CN104671263B - A kind of preparation method of boehmite - Google Patents
A kind of preparation method of boehmite Download PDFInfo
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- CN104671263B CN104671263B CN201310605029.8A CN201310605029A CN104671263B CN 104671263 B CN104671263 B CN 104671263B CN 201310605029 A CN201310605029 A CN 201310605029A CN 104671263 B CN104671263 B CN 104671263B
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Abstract
The invention discloses the preparation method of a kind of boehmite.The method includes preparing aluminum hydroxide precipitation, aging, washing, it is dried, the most aging carry out in following container: being provided with filter cloth in container vertically, make ageing tank be divided into an interlayer district and a center, center is provided with agitator, the negative and positive the two poles of the earth producing electric field are placed in interlayer district relatively, and control aging condition.The method can improve the performance of boehmite, and reduces the water consumption in subsequent laundering process.
Description
Technical field
The present invention relates to the preparation method of a kind of boehmite, particularly to the preparation method of a kind of boehmite with high-crystallinity.
Background technology
γ-Al2O3Aluminium oxide, as catalysis material, has a very wide range of applications in catalytic field particularly catalytic hydrogenation field.Preparation γ-Al2O3Usual method be first to produce boehmite, roasting the most at a certain temperature is converted into γ-Al2O3.Prepare boehmite method a lot, but be mainly precipitated as with acid system or alkaline process main, such as:
(1) the neutralization reaction of aluminium salt and alkaline precipitating agent, such as Alchlor process:
AlCl3+3NH4OH → Al(OH)3+3NH4Cl
(2) acid aluminium salt and the metathesis reaction of basic aluminate, such as aluminum sulfate method:
Al2(SO4)3+6NaAlO2+12H2O → 8Al(OH)3+3Na2SO4
(3) the neutralization reaction of basic aluminate and acidic precipitation agent, such as carbonizatin method:
2NaAlO2+CO2+3H2O → 2Al(OH)3+Na2CO3
Boehmite preparation process includes that precipitation, serosity are aging, washs and drying and other steps, wherein, aging and washing is also important preparation process, aging briefly, be exactly in serosity radius less or in irregular shape be prone to dissolve aluminium hydroxide dissolve, more greatly or in thicker part, result is that particle size tends to uniformly, shape tends to rule to deposit to radius；Washing is aging continuity, is again to remove impurity to improve the process of product purity.Conventional ageing process be by plastic after serosity directly carry out aging under the conditions of certain alkalescence, then the serosity washings after aging are repeatedly washed to neutrality.But owing in precipitation process, boehmite granularity is superfine, reach or close to colloid particle size, these particles can form glue core in alkaline slurry, owing to having the biggest specific surface area, substantial amounts of heteroion can be adsorbed on glue core surface, the double electrical layers formed under electrostatic attraction, molecular separating force and hydrogen bond act on jointly, by Na+It is firmly adsorbed on the surface of solids, the most in the basic conditions, owing to substantial amounts of alkali exists, the absorption of part alkali can be made or be mixed in boehmite crystal grain, therefore, the direct aging meeting of sediment slurry affects the crystalline state of boehmite because of aging condition and the difference of the existence of heteroion, and then also determines the degree of difficulty of subsequent wash.Further, owing to having wrapped up a large amount of alkaline solution between cluster of hydrous ions, when filtering, cluster of hydrous ions easily deforms, making filtration channel not smooth, resistance increases, and causes washing difficulty.Just because of production technology and the particularity of product property so that the washing process difficulty of boehmite.At present commercial production is taked to strengthen leaching requirement, improves temperature of washing water, increases stirring and controls the measures such as filter cake moisture, but effect inconspicuous, the water consumption of boehmite per ton is still between 40 ~ 100 tons.Meanwhile, improving wash temperature, increase stirring cost is high, controls filter cake moisture poor efficiency low, and strengthening leaching requirement increase wastewater flow rate also can increase cost.
CN
102309994A discloses the preparation method of a kind of alumina support, its boehmite uses pH swing method to prepare, and adds the organic stabilizer such as polyvinyl alcohol, Polyethylene Glycol-100 and prepare that crystal grain is relatively uniform and the boehmite of higher crystallinity in ageing process.Due to aging addition organic stabilizer, this is to reduce the aggregation extent of aluminium oxide particles to the method improving degree of crystallinity, and the process of follow-up water-washing process and water lotion is brought more difficulty, and the stabilizer Han Organic substance in the sewage produced, can be to environment.
CN
200910308546.2 preparations disclosing a kind of boehmite, the method is the purpose reaching washing process water saving, adds seed precipitation solution or plant point washing liquid with dilution concentration of slurry and the Na of displacement parcel when serosity is warmed up to aging temperature or in ageing process+.Although the method has reached the purpose of water saving, but there is not significant change in the index of boehmite.And, in serosity, add substantial amounts of seed precipitation solution or kind point washing liquid to carry out heating up or maintaining aging temperature, then need to consume substantial amounts of energy, add the cost of boehmite, simultaneously, due to seed precipitation solution or the addition of kind point washing liquid so that slurry volume increases, and too increases the load of subsequent wash filter plant.
Summary of the invention
In order to overcome deficiency of the prior art, the invention provides the preparation method of a kind of boehmite.The method can improve the performance of boehmite, and reduces the water consumption in subsequent laundering process.
The preparation method of boehmite of the present invention, including preparing aluminum hydroxide precipitation, aging, washing, it is dried, the most aging carry out in following container: ageing tank is vertical, top is provided with charging aperture, filter cloth it is provided with vertically in container, ageing tank is made to be divided into an interlayer district and a center, center is provided with agitator, the negative and positive the two poles of the earth producing electric field are placed in interlayer district relatively, control aging condition as follows: the solid content adding the aluminum hydroxide precipitate in ageing tank center is 25 ~ 150g/L, aging temperature is 20 ~ 100 DEG C, it is preferably 25 ~ 90 DEG C, aging pH value is 8.0 ~ 11.0, ageing time is 30 ~ 120min, pole strength is 30 ~ 150N/C；Bottom the interlayer district of ageing tank, it is provided with leakage fluid dram, bottom center, is provided with slurry discharge mouth, when after aging end, first open leakage fluid dram bottom interlayer district and make liquid in interlayer discharge, then open the stock discharge mouth bottom center and make serosity discharge.
In the inventive method, the anode and cathode material of routine can be used for producing the anode and cathode of electric field, controlling produced electric field intensity is 30 ~ 150N/C, it is preferably when the 1/3 of aging beginning to ageing time, electric field intensity is 30 ~ 80N/C, the electric field intensity of residue ageing time increases by 20 ~ 100N/C, and makes electric field intensity reach 80 ~ 150N/C.After electrifying electrodes, electric field is horizontally through the center of ageing tank.
In the inventive method, described ageing tank is spherical or cylindrical.In interlayer district, inwall accounts for the 1/20 ~ 1/15 of ageing tank radius with the spacing of filter cloth.
In the inventive method, prepare aluminum hydroxide precipitation and can use the acid-base neutralization sedimentation method of routine, the aluminium salt such as using acidity precipitates with alkaline precipitating agent, precipitates with the aluminate of acid aluminium salt with alkalescence, precipitates with acidic precipitation agent with the aluminate of alkalescence.Acid aluminium salt is generally one or more in aluminum chloride, aluminum sulfate, aluminum nitrate.Alkaline precipitating agent is one or more in sodium hydroxide, potassium hydroxide, sodium bicarbonate, potassium bicarbonate, sodium carbonate, potassium carbonate, ammonia.Acidic precipitation agent is generally carbon dioxide.The aluminate of alkalescence is sodium metaaluminate.The inventive method is particularly well-suited to introduce sodium ion and/or the intermediate processing of potassium ion.Described precipitation plastic process is typically carried out under certain pH value condition, typical pH is 6.0 ~ 10.0, relatively it is suitably for 7.0 ~ 9.5, gelling temperature is typically carried out at room temperature ~ 85 DEG C, relatively it is suitably for 40 ~ 80 DEG C, gelation time is 45min ~ 120min, and those skilled in the art suitably can adjust with the difference becoming gluing method according to used raw material.
The inventive method, it is provided with leakage fluid dram bottom the interlayer district of ageing tank, slurry discharge mouth it is provided with bottom center, when after aging end, first opening tapping valve bottom interlayer district makes liquid in interlayer be discharged by leakage fluid dram, opening the outlet valve bottom center again makes serosity be discharged by stock discharge mouth, prevents in the liquid reverse osmosis overfall liquid in interlayer.The inventive method, the most aging and washing is all carried out in ageing tank, specific as follows: after aging end, open the tapping valve bottom interlayer district, then in ageing tank center, directly add washings, and wash under agitation, control electric field intensity less than 10N/C simultaneously.After washing terminates, then open the outlet valve bottom center, discharge serosity and be dried after filtering.Described washing uses deionized water wash, and wash temperature is 20 ~ 100 DEG C, preferably 50 ~ 90 DEG C, typically can or slightly below aging temperature identical with aging temperature.
The inventive method, is dried after washing and conventional method and condition can be used to carry out.Drying condition is as follows: baking temperature 100 ~ 150 DEG C, 4 ~ 10 hours drying times.
The inventive method uses in ageing process and carries out under certain electric field intensity, electric field is horizontally through serosity in tank, and make the glue core of parcel impurity also can discharge heteroion because the effect of stirring external force is broken under conditions of stirring, under the effect of electric field, the heteroion quantity making entrance intra-die greatly reduces, and make serosity and free ion rearrangement under electric field action of absorption different ions, part heteroion can also be removed simultaneously, so be conducive to making boehmite granule more complete, homogeneous, effectively shorten and grow up the time, improve the degree of crystallinity of boehmite, and peptization is fine, be conducive to the carrying out of subsequent laundering process simultaneously, washing is easier to, reduce water consumption, reduce and pollute, reduce cost.
Accompanying drawing explanation
The ageing tank schematic diagram that Fig. 1 the inventive method uses；
The ageing tank cross-sectional view that Fig. 2 the inventive method uses；
In figure, 1 is stirring motor；2 is agitator；3 is filter cloth；4 is electrode；5 is leakage fluid dram；6 is slurry discharge mouth；7 is ageing tank；8 is charging aperture；9 is washing water inlet；10 is interlayer district；District centered by 11.
Detailed description of the invention
The ageing tank used the inventive method below in conjunction with the accompanying drawings is made an explanation.
Ageing tank 7 used by the inventive method is vertical, top is provided with charging aperture 8, filter cloth 3 it is provided with vertically in container, ageing tank is made to be divided into an interlayer district 10 and a center 11, center 11 is provided with agitator 2, and agitator 2 is driven by stirring motor 1, is relatively placed in interlayer district 10 at the negative and positive the two poles of the earth 4 producing electric field, the bottom in interlayer district 10 sets leakage fluid dram 5, and the bottom of center 11 sets slurry discharge mouth 6.
In the inventive method, preferably top at ageing tank is provided with washing water inlet 9, directly washs, it is not necessary to the most more exchange device after making aging end.
In the inventive method, serosity after precipitation plastic is entered in the center 11 of ageing tank 7 by charging aperture 8, under agitation, under the effect of certain electric field, carry out aging under appropriate conditions, after aging end, open the leakage fluid dram 5 bottom interlayer district, open the slurry discharge mouth 6 bottom center the most again, to avoid the liquid phase in interlayer district to return center.
In the inventive method, the most aging and washing is all carried out in ageing tank, specific as follows: after aging end, open the leakage fluid dram 5 bottom interlayer district, then in the center of ageing tank, injected deionized water by washing water inlet 9, under agitation the serosity after aging is washed, after washing terminates, then opening the slurry discharge mouth 6 bottom center, the serosity of discharge is after filtering, it is dried, obtains boehmite.
The technical scheme that the invention is further illustrated by the following examples, but it is not limited to embodiment.
Boehmite of the present invention is determined by indexs such as relative crystallinity, pore volume and acidity indexes.Boehmite relative crystallinity is that test powder obtains result in contrast with SB powder for reference to location 100%.Peptization index testing method is: take a certain amount of aluminium hydroxide (with Al2O3Meter) Al in mass ratio2O3 : HNO3After=1:0.2 adds the concentrated nitric acid that mass concentration is 65%, can the Al of peptization part2O3Account for the percent of total aluminium oxide.Peptization index is the biggest, and boehmite peptization is the best.Described pore volume, specific surface area and pore-size distribution use low temperature liquid nitrogen absorption method to record.
Embodiment 1
Preparation sodium aluminate solution concentration is 200gAl2O3/ L amounts to 1L, be heated to 70 DEG C stand-by, aluminum sulfate solution concentration is 80gAl2O3/ L amounts to 2L, be heated to 70 DEG C stand-by.
Adding 1.0L distilled water in plastic cans, be heated to 70 DEG C, and flow addition above two serosity, keeping pH value is 8.0, and during plastic, temperature is maintained at 70 DEG C.The ageing step is entered after cemented into bundles.Serosity after cemented into bundles is entered in ageing tank 7 by charging aperture 8, under the conditions of low whipping speed is 150rpm, under the effect that electric field intensity is 80N/C, it is 8.0 at pH value, temperature be 70 DEG C and the time be carry out under conditions of 60min aging, after aging end, open the leakage fluid dram 5 bottom interlayer district, then 65 DEG C of deionized waters are injected by washing water inlet 9, it is 200rpm in stir speed (S.S.) the serosity after aging is washed, after washing terminates, open the slurry discharge mouth 6 bottom center again, the serosity discharged is after filtering, filter cake obtains boehmite T-1 after 100 DEG C of dry 3h, its physico-chemical property is shown in Table 1.
Embodiment 2
Plastic pH value, with embodiment 1, simply is controlled to be 7.0 by preparation process, and gelling temperature is 80 DEG C, and ageing time is 100min, and in ageing process, electric field intensity is 50N/C, prepares boehmite T-2, and its physico-chemical property is shown in Table 1.
Embodiment 3
Preparation process is with embodiment 1, and simply adjusting aging pH value is 9.5, and ageing time is 30min, and in ageing process, electric field intensity is 100N/C, prepares boehmite T-3, and its physico-chemical property is shown in Table 1.
Embodiment 4
Preparation process is with embodiment 1, and simply 20min before ageing process, electric field intensity is 40N/C, and residue ageing time electric field intensity becomes 120N/C, prepares boehmite T-4, and its physico-chemical property is shown in Table 1.
Comparative example
Preparation sodium aluminate solution concentration is 200gAl2O3/ L amounts to 1L, be heated to 70 DEG C stand-by, aluminum sulfate solution concentration is 80gAl2O3/ L amounts to 2L, be heated to 70 DEG C stand-by.
Adding 1.0L distilled water in plastic cans, be heated to 70 DEG C, and flow addition above two serosity, keeping pH value is 8.0, and during plastic, temperature is maintained at 70 DEG C.The ageing step is entered after cemented into bundles.Serosity after cemented into bundles is entered in ageing tank by charging aperture, low whipping speed is 150rpm, pH value is 8.0, temperature is 70 DEG C and the time be carry out under conditions of 60min aging, after aging end, serosity is carried out washing and filtering, temperature of washing water is 65 DEG C, and filter cake obtains boehmite T-F after 100 DEG C of dry 3h, and its physico-chemical property is shown in Table 1.
Wherein ageing tank uses the conventional container being provided only with agitator, charging aperture and discharging opening.
The boehmite of above-mentioned preparation prepares after roasting 3h at 600 DEG C different aluminium oxide, and its physico-chemical property is shown in 2.
Table
1
The physico-chemical property of boehmite
Table
2
The physico-chemical property of aluminium oxide
| Numbering | Pore volume, mL/g | Specific surface area, m2/g | Pore-size distribution (10-50nm), % |
| T-1 | 1.0 | 311 | 55.6 |
| T-2 | 0.97 | 320 | 49.8 |
| T-3 | 1.02 | 298 | 59.3 |
| T-4 | 1.06 | 305 | 62.1 |
| Comparative example T-F | 0.90 | 350 | 40.8 |
Data from Tables 1 and 2, it can be seen that the boehmite impurity content using the present invention to prepare is low, degree of crystallinity is high and unit washings consumption is few, prepares aluminium oxide simultaneously and have bigger pore volume, and macropore ratio is high.
Claims (11)
1. the preparation method of a boehmite, including preparing aluminum hydroxide precipitation, aging, washing, it is dried, the most aging carry out in following container: ageing tank is vertical, top is provided with charging aperture, filter cloth it is provided with vertically in container, ageing tank is made to be divided into an interlayer district and a center, center is provided with agitator, the negative and positive the two poles of the earth producing electric field are placed in interlayer district relatively, control aging condition as follows: adding the solid content of aluminum hydroxide precipitate in ageing tank is 25 ~ 150g/L, aging temperature is 20 ~ 100 DEG C, aging pH value is 8.0 ~ 11.0, ageing time is 30 ~ 120min, pole strength is 30 ~ 150N/C；Bottom the interlayer district of ageing tank, it is provided with leakage fluid dram, bottom center, is provided with stock discharge mouth, when after aging end, first open leakage fluid dram bottom interlayer district and make liquid in interlayer discharge, then open the stock discharge mouth bottom center and make serosity discharge；Wherein, when the 1/3 of aging beginning to ageing time, electric field intensity is 30 ~ 80N/C, and the electric field intensity of residue ageing time increases by 20 ~ 100N/C, and makes electric field intensity reach 80 ~ 150N/C, and after electrifying electrodes, electric field is horizontally through the center of ageing tank.
The most in accordance with the method for claim 1, it is characterised in that: aging temperature is 25 ~ 90 DEG C.
The most in accordance with the method for claim 1, it is characterised in that: described ageing tank is spherical or cylindrical, and in interlayer district, container inner wall accounts for the 1/20 ~ 1/15 of ageing tank radius with the spacing of filter cloth.
The most in accordance with the method for claim 1, it is characterised in that: prepare aluminum hydroxide precipitation and use the acid-base neutralization sedimentation method.
5. according to the method described in claim 1 or 4, it is characterised in that: introduce sodium ion and/or the intermediate processing of potassium ion when preparing aluminum hydroxide precipitation.
The most in accordance with the method for claim 4, it is characterized in that: prepare aluminum hydroxide precipitation and use acid aluminium salt to precipitate with alkaline precipitating agent, or precipitate with the aluminate of acid aluminium salt with alkalescence, or precipitate with acidic precipitation agent with the aluminate of alkalescence.
The most in accordance with the method for claim 6, it is characterised in that: acid aluminium salt is one or more in aluminum chloride, aluminum sulfate, aluminum nitrate；Alkaline precipitating agent is one or more in sodium hydroxide, potassium hydroxide, sodium bicarbonate, potassium bicarbonate, sodium carbonate, potassium carbonate, ammonia；Acidic precipitation agent is carbon dioxide；The aluminate of alkalescence is sodium metaaluminate.
The most in accordance with the method for claim 6, it is characterised in that: the pH of described precipitation is 6.0 ~ 10.0, and gelling temperature is 40 ~ 80 DEG C, and gelation time is 45min ~ 120min.
The most in accordance with the method for claim 1, it is characterized in that: after aging, washing process is also carried out in ageing tank, specific as follows: after aging end, opens the leakage fluid dram bottom interlayer district, then in ageing tank, directly add washings, and wash under agitation, control electric field intensity simultaneously and be less than 10N/C, after washing terminates, open the stock discharge mouth bottom center again, discharge serosity and be dried after filtering.
10. according to the method described in claim 1 or 9, it is characterised in that: described washing uses deionized water wash, and wash temperature is 20 ~ 100 DEG C.
11. in accordance with the method for claim 1, it is characterised in that: described drying condition is as follows: baking temperature 100 ~ 150 DEG C, 4 ~ 10 hours drying times.
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| CN110639484B (en) * | 2019-09-25 | 2020-12-29 | 山东金滢新材料有限公司 | Preparation method of pseudo-boehmite |
| CN112755936B (en) * | 2019-10-21 | 2022-09-02 | 中国石油化工股份有限公司 | Device for continuously preparing pseudo-boehmite and preparation method thereof |
| CN110655096B (en) * | 2019-10-21 | 2022-01-14 | 湖南慧璟新材料有限公司 | Preparation method of pseudo-boehmite |
| CN111823678A (en) * | 2020-07-17 | 2020-10-27 | 枣庄市聚信新材料科技有限公司 | Pesticide slow-release film based on polyvinyl alcohol and preparation method thereof |
| CN112062144B (en) * | 2020-09-19 | 2021-05-18 | 河津市炬华铝业有限公司 | Large-pore-volume pseudo-boehmite and preparation method thereof |
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| US3714313A (en) * | 1971-01-27 | 1973-01-30 | Kaiser Aluminium Chem Corp | Agglomerating partially dehydrated gel-derived pseudoboehmitic alumina to form strong porous spheres |
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