CN102259900B - Hydrated alumina and preparation method thereof - Google Patents
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Abstract
The invention provides hydrated alumina, which contains pseudo-boehmite and also contains ammonium aluminum carbonate hydroxide. The invention also provides a preparation method of hydrated alumina. The preparation method comprises carrying out contact reaction on sodium metaaluminate and/or sodium aluminate and an acidic solution and aging the mixed slurry obtained by the contact reaction in the presence of an aging agent, wherein the contact reaction conditions are as follows: the reaction pH is 4.5-9 and the reaction temperature is 15-75 DEG C; the aging conditions are as follows: the aging temperature is 20-60 DEG C and the aging time is 2-6 hours; and the aging agent is ammonium carbonate and/or ammonium bicarbonate. An alumina carrier prepared from hydrated alumina which is prepared by the preparation method of hydrated alumina has the most probable diameter, an average pore diameter and a pore volume which are markedly improved as well as the ratio of the pore volume with pore diameter of 10-60 nm to the total pore volume.
Description
Technical field
The present invention relates to the preparation method of a kind of hydrated aluminum oxide and this hydrated aluminum oxide.
Background technology
Pseudo-boehmite, as the precursor of aluminum oxide, generates activated alumina after roasting at a certain temperature.Activated alumina has good thermostability, certain activity, suitable pore structure, suitable specific surface area, the higher premium propertiess such as physical strength, becomes the carrier of carrier, the especially hydrogenation catalyst of multiple catalysts in petroleum chemical industry.
Heavy-oil hydrogenation technology is the effective way that oil refining enterprise increased economic efficiency, realized high efficiency of energy clean utilization, gets more and more people's extensive concerning.The poor residuum that heavy oil, especially metal content are higher, has the advantages that molecule is large, the dirty thing of impurity is more, heavy-oil hydrogenation catalyst used carrier material requirements aperture is large as far as possible, pore volume is high as far as possible, to improve the ability that removes, holds metal of catalyzer, improves the running period of device.
The wide aperture of heavy-oil hydrogenation catalyst, high pore volume character depend primarily on carrier, depend on the starting material pseudo-boehmite of preparing carrier.
The conventional pseudo-boehmite for the preparation of large-pore alumina carrier is only adding physics expanding agent as carbon black or chemical enlargement agent as phosphide in the situation that conventionally, just can make all very large alumina supporters of pore volume and aperture.Yet, because the reaming effect of physics expanding agent or chemical enlargement agent is limited, therefore, by adding the pore structure of the alumina supporter that physics expanding agent or chemical enlargement agent make still not reach the requirement of hydrogenation catalyst cracking treatment process of the heavy oil of high metal content in the pseudo-boehmite to conventional.And, adopt pseudo-boehmite to add physics expanding agent or chemical enlargement agent not only can make complex manufacturing in preparing the process of alumina supporter, but also increasing production cost.
Summary of the invention
The present invention need to be by adding physics expanding agent or chemical enlargement agent to make wide-aperture alumina supporter in order to overcome existing pseudo-boehmite, even by adding physics expanding agent to be still difficult to make the shortcoming of the alumina supporter of enough large pore structure as phosphide as carbon black or chemical enlargement agent, a kind of new hydrated aluminum oxide and preparation method thereof is provided, adopting this hydrated aluminum oxide to prepare in the process of alumina supporter, do not need to add physics expanding agent or chemical enlargement agent to can be made into the alumina supporter with enough large pore structure.
The invention provides a kind of hydrated aluminum oxide, this hydrated aluminum oxide contains pseudo-boehmite, and wherein, this hydrated aluminum oxide also contains Aluminum Carbonate Basic ammonium.
The present invention also provides the preparation method of described hydrated aluminum oxide, and the method comprises makes sodium metaaluminate and/or sodium aluminate and acidic solution contact reacts, and the mixed serum obtaining after contact reacts is carried out aging under aging dose of existence; Described catalytic condition comprises: pH value in reaction is 4.5-9, and temperature of reaction is 15-75 ℃; Described aging condition comprises: temperature is 20-60 ℃, and the time is 2-6 hour; Described aging dose is volatile salt and/or bicarbonate of ammonia.
According to the preparation method of described hydrated aluminum oxide provided by the invention, by making sodium metaaluminate and/or sodium aluminate and acidic solution contact reacts, then in the mixed serum that obtains after reaction, add aging dose as volatile salt and/or bicarbonate of ammonia, and by controlling described catalytic condition and aging condition, thereby in the hydrated aluminum oxide making, except main ingredient pseudo-boehmite, also contain a small amount of Aluminum Carbonate Basic ammonium.At the described hydrated aluminum oxide of employing, prepare in the process of alumina supporter, described Aluminum Carbonate Basic ammonium has than conventional physics expanding agent as carbon black and chemical enlargement agent reaming ability as better in phosphide, thereby can make the alumina supporter with improved pore structure.
Accompanying drawing explanation
Fig. 1 represents the XRD spectra of the hydrated aluminum oxide that embodiment 1 makes.
Embodiment
Hydrated aluminum oxide according to the present invention contains pseudo-boehmite and Aluminum Carbonate Basic ammonium.At described hydrated aluminum oxide, by roasting, make in the process of alumina supporter, described Aluminum Carbonate Basic ammonium can play expanding agent on the one hand, on the other hand, described Aluminum Carbonate Basic ammonium can play skeleton to be supported, thereby makes described hydrated aluminum oxide can make the alumina supporter with very large pore structure.For the alumina supporter that makes to be made by described hydrated aluminum oxide has better thermostability and physical strength, under preferable case, in described hydrated aluminum oxide, the content of described pseudo-boehmite is 85-99 % by weight, and the content of Aluminum Carbonate Basic ammonium is 1-15 % by weight; Further, under preferable case, the content of described pseudo-boehmite is 86-97 % by weight, and the content of Aluminum Carbonate Basic ammonium is 3-14 % by weight; Further, under preferable case, the content of described pseudo-boehmite is 90-95 % by weight, and the content of Aluminum Carbonate Basic ammonium is 5-10 % by weight.
In the present invention, described hydrated aluminum oxide is after 400-650 ℃ of roasting, the pore structure parameter of its product of roasting as: most probable bore dia is 20-30 nanometer, and average pore diameter is 18-23 nanometer, and bore dia is the 80-96% that the pore volume of 10-60 nanometer accounts for total pore volume; In the preferred case, described hydrated aluminum oxide is after 400-650 ℃ of roasting, and the pore volume of its product of roasting is 1.3-1.7 ml/g, and specific surface area is 260-330 meters squared per gram.
The present invention also provides a kind of preparation method of hydrated aluminum oxide, and the method comprises makes sodium metaaluminate and/or sodium aluminate and acidic solution contact reacts, and the mixed serum obtaining after contact reacts is carried out aging under aging dose of existence; Described catalytic condition comprises: pH value in reaction is 4.5-9, and temperature of reaction is 15-75 ℃; Described aging condition comprises: temperature is 20-60 ℃, and the time is 2-6 hour; Described aging dose is volatile salt and/or bicarbonate of ammonia.
In the preparation method of described hydrated aluminum oxide provided by the invention, by making sodium metaaluminate and/or sodium aluminate and acidic solution contact reacts, then make the mixing solutions obtaining after reaction mix to carry out aging with volatile salt and/or bicarbonate of ammonia, and within described catalytic condition and aging adjusting are controlled to above-mentioned scope, thereby in the hydrated aluminum oxide that makes finally to make, contain Aluminum Carbonate Basic ammonium.
In the preferred case, for the hydrated aluminum oxide that makes finally to make has good crystalline structure, so that the alumina supporter that adopts this hydrated aluminum oxide to make has very large pore structure and physical strength, described sodium metaaluminate and/or sodium aluminate and the catalytic condition of described acidic solution comprise: pH value in reaction is 6-8.5, and temperature of reaction is 25-60 ℃.
According to the preparation method of described hydrated aluminum oxide provided by the invention, there is no particular limitation in the present invention for described acidic solution, can react and generate hydrated aluminum oxide with sodium metaaluminate and/or sodium aluminate (as AlO (OH) xH
2o, wherein, x is in the scope of 0.01-1, preferably within the scope of 0.1-0.9) the pH value of precipitation be less than 7 solution all can be used for the present invention in and realize object of the present invention, described acidic solution can be less than at least one in the aqueous solution of 7 metal-salt for aqueous solutions of organic acids, inorganic acid aqueous solution and pH value, under preferable case, described acidic solution is at least one in alum liquor, liquor alumini chloridi and aluminum nitrate solution.
According to the preparation method of described hydrated aluminum oxide provided by the invention, in the situation that described acidic solution is selected from least one in alum liquor, liquor alumini chloridi and aluminum nitrate solution, the weight ratio of total add-on of the Tai-Ace S 150 in described acidic solution, aluminum chloride and aluminum nitrate and total add-on of described sodium metaaluminate and sodium aluminate can be 2-4: 1, be preferably 2.3-3.6: 1.When aforementioned proportion is less than 2: 1 or is greater than 4: 1, in the hydrated aluminum oxide so making the content of Aluminum Carbonate Basic ammonium seldom, 1 % by weight of the hydrated aluminum oxide making described in being conventionally less than.In this case, the pore structure parameter that adopts the alumina supporter that this hydrated aluminum oxide makes does not increase significantly with respect to conventional pseudo-boehmite as average pore diameter, most probable bore dia and pore volume.
In the preparation method of described hydrated aluminum oxide provided by the invention, for the crystalline structure of the hydrated aluminum oxide that further improvement finally makes, described aging dose is preferably volatile salt.
According to the preparation method of described hydrated aluminum oxide provided by the invention, the weight ratio of total add-on of the weight of described aging dose and described sodium metaaluminate and sodium aluminate can be 1-2: 1, and 1.05-1.8 more preferably: 1.When total add-on of the weight of described aging dose and described sodium metaaluminate and sodium aluminate meets described ratio, within the content of the Aluminum Carbonate Basic ammonium in the hydrated aluminum oxide finally making can being controlled to the scope of 3-14 % by weight, thereby the hydrated aluminum oxide that assurance finally makes can be made the pore structure size being significantly improved with respect to conventional pseudo-boehmite tool.
In a kind of preferred implementation of the present invention, the preparation method of described hydrated aluminum oxide can also be included in described aging after, the mixing solutions obtaining through overaging is filtered successively, is washed and is dried.There is no particular limitation in the present invention for described filtration, washing and dry method, can adopt conventional method to implement.
The invention will be further described with comparative example by the following examples.
Embodiment 1
The present embodiment is used for illustrating described hydrated aluminum oxide provided by the invention and preparation method thereof.
Take the aluminum chloride (purchased from Beijing Chemical Plant) of 483 grams, be added in deionized water and dissolve and make the solution a1 that concentration is 1 mol/L; Take the sodium metaaluminate (purchased from Tianjin Jin Ke fine chemistry industry institute) of 210 grams, be added in deionized water and dissolve and make the solution b1 that concentration is 3.0 mol/L; Take the volatile salt (purchased from Beijing chemical reagents corporation) of 230 grams, be added in deionized water and dissolve and make the solution c1 that concentration is 0.5 mol/L.By solution a1 and solution b1 with and the mode of stream join in the plastic cans of 10 liters simultaneously and react, by controlling the inflow velocity of solution a1 and solution b1, make the pH value in described plastic cans remain 8.5, temperature of reaction is 60 ℃.While no longer producing precipitation in described plastic cans, in described plastic cans, add solution c1, and at 60 ℃ aging 2.5 hours.Then, the mixing solutions in described plastic cans is filtered, with the deionized water wash filter cake of 60 ℃ of 10 liters; In loft drier, at 150 ℃, make described filtration cakes torrefaction 2 hours, obtain hydrated aluminum oxide A1, the XRD spectra of this hydrated aluminum oxide as shown in Figure 1.By adopting the method for N content in chemiluminescence determination hydrated aluminum oxide can record the Aluminum Carbonate Basic ammonium that contains 7.3 % by weight in this hydrated aluminum oxide.
Comparative example 1
According to the method for embodiment 1, prepare solution a1, solution b1 and solution c1, then, by solution a1 and solution b1 with and the mode of stream join in the plastic cans of 10 liters simultaneously and react, by controlling the inflow velocity of solution a1 and solution b1, make the pH value in described plastic cans remain 4.8, temperature of reaction is 60 ℃.While no longer producing precipitation in described plastic cans, mixture in described plastic cans is filtered, filter cake and solution c1 are mixed, pulled an oar, at 75 ℃ aging 60 minutes, then filter, wash, and be dried 24 hours at 120 ℃, obtain hydrated aluminum oxide D1 (adopting XRD to show to have structure of similar to thin diaspore).By adopting the method for N content in chemiluminescence determination hydrated aluminum oxide to record, in this hydrated aluminum oxide, do not contain Aluminum Carbonate Basic ammonium.
Embodiment 2
The present embodiment is used for illustrating described hydrated aluminum oxide provided by the invention and preparation method thereof.
Take the Tai-Ace S 150 (purchased from Beijing Chemical Plant) of 666 grams, be added in deionized water and dissolve and make the solution a2 that concentration is 0.5 mol/L; Take the sodium metaaluminate (purchased from Tianjin Jin Ke fine chemistry industry institute) of 210 grams, be added in deionized water and dissolve and make the solution b2 that concentration is 2.0 mol/L; Take the bicarbonate of ammonia (purchased from Beijing chemical reagents corporation) of 370 grams, be added in deionized water and dissolve and make the solution c2 that concentration is 1.0 mol/L.By solution a2 and solution b2 with and the mode of stream join in the plastic cans of 10 liters simultaneously and react, by controlling the inflow velocity of solution a2 and solution b2, make the pH value in described plastic cans remain 6.0, temperature of reaction is 40 ℃.While no longer producing precipitation in described plastic cans, in described plastic cans, add solution c2, and at 40 ℃ aging 6 hours.Then, the mixing solutions in described plastic cans is filtered, with the deionized water wash filter cake of 40 ℃ of 15 liters; In loft drier, at 100 ℃, make described filtration cakes torrefaction 6 hours, obtain hydrated aluminum oxide A2 (adopting XRD to show to have structure of similar to thin diaspore).By adopting the method for N content in chemiluminescence determination hydrated aluminum oxide can record the Aluminum Carbonate Basic ammonium that contains 5.5 % by weight in this hydrated aluminum oxide.
Embodiment 3
The present embodiment is used for illustrating described hydrated aluminum oxide provided by the invention and preparation method thereof.
Take the aluminum nitrate (purchased from Beijing Chemical Plant's product) of 750 grams, be added in deionized water and dissolve and make the solution a3 that concentration is 1.5 mol/L; Take the sodium metaaluminate (purchased from Tianjin Jin Ke fine chemistry industry institute) of 210 grams, be added in deionized water and dissolve and make the solution b3 that concentration is 4.5 mol/L; Take the volatile salt (purchased from Beijing chemical reagents corporation) of 300 grams, be added in deionized water and dissolve and make the solution c3 that concentration is 1.5 mol/L.By solution a3 and solution b3 with and the mode of stream join in the plastic cans of 10 liters simultaneously and react, by controlling the inflow velocity of solution a3 and solution b3, make the pH value in described plastic cans remain 7.0, temperature of reaction is 25 ℃.While no longer producing precipitation in described plastic cans, in described plastic cans, add solution c3, and at 25 ℃ aging 4 hours.Then, the mixing solutions in described plastic cans is filtered, with the deionized water wash filter cake of 25 ℃ of 25 liters; In loft drier, at 120 ℃, make described filtration cakes torrefaction 4 hours, obtain hydrated aluminum oxide A3 (adopting XRD to show to have structure of similar to thin diaspore).By adopting the method for N content in chemiluminescence determination hydrated aluminum oxide can record the Aluminum Carbonate Basic ammonium that contains 9.6 % by weight in this hydrated aluminum oxide.
Test case 1
Make the hydrated aluminum oxide A1-A3, the D1 that in embodiment 1-3 and comparative example 1, make and purchased from the roasting 4 hours at 600 ℃ respectively of the pseudo-boehmite dry glue powder (D2) of Chang Ling catalyst plant, then, specific surface area, most probable bore dia, average pore diameter, pore volume and the diameter that adopts B E T Brunauer Emett Teller method of nitrogen adsorption at low temperature to measure respectively the product obtaining after roasting is the per-cent that the pore volume of 10-60 nanometer accounts for total pore volume, and its result is as shown in table 1 below.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | - | |
| Hydrated aluminum oxide | A1 | A2 | A3 | D1 | D2 |
| Specific surface area (m 2/g) | 317 | 279 | 281 | 287 | 297 |
| Most probable bore dia (nm) | 25.1 | 24.9 | 25.0 | 11.2 | 10.9 |
| Average pore diameter (nm) | 19.5 | 21.5 | 20.2 | 8.6 | 8.5 |
| Pore volume (ml/g) | 1.55 | 1.51 | 1.42 | 0.97 | 0.94 |
| Diameter is the per-cent (%) that the pore volume of 10-60 nanometer accounts for total pore volume | 83.5 | 88.0 | 85.0 | 45.0 | 37.0 |
Test case 2
100 grams of hydrated aluminum oxide A1 are mixed with the polyvinyl alcohol of 4 grams, adding the concentration containing 2.5 grams is 130 milliliters of 65 % by weight nitre aqueous acids, on screw rod banded extruder, be extruded into equivalent diameter and be the trilobal bar of 1.2 millimeters, then at 120 ℃, be dried 2 hours, and roasting 4.5 hours at 900 ℃, thereby obtain alumina supporter Z1.
With described hydrated aluminum oxide A2 and A3, replace above-mentioned hydrated aluminum oxide A1 respectively, thereby make alumina supporter Z2 and Z3.
By the described hydrated aluminum oxide D1 of 100 grams, the granular size of 6 grams, be that the carbon black of 30 microns and the sesbania powder of 3 grams mix, and add the phosphoric acid of 0.7 gram and the water of 130 grams, then after continuing kneading be plastic on double screw banded extruder, be extruded into equivalent diameter and be the trilobal bar of 1.2 millimeters, at 120 ℃, be dried 4 hours afterwards, and roasting 2 hours at 900 ℃, thereby make alumina supporter DZ1.
With described hydrated aluminum oxide D2 (purchased from the pseudo-boehmite dry glue powder of Chang Ling catalyst plant), replace above-mentioned hydrated aluminum oxide D1, thereby make alumina supporter DZ2.
Specific surface area, most probable bore dia, average pore diameter, pore volume and the diameter that adopts B E T Brunauer Emett Teller method of nitrogen adsorption at low temperature to measure respectively carrier Z1-Z3 and DZ1-DZ2 is the per-cent that the pore volume of 10-60 nanometer accounts for total pore volume, and its result is as shown in table 2 below.
Table 2
| Carrier | Z1 | Z2 | Z3 | DZ1 | DZ2 |
| Specific surface area (m 2/g) | 135 | 129 | 118 | 157 | 162 |
| Most probable bore dia (nm) | 24.9 | 25.0 | 26.5 | 18 | 17 |
| Average pore diameter (nm) | 28.3 | 29.3 | 30.5 | 19.5 | 18.7 |
| Pore volume (ml/g) | 0.95 | 0.94 | 0.90 | 0.78 | 0.76 |
| Diameter is the per-cent (%) that the pore volume of 10-60 nanometer accounts for total pore volume | 98.7 | 99.2 | 99.6 | 88.7 | 87.0 |
As can be seen from Table 2, most probable bore dia, average pore diameter, pore volume and diameter that the alumina supporter tool that employing is prepared according to the prepared hydrated aluminum oxide of the preparation method of hydrated aluminum oxide of the present invention is significantly improved are the pore volume of 10-60 nanometer.
Claims (8)
1. a hydrated aluminum oxide, this hydrated aluminum oxide contains pseudo-boehmite, it is characterized in that, and this hydrated aluminum oxide also contains Aluminum Carbonate Basic ammonium; The content of described pseudo-boehmite is 85-99 % by weight, and the content of Aluminum Carbonate Basic ammonium is 1-15 % by weight; This hydrated aluminum oxide is after 400-650 ℃ of roasting, and bore dia is the 80-96% that the pore volume of 10-60 nanometer accounts for total pore volume.
2. hydrated aluminum oxide according to claim 1, wherein, the content of described pseudo-boehmite is 86-97 % by weight, the content of Aluminum Carbonate Basic ammonium is 3-14 % by weight.
3. hydrated aluminum oxide according to claim 1 and 2, wherein, this hydrated aluminum oxide is after 400-650 ℃ of roasting, and most probable bore dia is 20-30 nanometer, and average pore diameter is 18-23 nanometer.
4. hydrated aluminum oxide according to claim 3, wherein, this hydrated aluminum oxide is after 400-650 ℃ of roasting, and pore volume is 1.3-1.7 ml/g, and specific surface area is 260-330 meters squared per gram.
5. the preparation method of hydrated aluminum oxide claimed in claim 1, is characterized in that, the method comprises makes sodium metaaluminate and/or sodium aluminate and acidic solution contact reacts, and the mixed serum obtaining after contact reacts is carried out aging under aging dose of existence; Described catalytic condition comprises: pH value in reaction is 4.5-9, and temperature of reaction is 15-75 ℃; Described aging condition comprises: temperature is 20-60 ℃, and the time is 2-6 hour; Described aging dose is volatile salt and/or bicarbonate of ammonia; The weight ratio of total add-on of the weight of described aging dose and described sodium metaaluminate and sodium aluminate is 1-2:1; The weight ratio of total add-on of the Tai-Ace S 150 in described acidic solution, aluminum chloride and aluminum nitrate and total add-on of described sodium metaaluminate and sodium aluminate is 2-4:1.
6. method according to claim 5, wherein, described catalytic condition comprises: pH value in reaction is 6-8.5, temperature of reaction is 25-60 ℃.
7. method according to claim 5, wherein, described acidic solution is at least one in alum liquor, liquor alumini chloridi and aluminum nitrate solution.
8. method according to claim 5, wherein, described method be also included in described aging after, the mixing solutions obtaining through overaging is filtered successively, is washed and is dried.
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| CN103785479B (en) * | 2012-11-01 | 2016-12-21 | 中国石油化工股份有限公司 | A kind of alumina support and preparation method thereof |
| CN104338563A (en) * | 2013-08-02 | 2015-02-11 | 天津润沃供水安装工程有限公司 | Preparation technology for hydrogenation catalyst carrier and method for controlling pore diameter |
| CN104445309B (en) * | 2013-09-17 | 2017-03-01 | 中国石油化工股份有限公司 | A kind of high purity aluminium oxide and preparation method thereof |
| CN104085907B (en) * | 2014-07-22 | 2016-06-08 | 温州精晶氧化铝有限公司 | The preparation method of large pore volume, high viscosity pseudo-boehmite |
| CN106629797A (en) * | 2016-10-25 | 2017-05-10 | 武汉理工大学 | A double-hydrolysis reaction preparing method for texture-property-controllable gamma-aluminum oxide |
| CN110935457B (en) * | 2018-09-25 | 2022-03-08 | 中国石油化工股份有限公司 | Preparation method of copper-zinc catalyst |
| CN110935455B (en) * | 2018-09-25 | 2022-07-08 | 中国石油化工股份有限公司 | Preparation method of copper-zinc catalyst |
| CN110935490B (en) * | 2018-09-25 | 2022-03-08 | 中国石油化工股份有限公司 | Copper-zinc catalyst and preparation method thereof |
| CN110451541A (en) * | 2019-08-05 | 2019-11-15 | 中海油天津化工研究设计院有限公司 | A kind of preparation method mixing aluminium hydroxide |
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| KR100633881B1 (en) * | 1999-10-14 | 2006-10-16 | 차이나 피트로케미컬 코포레이션 | Catalyst for hydrorefining distillate oil, its carrier and preparation thereof |
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| US6174511B1 (en) * | 1997-07-15 | 2001-01-16 | Japan Energy Corporation | Pseudoboehmite powder for catalyst carrier and process for preparing the same |
| CN1727063A (en) * | 2004-07-29 | 2006-02-01 | 中国石油化工股份有限公司 | Method for preparing alumina supporter in structure of double peak holes |
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