusion molding machine for extrusion to obtain a supporting voxel blank of the multichannel tubular boron carbide ceramic membrane;
s2, preparing membrane layer slurry: fully mixing boron carbide micro powder, hydroxypropyl methyl cellulose and silicon carbide micro powder according to a certain mass ratio to obtain 100 parts of mixed powder D, mixing deionized water, polyethylene glycol, phenolic resin and n-octanol according to a certain mass ratio to obtain 150 parts of mixed solution E, adding the mixed powder D and the mixed solution E into a conical mixer, adding 100 parts of silicon carbide grinding media balls into the conical mixer, and fully mixing for 10 hours to obtain uniformly mixed film slurry F;
s3, coating a film layer: grouting the membrane layer slurry F obtained in the step S2 into each channel of the support voxel blank obtained in the step S1 for 30-40S, and then placing the slurry in an oven for drying for 8h to obtain a boron carbide ceramic membrane blank;
s4, sintering: and (5) placing the dried boron carbide ceramic membrane blank obtained in the step (S3) in a vacuum sintering furnace for sintering, keeping the temperature for 3-5 hours after the temperature in the furnace rises, and then cooling the furnace to room temperature to obtain the high-purity boron carbide tubular ceramic filtering membrane.
2. The preparation method of the high-purity boron carbide tubular ceramic filtering membrane according to claim 1, which is characterized by comprising the following steps of: the mixed powder A in the step S1 comprises the following components: the boron carbide micro powder is 90-95 parts by mass, the boric acid is 1 part by mass, the hydroxypropyl methyl cellulose is 2 parts by mass, and the silicon carbide micro powder is 2-7 parts by mass.
3. The preparation method of the high-purity boron carbide tubular ceramic filter membrane according to claim 2, characterized by comprising the following steps: the mixed solution B in the step S2 comprises the following components in percentage by mass: 16-18 parts of ionized water, 4-5 parts of polyvinyl alcohol, 3 parts of phenolic resin and 0.5 part of n-octanol.
4. The preparation method of the high-purity boron carbide tubular ceramic filter membrane according to claim 3, characterized by comprising the following steps: the mixed powder D in the step S2 comprises the following components in percentage by mass: 90-95 parts of boron carbide micro powder, 2 parts of boric acid and 3-8 parts of silicon carbide micro powder.
5. The preparation method of the high-purity boron carbide tubular ceramic filter membrane according to claim 4, characterized by comprising the following steps: the mixed solution E in the step S2 comprises the following components in percentage by mass: 115-120 parts of ionized water, 20 parts of polyvinyl alcohol, 10 parts of phenolic resin and 1 part of n-octyl alcohol.
6. The preparation method of the high-purity boron carbide tubular ceramic filtering membrane according to claim 5, characterized by comprising the following steps: the particle size D50 range of the boron carbide micro powder in the step S1 is 50-70 microns, the purity of the boron carbide micro powder is larger than 98%, the purity of boric acid is larger than 99.9%, the purity of hydroxypropyl methyl cellulose is larger than 97.8%, the particle size D50 range of the silicon carbide micro powder is 50-70 microns, the purity of the silicon carbide micro powder is larger than 99%, the content of silicon carbide in the silicon carbide grinding media ball is larger than 95%, and the size of the silicon carbide grinding media ball is phi 12 mm;
the particle size D50 range of the boron carbide micro powder in the step S2 is 1-2 microns, the purity of the boron carbide micro powder is larger than 98%, the purity of the boric acid is larger than 99.9%, the particle size D50 range of the silicon carbide micro powder is 1-2 microns, the purity of the silicon carbide micro powder is larger than 98%, the content of silicon carbide in the silicon carbide grinding media ball is larger than 95%, and the size of the silicon carbide grinding media ball is phi 12 mm.
7. The preparation method of the high-purity boron carbide tubular ceramic filter membrane according to claim 6, characterized by comprising the following steps: and (3) before grouting, removing bubbles by using ultrasonic vibration for 1min before grouting the membrane layer slurry F obtained in the step S2.
8. The preparation method of the high-purity boron carbide tubular ceramic filter membrane according to claim 7, characterized by comprising the following steps: the furnace temperature raising process of the vacuum sintering furnace in the step S4 is as follows: when the temperature is between room temperature and 1000 ℃, the heating rate is 7-8 ℃/min; keeping the temperature for 1 hour after the temperature reaches 1000 ℃, keeping the temperature for 3-5 hours after the temperature reaches 2100 ℃ and keeping the temperature for 5-5 hours when the temperature reaches 1000-2100 ℃, and then slowly cooling the furnace body to the room temperature;
when the temperature in the furnace is below 1000 ℃, the furnace is in a vacuum state, the vacuum degree is less than 20KPa, when the temperature in the furnace is above 1000 ℃, argon is filled for protection, and the furnace is in a normal pressure state.
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