CN104014252B - A kind of preparation method of ceramic film support - Google Patents
A kind of preparation method of ceramic film support Download PDFInfo
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- CN104014252B CN104014252B CN201410187930.2A CN201410187930A CN104014252B CN 104014252 B CN104014252 B CN 104014252B CN 201410187930 A CN201410187930 A CN 201410187930A CN 104014252 B CN104014252 B CN 104014252B
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Abstract
The invention discloses a kind of preparation method of ceramic filter film support, the method comprises the following steps: (1) is equipped with raw material, wherein raw material comprises mixed-powder, contains: the alpha-alumina powder (1) of purity >=99.7%, and its median D50 is 18-35 μm; The alpha-alumina powder (2) of purity >=99.8%, its median D50 is 0.8-2 μm; Wherein the consumption of alpha-alumina powder (2) is with the 2-10% of alpha-alumina powder (1) (weight); (2) make aforementioned mixed-powder and crosslinking agent acrylamide, methylene bisacrylamide acid ammonium aqueous solution to form suspension; Make suspension gel casting forming; Moulded products heating using microwave 40-55 DEG C is made to dry 1-3 hour; The moulded products of oven dry is made to calcine 4-8 hour in 500-800 DEG C of air atmosphere; Make calcining goods with vacuum or atmospheric hydrogen or argon gas atmosphere, under the condition of 1800 DEG C to 1950 DEG C, be incubated 4-12 hour, become the supporter of pure alpha-phase aluminum oxide ceramic filter membrane.Product porosity of the present invention is high, flux is high and resistance to strong acid, alkali corrosion.
Description
Technical field
The present invention relates to the preparation method of ceramic membrane filter supporter, belong to porous ceramics preparation field.
Background technology
In UF membrane field, inoranic membrane is widely used in the micro-filtration of liquid medium and ultrafiltration and gas separaion.
The inoranic membrane that inorganic material is made on supporter may be used for filtration in environment-industry, metallurgical industry, food_beverage industry, biological industry, chemical industry, petro chemical industry and is separated application.Concrete example comprises that solution in the separation of oil water mixture, hydrometallurgy is separated with residue, the filtration of drinks and fruit juice, filter bacteria and virus from liquid.
In the technology of preparing of existing ceramic filter film support, in order to obtain the supporter of enough high strength at a relatively low sintering temperature, sub-micron or Nano grade aluminium oxide or other oxides and its esters are added in general employing in aluminium oxide aggregate, play the effect improving supporter intensity, but these methods all reduce the content of alpha-phase aluminum oxide in supporter without exception, the ability that owing to only having alpha-phase aluminum oxide (corundum), just there is very high intensity and strong alkali-acid resistance and corrode, 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 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 plugs the gap of aggregate, causes its filtration flux to reduce.
Meanwhile, it is shaping that existing ceramic filter film support generally adopts extrusion moulding to prepare, and its production cycle is long especially.Generally reach several weeks, this makes difficult quality control, and production cost is higher simultaneously.
Describe in CN101139206A and adopt the particle suspension liquid of the aluminium oxide such as aluminium, zirconium, titanium of ultra-fine nucleus to add in ceramic powder aggregate as sintering aid to manufacture ceramic film support, Ultra-fine Grained nuclear particle is filled in the gap of aggregate, provide high sintering activity, make supporter can realize sintering under the lower temperature of 1100-1500 DEG C, reduce manufacturing cost, but this filling makes the porosity of supporter reduce, and its flux only has 4600-11000L.M
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-1.Need old 3-7 days after preparing pug in this technology, need again nature to dry 15-30 hour after shaping, then dry 10-72 hour, the production cycle is longer, the more difficult control of quality.
Describe 100 parts of emergies and 10-15 part kaolin in CN101318808A, the sintering aids such as 8-15 part potassic feldspar have prepared the inorganic separating film supporter of low cost, high strength together, but the ability of its resistance to strong acid completely not mentioned, alkali corrosion.
Summary of the invention
The object of the invention is 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 caused porosity low by fine powder blocking, the problem that flux is low, and a kind of gel casting forming that adopts is provided, microwave drying, it is with short production cycle that a small amount of alpha-phase aluminum oxide high temperature evaporation-condense under atmosphere protection alpha-phase aluminum oxide aggregate is formed having of connecting neck portion, 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, methylene bisacrylamide acid ammonium 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) two kinds of pure alpha-phase aluminum oxide powder are equipped with:
The alpha-alumina powder (1) of purity >=99.7%, its median D50 is 18-35 μm;
The alpha-alumina powder (2) of purity >=99.8%, its median D50 is 0.8-2 μm;
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 makes its gel casting forming in a mold.
6) make moulded products heating using microwave 30-60 DEG C dry 1-5 hour, become water content lower than 3% hard base substrate;
7) moulded products of oven dry is made to calcine 3-10 hour in 400-900 DEG C of air atmosphere;
8) make calcining goods with vacuum or atmospheric hydrogen or argon gas atmosphere, 3-15 hour is incubated under the condition of 1800 DEG C to 1950 DEG C, 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 the particle diameter of alumina powder (2) and addition, particle diameter is larger, addition more at most the heat preservation sintering time longer, then temperature retention time is shorter on the contrary.
In the present invention, as the alpha-phase aluminum oxide powder (1) in component, purity >=99.7% alpha alumina particles of 18-35 micron can be adopted, 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 μm, is preferably the alumina particle of 0.8-1.2 μm.But the present invention does not adopt thinner alumina powder, because when diameter of particle D50 is below 0.6 μm, when not reaching 1800 DEG C, self will sinter the bulky grain forming 5-10 μm, reducing its evaporation rate on the contrary, sintering time is extended.
In the present invention, at high temperature form aluminium nitride with nitrogen pollute supporter to prevent aluminium oxide, 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 methylene bisacrylamide acid ammonium 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, methylene bisacrylamide acid ammonium 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.
During sintering, preferably under the condition of 1800 DEG C to 1950 DEG C, be incubated 4-12 hour.
Compare with background technology, advantage of the present invention is as follows:
1/ makes the production cycle of ceramic filter film support shorten dramatically, the shaping drying course reaching several weeks with extrusion moulding is compared, product of the present invention is configured to suspension and gel casting forming within a few hours, dry within a few hours again, the shaping drying course of product in 8 hours, can be completed.This not only increases production efficiency, and succinct flow process also can increase substantially product percent of pass, reduces costs.
2/ the present invention adopt can resistance to dense strong acid, alkali corrosion the unique composition material of high-purity alpha-phase aluminum oxide, the at high temperature surface constantly melting 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 connecting neck portion, 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 completely and is agglomerated to meal connecting neck portion in specific temperature and time.Like this, the supporter sintered only has meal to exist, and its porosity will far above the mode adopting fine powder bonding meal, and meanwhile, because fine powder disappears, the tortuosity in its duct is less than the structure of thickness powder mixing, and fluid passage resistance is little.Under high porosity, low hole tortuosity, its filtration flux can greatly increase.In an embodiment of the present invention, reach 17000 respectively, 26000,31000L.M
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-14600-11000L.M in background technology
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3, the present invention is passed through, ceramic film support is made up of pure alpha-phase aluminum oxide, there is not the mesophase spherule of aluminium oxide in the sintered neck particularly between aggregate powder, or other materials such as aluminosilicate, silicate, be entirely alpha-phase aluminum oxide to 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, thus can use and the breakage that is not corroded for a long time in various dense strong acid, highly basic, strong corrosive environment, the visible each embodiment of its anti-corrosive parameters.
Detailed description of the invention
Embodiment one
Acrylamide 165g and methylene bisacrylamide acid ammonium 35g is slowly added in 1800g pure water, stir and make it dissolve completely, form the aqueous solution, to be alpha-phase aluminum oxide 5kg and D50 of 18 microns by D50 be is that the alpha-phase aluminum oxide 0.1kg of 0.8 micron slowly adds in the above-mentioned aqueous solution and stirs, form the suspension of aluminium oxide, regulate pH value to 3.8 with nitric acid, 2g tetramethylethylenediamine and 2g ammonium persulfate are dissolved in 20g water, slowly add above-mentioned suspension again, stir.Afterwards suspension is injected multi-channel die, leave standstill 60 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the honeycomb green of diameter 4mm, base substrate is put into microwave drying oven, dry 1 hour at 40 DEG C, dry 2 hours at 50 DEG C, again the green compact of oven dry are placed in atmosphere furnace be slowly heated to 600 DEG C and be incubated 5 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, 4 hours are incubated under 1800 DEG C of conditions, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 54%, average pore size is 9 μm, pure water flux is 17000L.M
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-1, 3 rupture strengths reach 5800N, are immersed in by supporter in the sulfuric acid of 98% and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.Be immersed in by supporter in the sodium hydrate aqueous solution of 30% and be heated to 100 DEG C, soak 24,120,240 hours respectively, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Embodiment two
Acrylamide 180g and methylene bisacrylamide acid ammonium 20g is slowly added in 1500g pure water, stir and make it dissolve completely, form the aqueous solution, to be alpha-phase aluminum oxide 5kg and D50 of 25 microns by D50 be is that the alpha-phase aluminum oxide 0.25kg of 1.2 microns slowly adds in the above-mentioned aqueous solution and stirs, form the suspension of aluminium oxide, regulate pH value to 4.1 with nitric acid, 5g tetramethylethylenediamine and 3g ammonium persulfate are dissolved in 200g water, slowly add above-mentioned suspension again, stir.Afterwards suspension is injected multi-channel die, leave standstill 25 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the honeycomb green of diameter 4mm, base substrate is put into microwave drying oven, dry 1 hour at 40 DEG C, dry 1 hour at 55 DEG C, again the green compact of oven dry are placed in atmosphere furnace be slowly heated to 600 DEG C and be incubated 4 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, 12 hours are incubated under 1850 DEG C of conditions, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 56%, average pore size is 11 μm, pure water flux is 24000L.M
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-1, 3 rupture strengths reach 6700N, are immersed in by supporter in the sulfuric acid of 98% and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.Be immersed in by supporter in the sodium hydrate aqueous solution of 30% and be heated to 100 DEG C, soak 24,120,240 hours respectively, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Embodiment three
Acrylamide 170g and methylene bisacrylamide acid ammonium 30g is slowly added in 2000g pure water, stir and make it dissolve completely, form the aqueous solution, to be alpha-phase aluminum oxide 5kg and D50 of 35 microns by D50 be is that the alpha-phase aluminum oxide 0.5kg of 2 microns slowly adds in the above-mentioned aqueous solution and stirs, form the suspension of aluminium oxide, regulate pH value to 4.5 with nitric acid, 20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add above-mentioned suspension again, stir.Afterwards suspension is injected multi-channel die, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the honeycomb green of diameter 4mm, base substrate is put into microwave drying oven, dry 1 hour at 40 DEG C, dry 2 hours at 55 DEG C, again the green compact of oven dry are placed in atmosphere furnace be slowly heated to 550 DEG C and be incubated 6 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, 12 hours are incubated under 1950 DEG C of conditions, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 59%, average pore size is 15 μm, pure water flux is 33000L.M
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-1, 3 rupture strengths reach 6100N, are immersed in by supporter in the sulfuric acid of 98% and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.Be immersed in by supporter in the sodium hydrate aqueous solution of 30% and be heated to 100 DEG C, soak 24,120,240 hours respectively, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Comparative example one
Acrylamide 170g and methylene bisacrylamide acid ammonium 30g is slowly added in 2000g pure water, stir and make it dissolve completely, form the aqueous solution, to be alpha-phase aluminum oxide 5kg and D50 of 25 microns by D50 be is that the alpha-phase aluminum oxide 0.25kg of 0.3 micron slowly adds in the above-mentioned aqueous solution and stirs, form the suspension of aluminium oxide, regulate pH value to 4.5 with nitric acid, 20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add above-mentioned suspension again, stir.Afterwards suspension is injected multi-channel die, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the honeycomb green of diameter 4mm, base substrate is put into microwave drying oven, dry 1 hour at 40 DEG C, dry 2 hours at 55 DEG C, again the green compact of oven dry are placed in atmosphere furnace be slowly heated to 550 DEG C and be incubated 6 hours and pass into air, complete deaeration more afterwards, be filled with hydrogen, 4 hours are incubated under 1850 DEG C of conditions, obtain pure alpha-phase aluminum oxide supporter, recording its porosity is 42%, average pore size is 10 μm, pure water flux is 12000L.M
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-1, 3 rupture strengths reach 2700N, are immersed in by supporter in the sulfuric acid of 98% and are heated to 100 DEG C, continue 24,120,240 hours respectively, and all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.Be immersed in by supporter in the sodium hydrate aqueous solution of 30% and be heated to 100 DEG C, soak 24,120,240 hours respectively, all≤0.01%, its loss of strength rate all≤1% for its mass loss rate.
Comparative example two
Acrylamide 170g and methylene bisacrylamide acid ammonium 30g is slowly added in 2000g pure water, stir and make it dissolve completely, form the aqueous solution, to be alpha-phase aluminum oxide 5kg and D50 of 25 microns by D50 be, and the nano aluminium oxide 0.500kg of 0.05 micron slowly adds in the above-mentioned aqueous solution stirs, form the suspension of aluminium oxide, regulate pH value to 4.5 with nitric acid, 20g tetramethylethylenediamine and 5g ammonium persulfate are dissolved in 400g water, slowly add above-mentioned suspension again, stir.Afterwards suspension is injected multi-channel die, leave standstill 20 minutes after its gel, take out mould, prepare diameter 30mm, inner 19 passages, the honeycomb green of diameter 4mm, puts into microwave drying oven by base substrate, dries 1 hour at 40 DEG C, dry 2 hours at 55 DEG C, again the green compact of oven dry are placed in air furnace to sinter, sintering temperature is 1500 DEG C, temperature retention time 4 hours.Afterwards, recording its porosity is 37%, and average pore size is 8 μm, and pure water flux is 8400L.M
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-13 rupture strengths reach 5700N, are immersed in by supporter in the sulfuric acid of 98% 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%.Be immersed in by supporter in the sodium hydrate aqueous solution of 30% and be heated to 100 DEG C, soak 24,120,240 hours respectively, 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 methylene bisacrylamide acid ammonium 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 one of purity >=99.7%, its median D50 is 18-35 μm;
The alpha-alumina powder two of purity >=99.8%, its median D50 is 0.8-2 μm;
Wherein the consumption of alpha-alumina powder two is the 2-10% of alpha-alumina powder one weight;
3) aforementioned mixed-powder and step 1 is made) 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 one 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 makes its gel casting forming in a mold;
6) moulded products heating using microwave 30-60 DEG C is made to dry 1-5 hour;
7) moulded products of oven dry is made to calcine 3-10 hour in 400-900 DEG C of air atmosphere;
8) make calcining 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 one, and its median D50 is 20-25 μm.
3. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: alpha-alumina powder two, and its median D50 is 0.8-1.2 μm.
4. the preparation method of a kind of ceramic film support as claimed in claim 1, is characterized in that: step 1) in, the mass ratio of crosslinking agent and water is 1:8-12, and in crosslinking agent, the mass ratio of acrylamide and methylene bisacrylamide acid ammonium 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 nitric acid of suspension 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 is 1-10:100, and 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 heating using microwave 40-55 DEG C 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 calcines 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: step 8) calcining goods under the condition of 1800 DEG C to 1950 DEG C, be incubated 4-12 hour.
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