CN104014252A - Preparation method of ceramic membrane supporting body - Google Patents
Preparation method of ceramic membrane supporting body Download PDFInfo
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- CN104014252A CN104014252A CN201410187930.2A CN201410187930A CN104014252A CN 104014252 A CN104014252 A CN 104014252A CN 201410187930 A CN201410187930 A CN 201410187930A CN 104014252 A CN104014252 A CN 104014252A
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Abstract
The invention discloses a preparation method of a ceramic filtering membrane supporting body. The method comprises the steps of (1) preparing a raw material, wherein the raw material comprises mixing powder, namely alpha aluminium oxide powder (1) the purity of which is greater than or equal to 99.7% and alpha aluminium oxide powder (2) the purity of which is greater than or equal to 99.8%, the median particle diameter D50 of the alpha aluminium oxide powder (1) is 18-35mum, the median particle diameter D50 of the alpha aluminium oxide powder (2) is 0.8-2mum, and the dosage of the alpha aluminium oxide powder (2) is 2%-10% (weight) of that of the alpha aluminium oxide powder (1); (2), mixing the mixing powder with a water solution of cross-linking agent acrylamide and methylene double crylic acid ammonium to form a suspension, and carrying out gel casting on the suspension; heating a formed product to 40-55 DEG C in a microwave manner, drying for 1-3 hours, calcining the dried formed product for 4-8 hours under 500-800 DEG C in air atmosphere, placing a calcined product in vacuum or atmospheric hydrogen or argon atmosphere, carrying out heat preservation on the calcined product for 4-12 hours under the condition of 1800 DEG C-1950 DEG C so as to form a supporting body of a pure alpha phase aluminum oxide ceramic filtering membrane. The preparation method provided by the invention has the advantages that the porosity of a product is high, the flux is high, and the product is strong-acid-resisting and strong-alkali-corrosion-resisting.
Description
Technical field
The present invention relates to the preparation method of ceramic membrane filter supporter, belong to porous ceramics preparation field.
Background technology
At film separation field, the micro-filtration that inoranic membrane is widely used in liquid medium separates with ultrafiltration and gas.
On supporter, deposit inoranic membrane that inorganic material makes can for the filtration in environment-industry, metallurgical industry, food_beverage industry, biological industry, chemical industry, petro chemical industry with separate application.Concrete example comprises in the separation, hydrometallurgy of oil water mixture that solution separates with residue, the filtration of drinks and fruit juice, from liquid, filter bacterium and virus.
In the technology of preparing of existing ceramic filter film support, in order to obtain enough high-intensity supporters under lower sintering temperature, generally adopt and in aluminium oxide aggregate, add sub-micron or Nano grade aluminium oxide or other oxides and its esters, play the effect that improves supporter intensity, but these methods have all reduced the content of alpha-phase aluminum oxide in supporter without exception, owing to only having alpha-phase aluminum oxide (corundum) just to there is the ability of very high intensity and strong alkali-acid resistance corrosion, other γ phases, β phase alumina, or other aluminosilicates, silicate does not have the ability of high strength and strong alkali-acid resistance corrosion, and the surface area of porous ceramics is large especially, the area being corroded is large, speed is fast, therefore the ability of its intensity and acid-alkali-corrosive-resisting is inevasible has been lowered.Meanwhile, trickle powder has stopped up the gap of aggregate, causes its filtration flux to reduce.
Meanwhile, existing ceramic filter film support generally adopts extrusion moulding to prepare moulding, and its production cycle is long especially.Generally reach several weeks, this makes difficult quality control, and production cost is higher simultaneously.
In CN101139206A, having described the particle suspension liquid that adopts the aluminium oxide such as the aluminium, zirconium, titanium of ultra-fine nucleus adds to and in ceramic powder aggregate, manufactures ceramic film support as sintering aid, Ultra-fine Grained nuclear particle is filled in the gap of aggregate, high sintering activity is provided, make supporter under the lower temperature of 1100-1500 DEG C, realize sintering, reduce manufacturing cost, but this filling reduces the porosity of supporter, and its flux only has 4600-11000L.M
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-1.After preparing pug in this technology, need old 3-7 days, need again nature to dry 15-30 hour, then dry 10-72 hour after moulding, the production cycle is longer, the more difficult control of quality.
In CN101318808A, described 100 parts of emergies and 10-15 part kaolin, the sintering aids such as 8-15 part potassic feldspar have been prepared low cost, high-intensity inorganic separating film supporter together, but the ability of complete not mentioned its resistance to strong acid, alkali corrosion.
Summary of the invention
The object of the invention is in order to improve in existing ceramic filter film support production technology, the production cycle is long, supporter alpha-phase aluminum oxide content is lower makes it can not tolerate strong acid and strong base corrosion, supporter space is stopped up and is caused porosity low by fine powder, the problem that flux is low, and provide one to adopt gel casting forming, microwave drying, a small amount of alpha-phase aluminum oxide high temperature evaporation-condense under atmosphere protection forms on alpha-phase aluminum oxide aggregate that to connect having of neck with short production cycle, high flux, high strength, the preparation method of the ceramic filter film support of resistance to dense strong acid and strong base corrosion, for the filtering and impurity removing of strong acid solution in hydrometallurgy, filtration operation under the various severe corrosive environment such as the filtering and impurity removing of the strong acid electrolyte of purifying metals with electrolysis process used for non-ferrous metal.
To achieve these goals, technical scheme of the present invention is as follows:
1) crosslinking agent acrylamide, di-2-ethylhexylphosphine oxide ammonium acrylate powder are mixed according to the mass ratio of 3-15:1, be added to the water, the ratio of sum of the two and water is 1:5-20, stirs and makes it fully dissolve formation cross-linking agent aqueous solution.
2) be equipped with two kinds of pure alpha-phase aluminum oxide powder:
The alpha-alumina powder (1) of purity >=99.7%, its meta particle diameter D50 is 18-35 μ m;
The alpha-alumina powder (2) of purity >=99.8%, its meta particle diameter D50 is 0.8-2 μ m;
Wherein the consumption of alpha-alumina powder (2) is with the 2-10% of alpha-alumina powder (1) weight;
3) make aforementioned mixed-powder slowly add cross-linking agent aqueous solution, and be uniformly mixed to form suspension, the mass ratio of the aqueous solution and alpha-alumina powder (1) is 1:2.5-3.5;
4) regulate the pH scope of suspension to 3-5;
5) in suspension, add catalyst and initator, the mass ratio of catalyst and crosslinking agent total amount is 1-10:100, and the mass ratio of initator and crosslinking agent total amount is 1-5:100, mixes and make its gel casting forming in mould.
6) make 30-60 DEG C of moulded products heating using microwave dry 1-5 hour, become water content lower than 3% hard base substrate;
7) make the moulded products of oven dry calcine 3-10 hour in 400-900 DEG C of air atmosphere;
8) make to calcine goods with vacuum or atmospheric hydrogen or argon gas atmosphere, under the condition of 1800 DEG C to 1950 DEG C, be incubated 3-15 hour, at this temperature, thin alumina powder constantly evaporate and condense between meal contact point, form neck, finally form the supporter of pure alpha-phase aluminum oxide ceramic filter membrane.The time of heat preservation sintering determines according to particle diameter and the addition of alumina powder (2), particle diameter is larger, addition more at most the heat preservation sintering time longer, temperature retention time is shorter on the contrary.
In the present invention, as the alpha-phase aluminum oxide powder (1) in component, can adopt purity >=99.7% alpha alumina particles of 18-35 micron, be preferably the alumina particle of 25-30 micron.Alpha-phase aluminum oxide powder (2) can adopt the alumina particle of purity >=99.8% of particle diameter 0.8-2 μ m, is preferably the alumina particle of 0.8-1.2 μ m.But the present invention does not adopt thinner alumina powder, because in the time that diameter of particle D50 is below 0.6 μ m, in the time not reaching 1800 DEG C, will self sintering form the bulky grain of 5-10 μ m, reduce on the contrary its evaporation rate, sintering time is extended.
In the present invention, in order to prevent that aluminium oxide from high temperature forming aluminium nitride with nitrogen and polluting supporter, the present invention adopts hydrogen or argon gas or vacuum in atmosphere protection, and does not adopt more cheap nitrogen.
In the present invention, step 2) in, the mass ratio of crosslinking agent and water is preferably 1:8-12, and in crosslinking agent, the mass ratio of acrylamide and di-2-ethylhexylphosphine oxide ammonium acrylate is preferably 4.5-10:1.
The pH value of suspension is preferably adjusted to 3.5-4.5.
Catalyst is preferably tetramethylethylenediamine, and the mass ratio of its quality and crosslinking agent acrylamide, di-2-ethylhexylphosphine oxide ammonium acrylate is 1-10:100, and initator is preferably ammonium persulfate, and the mass ratio of its quality and crosslinking agent is 1-5:100.
The moulded products of gel injection-moulding uses heating using microwave to be preferably 40-55 DEG C and dries 1-3 hour.
The moulded products of drying is preferably in 500-800 DEG C of air atmosphere calcines 4-8 hour.
When sintering, be preferably under the condition of 1800 DEG C to 1950 DEG C and be incubated 4-12 hour.
Compare with background technology, advantage of the present invention is as follows:
1/ shortens dramatically the production cycle of ceramic filter film support, the moulding drying course that reaches several weeks with extrusion moulding is compared, product of the present invention is configured to suspension gel casting forming within a few hours, within a few hours, dry again, in 8 hours, can complete the moulding drying course of product.This has not only improved production efficiency, and succinct flow process also can increase substantially product percent of pass, reduces costs.
2/ the present invention adopts can resistance to dense strong acid, the unique composition material of high-purity alpha-phase aluminum oxide of alkali corrosion, the at high temperature constantly melting of surface of the convex surface of alpha-phase aluminum oxide, evaporation under high-temperature vacuum or hydrogen or argon gas atmosphere, then condense in thick alumina powder and connect neck, again form pure alpha-aluminium oxide phase crystal structure.According to kelvin's law, radius of curvature is less, and surperficial saturated vapor pressure is higher, and evaporation rate is faster.Therefore thin alpha-phase aluminum oxide because of its radius of curvature little, evaporation rate, just far away higher than meal, can be evaporated and is agglomerated to meal completely and be connected neck in specific temperature and time.Like this, the supporter that sintering completes only has meal to exist, and its porosity will be far above the mode that adopts fine powder bonding meal, and meanwhile, because fine powder disappears, the tortuosity in its duct is less than the structure that thickness powder mixes, and fluid circulating resistance is little.Under high porosity, low hole tortuosity, its filtration flux can greatly increase.In an embodiment of the present invention, reached respectively 17000,26000,31000L.M
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-1much larger than 4600-11000L.M in background technology
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3, by the present invention, ceramic film support is made up of pure alpha-phase aluminum oxide, there is not the middle phase of aluminium oxide in the sintered neck between aggregate powder particularly, or other materials such as aluminosilicate, silicate, be entirely alpha-phase aluminum oxide and exist, its intensity, corrosion resistance have very large raising by contrast.Therefore whole supporter will possess the ability of alpha-phase aluminum oxide high strength, the corrosion of high strong alkali-acid resistance, thereby can in various dense strong acid, highly basic, strong corrosive environment, use and the breakage that is not corroded the visible each embodiment of its anti-corrosive parameters for a long time.
Detailed description of the invention
Embodiment mono-
Acrylamide 165g and di-2-ethylhexylphosphine oxide ammonium acrylate 35g are slowly added in 1800g pure water, stir and it is dissolved completely, form the aqueous solution, be that the alpha-phase aluminum oxide 5kg of 18 microns and D50 are that the alpha-phase aluminum oxide 0.1kg of 0.8 micron slowly adds in the above-mentioned aqueous solution and stirs by D50, form the suspension of aluminium oxide, with nitric acid adjusting pH value to 3.8,2g tetramethylethylenediamine and 2g ammonium persulfate are dissolved in 20g water, slowly add again above-mentioned suspension, stir.Afterwards suspension is injected to multichannel mould, leave standstill 60 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the cellular green compact of diameter 4mm, base substrate is put into microwave drying oven, at 40 DEG C, dry 1 hour, at 50 DEG C, dry 2 hours, again the green compact of oven dry are placed in to atmosphere furnace and are slowly heated to 600 DEG C and be incubated 5 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, under 1800 DEG C of conditions, be incubated 4 hours, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 54%, average pore size is 9 μ m, pure water flux is 17000L.M
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-1, 3 rupture strengths reach 5800N, supporter are immersed in 98% sulfuric acid and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate is all≤1% for its mass loss rate.Supporter is immersed in 30% sodium hydrate aqueous solution and is heated to 100 DEG C, soak respectively 24,120,240 hours, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Embodiment bis-
Acrylamide 180g and di-2-ethylhexylphosphine oxide ammonium acrylate 20g are slowly added in 1500g pure water, stir and it is dissolved completely, form the aqueous solution, be that the alpha-phase aluminum oxide 5kg of 25 microns and D50 are that the alpha-phase aluminum oxide 0.25kg of 1.2 microns slowly adds in the above-mentioned aqueous solution and stirs by D50, form the suspension of aluminium oxide, with nitric acid adjusting pH value to 4.1,5g tetramethylethylenediamine and 3g ammonium persulfate are dissolved in 200g water, slowly add again above-mentioned suspension, stir.Afterwards suspension is injected to multichannel mould, leave standstill 25 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the cellular green compact of diameter 4mm, base substrate is put into microwave drying oven, at 40 DEG C, dry 1 hour, at 55 DEG C, dry 1 hour, again the green compact of oven dry are placed in to atmosphere furnace and are slowly heated to 600 DEG C and be incubated 4 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, under 1850 DEG C of conditions, be incubated 12 hours, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 56%, average pore size is 11 μ m, pure water flux is 24000L.M
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-1, 3 rupture strengths reach 6700N, supporter are immersed in 98% sulfuric acid and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate is all≤1% for its mass loss rate.Supporter is immersed in 30% sodium hydrate aqueous solution and is heated to 100 DEG C, soak respectively 24,120,240 hours, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Embodiment tri-
Acrylamide 170g and di-2-ethylhexylphosphine oxide ammonium acrylate 30g are slowly added in 2000g pure water, stir and it is dissolved completely, form the aqueous solution, be that the alpha-phase aluminum oxide 5kg of 35 microns and D50 are that the alpha-phase aluminum oxide 0.5kg of 2 microns slowly adds in the above-mentioned aqueous solution and stirs by D50, form the suspension of aluminium oxide, with nitric acid adjusting pH value to 4.5,20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add again above-mentioned suspension, stir.Afterwards suspension is injected to multichannel mould, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the cellular green compact of diameter 4mm, base substrate is put into microwave drying oven, at 40 DEG C, dry 1 hour, at 55 DEG C, dry 2 hours, again the green compact of oven dry are placed in to atmosphere furnace and are slowly heated to 550 DEG C and be incubated 6 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, under 1950 DEG C of conditions, be incubated 12 hours, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 59%, average pore size is 15 μ m, pure water flux is 33000L.M
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-1, 3 rupture strengths reach 6100N, supporter are immersed in 98% sulfuric acid and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate is all≤1% for its mass loss rate.Supporter is immersed in 30% sodium hydrate aqueous solution and is heated to 100 DEG C, soak respectively 24,120,240 hours, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Comparative example one
Acrylamide 170g and di-2-ethylhexylphosphine oxide ammonium acrylate 30g are slowly added in 2000g pure water, stir and it is dissolved completely, form the aqueous solution, be that the alpha-phase aluminum oxide 5kg of 25 microns and D50 are that the alpha-phase aluminum oxide 0.25kg of 0.3 micron slowly adds in the above-mentioned aqueous solution and stirs by D50, form the suspension of aluminium oxide, with nitric acid adjusting pH value to 4.5,20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add again above-mentioned suspension, stir.Afterwards suspension is injected to multichannel mould, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the cellular green compact of diameter 4mm, base substrate is put into microwave drying oven, at 40 DEG C, dry 1 hour, at 55 DEG C, dry 2 hours, again the green compact of oven dry are placed in to atmosphere furnace and are slowly heated to 550 DEG C and be incubated 6 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, under 1850 DEG C of conditions, be incubated 4 hours, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 42%, average pore size is 10 μ m, pure water flux is 12000L.M
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-1, 3 rupture strengths reach 2700N, supporter are immersed in 98% sulfuric acid and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate is all≤1% for its mass loss rate.Supporter is immersed in 30% sodium hydrate aqueous solution and is heated to 100 DEG C, soak respectively 24,120,240 hours, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Comparative example two
Acrylamide 170g and di-2-ethylhexylphosphine oxide ammonium acrylate 30g are slowly added in 2000g pure water, stir and it is dissolved completely, form the aqueous solution, be that the alpha-phase aluminum oxide 5kg of 25 microns and D50 are that the nano aluminium oxide 0.500kg of 0.05 micron slowly adds in the above-mentioned aqueous solution and stirs by D50, form the suspension of aluminium oxide, with nitric acid adjusting pH value to 4.5,20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add again above-mentioned suspension, stir.Afterwards suspension is injected to multichannel mould, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the cellular green compact of diameter 4mm, put into microwave drying oven by base substrate, dry 1 hour at 40 DEG C, at 55 DEG C, dry 2 hours, again the green compact of oven dry are placed in to air furnace sintering, sintering temperature is 1500 DEG C, temperature retention time 4 hours.Afterwards, recording its porosity is 37%, and average pore size is 8 μ m, and pure water flux is 8400L.M
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-13 rupture strengths reach 5700N, supporter are immersed in 98% sulfuric acid and are heated to 100 DEG C, continue 24,120,240 hours respectively, its mass loss rate is respectively≤and 0.5%, 1.2%, 1.7%, its loss of strength rate is respectively≤and 44%, 62%, 79%.Supporter is immersed in 30% sodium hydrate aqueous solution and is heated to 100 DEG C, soak respectively 24,120,240 hours, its mass loss rate is respectively≤0.5%, 1.1%, 1.4%, and its loss of strength rate is respectively≤and 42%, 57%, 71%.
Claims (9)
1. a preparation method for ceramic film support, the method comprises the following steps:
1) crosslinking agent acrylamide and di-2-ethylhexylphosphine oxide ammonium acrylate powder are mixed according to the mass ratio of 3-15:1, be added to the water, the ratio of sum of the two and water is 1:5-20, stirs and makes it fully dissolve formation cross-linking agent aqueous solution;
2) be equipped with raw material, wherein raw material comprises mixed-powder, contains:
The alpha-alumina powder (1) of purity >=99.7%, its meta particle diameter D50 is 18-35 μ m;
The alpha-alumina powder (2) of purity >=99.8%, its meta particle diameter D50 is 0.8-2 μ m;
Wherein the consumption of alpha-alumina powder (2) is the 2-10% of alpha-alumina powder (1) weight;
3) making aforementioned mixed-powder and step 1) cross-linking agent aqueous solution is uniformly mixed to form suspension, and the mass ratio of cross-linking agent aqueous solution and alpha-alumina powder (1) is 1:2.5-3.5;
4) regulate the pH scope of suspension to 3-5;
5) in suspension, add catalyst and initator, the mass ratio of catalyst and crosslinking agent total amount is 1-10:100, and the mass ratio of initator and crosslinking agent total amount is 1-5:100, mixes and make its gel casting forming in mould;
6) make 30-60 DEG C of moulded products heating using microwave dry 1-5 hour;
7) make the moulded products of oven dry calcine 3-10 hour in 400-900 DEG C of air atmosphere;
8) make to calcine goods with vacuum or atmospheric hydrogen or argon gas atmosphere, under the condition of 1800 DEG C to 1950 DEG C, be incubated 3-15 hour, become the supporter of pure alpha-phase aluminum oxide ceramic filter membrane.
2. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: alpha-alumina powder (1), its meta particle diameter D50 is 20-25 μ m.
3. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: alpha-alumina powder (2), its meta particle diameter D50 is 0.8-1.2 μ m.
4. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: step 2) in, the mass ratio of crosslinking agent and water is 1:8-12, in crosslinking agent, the mass ratio of acrylamide and di-2-ethylhexylphosphine oxide ammonium acrylate is 4.5-10:1.
5. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: the pH value of suspension nitric acid or acetic acid or hydrochloric acid are adjusted to 3.5-4.5.
6. the preparation method of a kind of ceramic film support as claimed in claim 1, it is characterized in that: catalyst is tetramethylethylenediamine, the mass ratio of its quality and crosslinking agent acrylamide, di-2-ethylhexylphosphine oxide ammonium acrylate is 1-10:100, initator is ammonium persulfate, and the mass ratio of its quality and crosslinking agent is 1-5:100.
7. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: the moulded products of gel injection-moulding uses 40-55 DEG C of heating using microwave to dry 1-3 hour.
8. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: the moulded products of oven dry is calcined 4-8 hour in 500-800 DEG C of air atmosphere.
9. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: under the condition of 1800 DEG C to 1950 DEG C, be incubated 4-12 hour.
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| CN105565785B (en) * | 2015-12-25 | 2016-08-17 | 山东硅元新型材料有限责任公司 | The preparation method of ceramic film support |
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| CN109851328A (en) * | 2019-02-15 | 2019-06-07 | 江苏埃梯恩膜过滤技术有限公司 | A kind of preparation process of high-performance ceramic flat membrane support |
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