CN102923744A - Preparation method for aluminum oxide by direct forming method - Google Patents
Preparation method for aluminum oxide by direct forming method Download PDFInfo
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- CN102923744A CN102923744A CN2012104736284A CN201210473628A CN102923744A CN 102923744 A CN102923744 A CN 102923744A CN 2012104736284 A CN2012104736284 A CN 2012104736284A CN 201210473628 A CN201210473628 A CN 201210473628A CN 102923744 A CN102923744 A CN 102923744A
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Abstract
The invention discloses a preparation method for aluminum oxide by a direct forming method. The method is characterized in that the aluminum oxide is directly formed by a wet filter cake, wherein pore volume is 0.3-0.8ml/g; a specific surface area is 150-300 m<2>/g; and crushing strength is 30-120 N/particle; the preparation process comprises the steps: a) meta-aluminate containing aluminum or a strong acid salt compound is neutralized with a precipitator solution at a temperature of 30-80 DEG C and pH of 6-9; accessory ingredient is added in a neutralizing process; mixture is aged for at least 10min after neutralizing; b) prepared aluminium hydroxide gel is washed by de-ionized water for 4-10 times; dosage of the de-ionized water for each time is 10-40 times of mass of a dried substrate of prepared aluminium hydroxide; a hydrated alumina filter cake is obtained after washing and filtering; content of the aluminium hydroxide in the filter cake is controlled to be 5-50%; and c) the accessory ingredient is added into one or various liquid in the step a) and step b); the filter cake after washing is formed by a normal forming method; and the formed filter cake is dried at a temperature of 80-120 DEG C and calcined at a temperature of 450-1000 DEG C to obtain a finished product of the aluminum oxide.
Description
Technical field
The present invention relates to the preparation method of aluminum oxide, is directly to utilize the filter cake that obtains after aluminum oxide neutralization precipitation, the aging and washing directly to carry out the preparation method of the aluminum oxide of moulding specifically.
Background technology
Aluminum oxide has flourishing hole and good thermostability, is very widely inorganic oxide of a kind of industrial application, can be used for siccative, sorbent material and support of the catalyst, also can be used as catalyzer and uses separately.Aluminum oxide is during as catalyzer or its carrier, and its character plays very important effect to the performance of whole catalyzer.The degree of crystallinity of general requirement aluminum oxide should be higher, and the content of foreign ion should be lower.The aluminum oxide that forms after roasting should have suitable specific surface area, higher intensity and moderate pore volume.
The preparation process of aluminum oxide generally prepares first its presoma-pseudo-boehmite, and then moulding is carried out high-temperature roasting again and made it the crystalline phase conversion.In the various methods that openly prepare pseudo-boehmite, its master operation is the raw material preparation, becomes glue, aging, and washing, solid-liquid separation obtain filter cake, and filtration cakes torrefaction is pulverized, and then the step such as aluminium hydrate powder is body formed, roasting is made the aluminum oxide finished product.The CN1088397C patent disclosure a kind of preparation method of aluminum oxide, comprise a kind of aluminum contained compound solution is contacted with a kind of precipitant solution, obtain containing the slurries of aluminium hydroxide, filtration, washing obtain filter cake, and the alumina supporter that is suitable as heavy-oil hydrogenation catalyst is prepared in drying, pulverizing, moulding.The disclosed production technique of CN1057443A comprises by pass into sour gas in sodium aluminate solution carries out neutralization reaction, obtains pseudo-boehmite through overaging, washing, solid-liquid separation and drying and other steps, and then makes aluminum oxide.CN1762579A discloses a kind of large pore capacity, high specific surface area alumina preparation method, with water, Organic Alcohol, a kind of as solvent in the aqueous solution of the organic solvent that perhaps dissolves each other with water, aluminium salt and cyclodextrin are dissolved in wherein, be made into mixing solutions, the concentration of cyclodextrin is 0.005-1.6mol/L in the mixing solutions, and the aluminium salt concn is counted 0.1-3.0mol/L with aluminium.Add in the mixing solutions alkaline solution to pH value more than or equal to 6, pass through again the aluminum oxide that the steps such as deionized water washing, drying, pulverizing, moulding are prepared.
If filter cake is drying, pulverizing and then forming step not, also need to carry out moulding by other the form such as spraying drying.A kind of preparation method of particulate alumina in US4371513 is open.Precipitated alumina under the condition of the reactant concn, temperature of reaction, time and the pH that control, and under high pH value, filter, filter cake obtains the pseudo-boehmite particle with spray-dired form after washing, then carry out roasting and obtain alumina particle.CN1068975A discloses the preparation method of low density, large pore volume, high-strength alumina carrier, obtain pseudo-boehmite with aluminium salt or aluminate through neutralization, add peptizing agent and alumina powder,, roasting aging, dry through forming oil column prepares specific surface area 120-280m
2/ g, bulk density are 0.18-0.35g/cm
3, pore volume is 1.5-2.0cm
3//g, crushing strength is the 0.5-3.0kgf/ grain.The method in and need to have carbanion auxiliary in the preparation process, and to add the aluminum oxide powder through roasting, the minimum 0.5kgf/ of the only having grain of the aluminum oxide intensity of preparing, actual application value is little.
Summary of the invention
It is complicated to the objective of the invention is to overcome existing alumina preparation technology, reduces drying process in the preparation process, provides a kind of and new can reduce the alumina preparation method that energy consumption can be enhanced productivity again.
The present invention is a kind of preparation method of straight forming aluminum oxide, it is characterized in that:
For directly carrying out moulding by wet filter cake, its pore volume is 0.3～0.8ml/g, and specific surface area is 150～300m
2/ g, crushing strength is 30～120N/ grain; Preparation process is:
A) a kind of Aluminum Compounds solution and a kind of precipitant solution of containing be 30～80 ℃ of temperature, and the pH value is to neutralize under 6～9 the condition, adds auxiliary agent in the N-process, neutralizes complete aging at least 10 minutes;
B) with deionized water the aluminum hydroxide gel for preparing is carried out 4～10 washings, each washing deionized water consumption is 10～40 times of prepared aluminium hydroxide butt quality, obtain the hydrated alumina wet cake behind the washing filtering, the middle aluminium hydroxide content of control filter cake is 5%～50%;
C) add auxiliary agent in one or more liquid in step a) and step b); The filter cake that washing finishes to obtain obtains finished product according to conventional forming method moulding in 80-120 ℃ of drying, a 450-1000 ℃ calcining.
According to preparation method of the present invention, it is characterized in that aluminum contained compound is selected from one or more in the alkali-metal meta-aluminate, or in the strong acid salt of aluminium one or more; Described precipitation agent refers to can generate in the material of aluminum hydroxide precipitation one or more with the reaction of described aluminum contained compound.
According to preparation method of the present invention, it is characterized in that; When described aluminum contained compound was selected from sodium metaaluminate, potassium metaaluminate or their mixture, then corresponding described precipitation agent was selected from and is Tai-Ace S 150, aluminum nitrate, aluminum chloride, sulfuric acid, nitric acid, hydrochloric acid or their mixture; When described aluminum contained compound was selected from as Tai-Ace S 150, aluminum nitrate, aluminum chloride or their mixture, then corresponding described precipitation agent was selected from sodium hydroxide, potassium hydroxide, yellow soda ash, ammoniacal liquor, sodium metaaluminate.
According to preparation method of the present invention, it is characterized in that the auxiliary agent that adds in the N-process is gained alumina amount 0.1～55%.Described auxiliary agent is selected from water-soluble inorganic salt and water miscible organism, wherein water miscible inorganic salt are selected from one or more in volatile salt, ammonium phosphate, the bicarbonate of ammonia, and water miscible organism or organic acid salt are selected from one or more in ethanol, propyl alcohol, butanols, polyoxyethylene glycol, poly-propyl alcohol, oxyethane, polyacrylamide, polyvinyl alcohol, methylcellulose gum, sodium stearate, the potassium stearate.
According to preparation method of the present invention, it is characterized in that the sour dispersion index of the hydrated alumina filter cake of preparing is 30%～100%.
Alumina preparation method of the present invention comprises that the solution with a kind of aluminum contained compound contacts with a kind of precipitation agent and carries out acid-base neutralisation, obtains containing the slurries of aluminium hydroxide, obtains filter cake through filtration washing, directly uses the filter cake moulding, then carries out drying, roasting.Wherein, described neutralization reaction is 30～80 ℃ in temperature, carries out under the condition of pH6～9, and neutralizing complete and filtering has a weathering process before, and aging temperature is 30～80 ℃, aging pH8～10, digestion time at least 10 minutes.
In whole N-process, comprise several liquid, stock liquid before namely neutralizing, stock liquid generally comprises the slurries that contain aluminium hydroxide in a kind of alkaline liquid and a kind of acidic liquid, the N-process, the temperature of these slurries and pH value enter the slurries that contain aluminium hydroxide of aging step after finishing for the index, the neutralization that need control, and the temperature of these slurries and pH are for needing the index of control.Need in the present invention in above-mentioned at least a liquid, to sneak into the water-soluble additive that will prepare alumina amount 0.1～55%.
In the method provided by the invention, the solution of described aluminum contained compound is under agitation the two to be joined in the container simultaneously with certain separately speed with contacting of precipitation agent, so that the two mixed occurrence reaction, also can be under agitation the two to be joined in the container that fills deionized water simultaneously with certain separately speed, so that the two mixed occurrence reaction.Adjust the adding speed of aluminum contained compound solution and precipitation agent, so that mixed slurry pH value remains at 6～9, preferred 7.0～8.8.
According to method provided by the invention, described aluminum contained compound be water-soluble one or more, one or more in the meta-aluminate of preferred as alkali, or in the strong acid salt of aluminium one or more.The preferred sodium metaaluminate of described alkali-metal meta-aluminic acid sodium salt, potassium metaaluminate or their mixture.In described strong acid salt preferably sulfuric acid aluminium, aluminum nitrate, the aluminum chloride one or more.
According to method provided by the invention, described precipitation agent refers to can generate in the species of aluminium hydroxide one or more with the reaction of described aluminum contained compound.If aluminum contained compound solution is when presenting alkalescence, such as alkali-metal meta-aluminate solution, described precipitant solution is generally the solution of one or more acidic substance.In the strong acid salt of preferred organic acid, mineral acid, aluminium one or more.Described organic acid is selected from one or more in formic acid, acetic acid, propionic acid and various isomer thereof, butyric acid and various isomer thereof, Succinic Acid, oxalic acid, the phenylformic acid.In the preferred nitric acid of described mineral acid, sulfuric acid, hydrochloric acid, hydrofluoric acid, the carbonic acid one or more.In strong acid salt preferably sulfuric acid aluminium, aluminum nitrate and the aluminum chloride of described aluminium one or more.
When described aluminum contained compound solution is acidity, as when being the strong acid salt of aluminium, described precipitation agent is selected from a kind of alkaline matter, one or more in the oxyhydroxide of preferred as alkali (such as sodium hydroxide, potassium hydroxide), alkali-metal carbonate (such as yellow soda ash, sodium bicarbonate, salt of wormwood, saleratus, volatile salt, bicarbonate of ammonia), ammonia, ammoniacal liquor, urea and the alkali-metal meta-aluminate.
According to method provided by the invention, the water-soluble additive that in the slurries of the aluminium hydroxide that stock liquid and neutralization produce, adds in the described N-process, be selected from one or more in the water-soluble inorganic salt, or can be dissolved in the water organic one or more.In the preferred volatile salt of described water-soluble additive, ammonium phosphate, the bicarbonate of ammonia one or more.In described organic additive preferred alcohol, propyl alcohol, butanols, polyoxyethylene glycol, poly-propyl alcohol, oxyethane, polyacrylamide, polyvinyl alcohol, methylcellulose gum, the stearate (such as sodium stearate, potassium stearate) one or more.
According to method provided by the invention, in described washing step, describedly carry out according to a conventional method with deionized water wash, wash used amount of deionized water at every turn and be more than 10 times of preparation alumina dry base unit weight.The purpose of washing is the foreign ion of removing wherein, makes the content of acid ion in the alumina product such as sulfate ion be not more than 0.1% of pseudo-boehmite butt, and alkali metal oxide content is not more than 0.05% of pseudo-boehmite butt.The aluminium hydroxide solid content is 5～50% in the filter cake that washing finishes to obtain after last time.
Neutralisation prepares aluminium hydroxide gained filter cake determination of solid content method and is generally: get a certain amount of filter cake, dry to constant weight under 120 ℃ condition, calculate its solid content, namely solid content is the ratio of the rear filter cake quality of oven dry and the front filter cake quality of oven dry.
According to method provided by the invention, the sour dispersion index of the hydrated alumina filter cake of preparing is 30%～100%.The sour dispersion index of filter cake is measured as follows:
1) gets a certain amount of filter cake, measure its solid content, be designated as X;
2) get 10 gram filter cakes in beaker, add the grams that is estimated the nitric acid that needs by following formula:
Quality=the X/1.4 that adds nitric acid
Add simultaneously the quality that is estimated the water of needs adding by following formula:
The quality of the water that adds=10 * (7.5 * X-1)
3) be stirred to filter cake and be dispersed in fully in the acidic liquid, left standstill 24～72 hours, supernatant liquid is dried to constant weight at 120 ℃, claim its quality to be designated as Y gram, then the sour dispersion index of filter cake is 100 * Y/(10 * X).
According to method provided by the invention, according to a conventional method moulding of described moulding can be adopted spray drying process moulding, forming oil column, and extruded moulding, the more preferred latter.Described extruded moulding refers to the filter cake behind the final step washing filtering is directly carried out extruded moulding.Also can aluminium hydroxide, aluminum oxide, sizing agent, auxiliary agent etc. be mediated then extrusion moulding with filter cake according to ordinary method, also in the end in advance aluminium hydroxide, aluminum oxide, sizing agent, auxiliary agent etc. are added in the aluminum hydroxide slurry in the water washing process of several steps, after the filtration with the filter cake straight forming that obtains.If need so that in the aluminium hydroxide of preparation or aluminum oxide, contain have catalysis, effect metal ion, metal oxide, the acid ion such as fractionation by adsorption, then in the end add suitable metal-salt, metal oxide etc. in the slurries of water washing process of several steps or in the kneading process of the filter cake that washing is finished, in finished product aluminium hydroxide or aluminum oxide, have the suitable concentration that can play a role so that these have effect metal ion, metal oxide, the acid ions such as catalysis, fractionation by adsorption.
Advantage of the present invention is needn't pass through pseudo-boehmite gel drying, pulverizing reshaping, but directly will be through the filter cake moulding after the washing.But also in the end add other composition in the aluminum hydroxide slurry whipping process of several steps, comprise aluminium hydroxide, aluminum oxide, sizing agent, metal ion, metal oxide, in the acid ion one or more, the mode that adds has like this guaranteed that the substance that adds mixes with aluminium hydroxide fully, be attached together, and so that the finished product of preparing has more widely function, not only can do aluminum oxide, also can add each metal ion species at aluminum oxide, metal-salt, metal oxide etc., simultaneously also can be after adding these materials so that the pore structure of aluminum oxide change, save pseudo-boehmite gel drying in the preparation alumina process, crushing process, simplified loaded metal ion, metal oxide, the operating process of metal-salt etc.
Method provided by the invention not only can prepare aluminum oxide, simultaneously because can add also direct Kaolinite Preparation of Catalyst of other component.The aluminum oxide of preparation can directly be used as various sorbent materials and various catalyzer, such as carrier or the matrix of the catalyzer such as hydrotreatment, hydrocracking, catalytic cracking, reformation, isomerization, alkylation, disproportionation.Directly prepare take aluminum oxide as matrix or being used for as catalyzer that hydrotreatment, hydrocracking, catalytic cracking, reformation, isomerization, alkylation, disproportionation etc. are reacted of carrier.
Embodiment
Embodiment 1
Under the condition that stirs, with concentration be 150 gram aluminum oxide/liter sodium aluminate solution 3000 gram, with concentration be 80 gram aluminum oxide/liter alum liquor carry out and flow neutralization reaction, in sodium aluminate solution, add 4 gram ammonium phosphate, the feed rate of sodium metaaluminate is 1.8 l/hs and joins in one 5 liters the plastic cans, become the glue temperature to keep 40 ± 2 ℃, adjust the Tai-Ace S 150 flow and make the pH value keep 8.5 ± 0.3, add 2 gram sodium stearate in the slurries of neutralization beginning.Wore out 60 minutes after neutralization reaction finishes, aging temperature is 50 ℃, and aging pH is 8.5 ± 0.3, adds 120 gram bicarbonate of ammonia during aging the end.With 15 liters of deionized water wash 6 times, filter and obtain wet cake.Filter cake is extruded into the bar shaped of 4 millimeters of diameters, 120 ℃ of oven dry, and 550 ℃ of roastings 4 hours obtain aluminum oxide A1, and the physico-chemical property of aluminum oxide A1 is shown in Table 1.
Embodiment 2
Method according to embodiment 1 prepares aluminum oxide, different is that neutral temperature is 75 ℃, in and pH be 7.5 ± 0.3, sneak into 5 gram Macrogol 4000s in the raw material sodium aluminate solution, with ammoniacal liquor its pH is adjusted into 8.5 ± 0.3 during aging the end, 75 ℃ of aging temperatures, aging pH are 8.0 ± 0.3, get aluminum oxide A2, the physico-chemical property of aluminum oxide A2 is shown in Table 1.
Embodiment 3
Method according to embodiment 1 prepares aluminum oxide, and different is that neutral temperature is 60 ℃, in and pH be 8.8, when beginning neutralization adds 10 gram sodium stearate in slurries, aging temperature is 70 ℃, gets aluminum oxide A3, the physico-chemical property of aluminum oxide A3 is shown in Table 1.
Embodiment 4
Method according to embodiment 1 prepares aluminum oxide, the concentration of different is sodium aluminate be 200 gram aluminum oxide/liter, adding speed is 1.2 l/hs, the concentration of Tai-Ace S 150 be 60 the gram aluminum oxide/liter, dissolve in the poly-propyl alcohol of 10 grams in alum liquor, neutral temperature is 55 ℃, in and pH be controlled to be 8.0 ± 0.3, get aluminum oxide A4, the physico-chemical property of aluminum oxide A4 is shown in Table 1.
Embodiment 5
Method according to embodiment 4 prepares aluminum oxide, adds 120 gram saleratus during aging beginning that different is, neutral temperature is 65 ℃, in and pH be 7.0, get aluminum oxide A5, the physico-chemical property of aluminum oxide A1 is shown in Table 1.
Embodiment 6
Method according to embodiment 1 prepares aluminum oxide, the concentration of different is sodium aluminate be 120 gram aluminum oxide/liter, add 5 gram polyacrylamides after neutralization finishes, aging 10 minutes, aging temperature was 65 ℃, gets aluminum oxide A6, the physico-chemical property of aluminum oxide A6 is shown in Table 1.
The physical index of the aluminum oxide of above-mentioned example preparation sees the following form:
Claims (5)
1. the preparation method of a straight forming aluminum oxide is characterized in that:
For directly carrying out moulding by wet filter cake, its pore volume is 0.3～0.8ml/g, and specific surface area is 150～300m
2/ g, crushing strength is 30～120N/ grain; Preparation process is:
A) a kind of Aluminum Compounds solution and a kind of precipitant solution of containing be 30～80 ℃ of temperature, and the pH value is to neutralize under 6～9 the condition, adds auxiliary agent in the N-process, neutralizes complete aging at least 10 minutes;
B) with deionized water the aluminum hydroxide gel for preparing is carried out 4～10 washings, each washing deionized water consumption is 10～40 times of prepared aluminium hydroxide butt quality, obtain the hydrated alumina wet cake behind the washing filtering, the middle aluminium hydroxide content of control filter cake is 5%～50%;
C) add auxiliary agent in one or more liquid in step a) and step b); The filter cake that washing finishes to obtain obtains finished product according to conventional forming method moulding in 80-120 ℃ of drying, a 450-1000 ℃ calcining.
2. preparation method according to claim 1, it is characterized in that: aluminum contained compound is selected from one or more in the alkali-metal meta-aluminate, or in the strong acid salt of aluminium one or more; Described precipitation agent refers to can generate in the material of aluminum hydroxide precipitation one or more with the reaction of described aluminum contained compound.
3. preparation method according to claim 1 is characterized in that; When described aluminum contained compound was selected from sodium metaaluminate, potassium metaaluminate or their mixture, then corresponding described precipitation agent was selected from and is Tai-Ace S 150, aluminum nitrate, aluminum chloride, sulfuric acid, nitric acid, hydrochloric acid or their mixture; When described aluminum contained compound was selected from as Tai-Ace S 150, aluminum nitrate, aluminum chloride or their mixture, then corresponding described precipitation agent was selected from sodium hydroxide, potassium hydroxide, yellow soda ash, ammoniacal liquor, sodium metaaluminate.
4. preparation method according to claim 1 is characterized in that the auxiliary agent that adds in the N-process is gained alumina amount 0.1～55%; Described auxiliary agent is selected from water-soluble inorganic salt and water miscible organism, wherein water miscible inorganic salt are selected from one or more in volatile salt, ammonium phosphate, the bicarbonate of ammonia, and water miscible organism or organic acid salt are selected from as ethanol, propyl alcohol, butanols, polyoxyethylene glycol, gather one or more in propyl alcohol, oxyethane, polyacrylamide, polyvinyl alcohol, methylcellulose gum, sodium stearate, the potassium stearate.
5. preparation method according to claim 1 is characterized in that, the sour dispersion index of the hydrated alumina filter cake of preparing is 30%～100%.
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