CN113998717B - Method for stably preparing pseudo-boehmite under mild condition - Google Patents
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Abstract
The invention discloses a method for stably preparing pseudo-boehmite under mild conditions. The method mainly comprises the following steps: adding ethylene glycol into the aqueous solution of sodium aluminate, stirring uniformly to obtain a clear mixed solution, placing the mixed solution into a reaction kettle for hydrothermal reaction, and centrifuging, washing and drying to obtain the pseudo-boehmite. The preparation method expands the preparation process of the single-phase pseudo-boehmite into an environment system with lower temperature, has milder reaction conditions and short reaction time, and can more stably separate out reaction products, namely, the products are still single-phase boehmite along with the extension of the reaction time. The specific surface area of the pseudo-boehmite prepared by the invention is 234.6-449.8m 2 Per g, pore volume of 0.13-0.36cm 3 Per g, average pore diameter of 2.2-4.0nm, can be used as binder and vaccine adjuvant for refractory aluminium silicate fibres, and its calcined product gamma-Al 2 O 3 Can be applied to the fields of catalysis and adsorption.
Description
Technical Field
The invention belongs to the technical field of chemical alumina preparation, and particularly relates to a method for stably preparing pseudo-boehmite under mild conditions.
Background
Pseudo-boehmite (gamma-AlOOH.nH) 2 O) is also known as gelatinous boehmite, boehmite colloid, pseudo-boehmite, which has excellent properties of higher gibbs free energy, larger porosity, high specific surface area and the like, and is widely used as a catalytic material, an adsorbent, a binder and a vaccine adjuvant [ Ananthakumar S, manohar P, warrier K G K.Effect of boehmite and organic binders on extrusion of alumina [ J ]].Ceramics international,2004,30(6):837-842.]Etc., and its calcined product gamma-Al 2 O 3 Can be widely used as a catalyst carrier in the petrochemical industry field.
The method for preparing pseudo-boehmite mainly comprises a hydrothermal method, an aluminum alkoxide hydrolysis method, an acid-base method, a sol-gel method, a carbonization method and the like, wherein the hydrothermal synthesis methods such as the hydrothermal aluminum alkoxide method, the hydrothermal aluminum salt method and the hydrothermal crystallization method are widely adopted by domestic and foreign scientific researchers in recent years. For example, wu et al [ Wu X, zhang B, hu Z.Large-scale and additive-free hydrothermal synthesis of lamellar morphology boehmite [ J ]].Powder technology,2013,239:155-161.]Using aluminum nitrate and urea as raw materials, 3031g was charged into a stainless steel autoclave having a capacity of 10LAluminum nitrate, 910g urea and 6L water, and uniformly layered fine crystal structure pseudo-boehmite powder was synthesized on a large scale by a hydrothermal process in the absence of other additives. The method has the defects of high reaction temperature (150 ℃), high preparation cost and high energy consumption in the preparation process.Et al->M,/>Z,I,et al.Nanocrystalline boehmite obtained at room temperature[J].Ceramics International,2018,44(11):12917-12920.]The mesoporous pseudo-boehmite powder is prepared by taking glucose as a template and hydrolyzing Bayer liquor at room temperature. The disadvantage of this preparation method is that a template is required and sulfuric acid is required as a pH adjustor, so that the process is complicated and the added sulfate ions are difficult to remove. Yang et al [ Yang Z, cai W.surfactant-free preparation of mesoporous solid/hollow boehmite and bayerite microspheres via double hydrolysis of NaAlO ] 2 and formamide from room temperature to 180℃[J].Journal of Colloid and Interface Science,2020,564:182-192.]The precipitation rule of pseudo-boehmite in a sodium aluminate-formamide system at 25-180 ℃ is researched, and the pseudo-boehmite microsphere with the congo red adsorption capacity reaching 751.9mg/g is obtained at room temperature. The disadvantage of this process is that the pseudo-boehmite prepared at room temperature does not exist stably, changes to other phases when the reaction time is prolonged, and the precipitant formamide thereof is slightly toxic.
Although the pseudo-boehmite is prepared under certain conditions, the preparation process often needs a pH regulator or is carried out under hydrothermal conditions with higher temperature, so that the preparation cost is higher. Therefore, how to reduce the preparation temperature and stably prepare the single-phase pseudo-boehmite for a long time in a low-temperature reaction environment becomes an important problem to be solved in the preparation process.
Disclosure of Invention
In view of the shortcomings and drawbacks of the prior art, the present invention is directed to a method for stably preparing pseudo-boehmite under mild conditions. The invention takes refined sodium aluminate solution as an aluminum source, which is a main intermediate product in leaching liquid in bauxite in aluminum industry, and cheap and environment-friendly glycol as a precipitator to form a stable glycol-sodium aluminate homogeneous system by a certain proportion, and single-phase pseudo-boehmite powder samples are obtained by controlling the concentration, reaction temperature and reaction time of the sodium aluminate solution.
The invention aims at realizing the following technical scheme:
a method for stably preparing pseudo-boehmite under mild conditions, comprising the following steps:
(1) Dissolving sodium aluminate in water, stirring at room temperature, adding ethylene glycol, and continuously stirring to form a clear mixed solution;
(2) And (3) placing the mixed solution prepared in the step (1) into a reaction kettle for hydrothermal reaction, centrifuging and washing a reaction product to obtain a filter cake, and drying the filter cake to obtain the pseudo-boehmite.
Preferably, the concentration of the sodium aluminate solution in the step (1) is 0.4-0.58mol/L.
Preferably, the volume ratio of the glycol to the sodium aluminate solution in the step (1) is 2:3-3:2.
Preferably, the temperature of the hydrothermal reaction in the step (2) is 50-80 ℃.
Preferably, the hydrothermal reaction in the step (2) is carried out for 2-12 hours.
Preferably, the washing in the step (2) is to wash 3 times with deionized water or wash 3 times with deionized water and then wash 1 time with absolute ethyl alcohol.
Preferably, the drying in step (2) is performed at 60 ℃ for 12 hours.
The specific surface area of the pseudo-boehmite prepared by the invention is 234.6-449.8m 2 Per g, pore volume of 0.13-0.36cm 3 And/g, the average pore diameter is 2.2-4.0nm.
The pseudo-boehmite prepared by the invention can be used as a binder of aluminum silicate refractory fibers, and the calcined product gamma-Al thereof 2 O 3 Can be applied to the fields of catalysis and adsorption.
Compared with the prior art, the invention has the following advantages:
(1) The invention takes sodium aluminate in bauxite leaching liquid as an aluminum source, and the raw materials are cheap and easy to obtain, nontoxic and harmless.
(2) The invention uses cheap and environment-friendly glycol as a precipitator, and has no other auxiliary additives, and the process is simple.
(3) The preparation method expands the preparation process of the single-phase pseudo-boehmite into an environment system with lower temperature, has milder reaction conditions and short reaction time, and can more stably separate out reaction products, namely, the products are still the single-phase pseudo-boehmite along with the extension of the reaction time.
Drawings
Fig. 1 is an SEM image of pseudo-boehmite prepared in example 1.
Fig. 2 is an SEM image of pseudo-boehmite prepared in example 2.
Fig. 3 is an SEM image of pseudo-boehmite prepared in example 2.
Fig. 4 is an SEM image of pseudo-boehmite prepared in example 4.
Fig. 5 is an SEM image of pseudo-boehmite prepared in example 5.
Fig. 6 is an SEM image of pseudo-boehmite prepared in example 6.
Fig. 7 is an SEM image of pseudo-boehmite prepared in example 7.
Fig. 8 is an SEM image of pseudo-boehmite prepared in example 8.
Fig. 9 is an SEM image of pseudo-boehmite prepared in example 9.
Fig. 10 is an XRD pattern of pseudo-boehmite prepared in examples 1-9.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market, and the process parameters which are not specially noted can be carried out by referring to the conventional technology.
The room temperature in the examples is 25 ℃.
Example 1
(1) 0.83g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 2 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times to obtain a filter cake, and drying the filter cake in a blast drier at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 2
(1) 1.0g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 2 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times to obtain a filter cake, and drying the filter cake in a blast drier at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 3
(1) 1.2g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 2 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times to obtain a filter cake, and drying the filter cake in a blast drier at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 4
(1) 1.2g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction for 2 hours at 50 ℃, centrifuging a reaction product, washing the reaction product with deionized water for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time to obtain a filter cake, and drying the filter cake in a blast dryer at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 5
(1) 1.2g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 80 ℃ for 2 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time to obtain a filter cake, and drying the filter cake in a blast dryer at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 6
(1) 1.2g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 6 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times to obtain a filter cake, and drying the filter cake in a blast drier at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 7
(1) 1.2g of sodium aluminate is weighed and dissolved in 25mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 25mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 12 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times to obtain a filter cake, and drying the filter cake in a blast drier at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 8
(1) 1.2g of sodium aluminate is weighed and dissolved in 20mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 30mL of ethylene glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 6 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time to obtain a filter cake, and drying the filter cake in a blast dryer at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Example 9
(1) 1.2g of sodium aluminate is weighed and dissolved in 30mL of deionized water, the solution is magnetically stirred and dissolved at room temperature to obtain sodium aluminate solution, 20mL of glycol is weighed and added into the sodium aluminate solution, and the magnetic stirring is continued for 1min, so that a clear mixed solution is formed;
(2) And (3) placing the mixed solution obtained in the step (1) into a reaction kettle for hydrothermal reaction at 60 ℃ for 6 hours, centrifuging a reaction product, washing the reaction product with deionized water for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time to obtain a filter cake, and drying the filter cake in a blast dryer at 60 ℃ for 12 hours to obtain the pseudo-boehmite.
Table 1 pore Structure parameters of pseudo-boehmite samples prepared in examples
As can be seen from Table 1, the BET specific surface area of the pseudo-boehmite prepared by the invention is 234.6-449.8m 2 Per g, pore volume of 0.13-0.36cm 3 And/g, the average pore diameter is 2.2-4.0nm.
As can be seen from FIGS. 1 to 9, the pseudo-boehmite prepared in example 9 (sodium aluminate concentration of 0.58mol/L, water-alcohol ratio of 3:2, reaction temperature of 60 ℃ C., reaction time of 6 h) has a particle size of micrometer scale and a spherical morphology, and example 9 is a preferred embodiment as compared with pseudo-boehmite prepared in other examples.
As can be seen from fig. 10, all example products described in this scheme are single phase pseudo-boehmite.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (1)
1. A method for stably preparing pseudo-boehmite under mild conditions, which is characterized by comprising the following steps:
(1) Dissolving sodium aluminate in water, stirring at room temperature to obtain sodium aluminate solution, adding ethylene glycol, and continuously stirring to form clear mixed solution; the concentration of the sodium aluminate solution is 0.4-0.58mol/L, and the volume ratio of the glycol to the sodium aluminate solution is 2:3-3:2;
(2) Placing the mixed solution prepared in the step (1) into a reaction kettle for hydrothermal reaction, sequentially centrifuging the reaction product, washing the reaction product with deionized water for 3 times or washing the reaction product with deionized water for 3 times, washing the reaction product with absolute ethyl alcohol for 1 time to obtain a filter cake, and drying the filter cake to obtain pseudo-boehmite; the temperature of the hydrothermal reaction is 60 ℃, and the time of the hydrothermal reaction is 2-12 h; the drying is 12h dried at 60 ℃;
the specific surface area of the pseudo-boehmite is 245.1-449.8 m 2 /g, pore volume of 0.18-0.36 and 0.36cm 3 /g, average pore size of 2.3-4.0. 4.0nm.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120943A (en) * | 1973-04-06 | 1978-10-17 | Asahi Kasei Kogyo Kabushiki Kaisha | Process for producing pseudo-boehmite |
| CN1884082A (en) * | 2006-06-22 | 2006-12-27 | 武汉理工大学 | Method for preparing pseudo-boehmite with large pore volume and high specific surface area |
| CN101704538A (en) * | 2009-11-13 | 2010-05-12 | 武汉理工大学 | Hydrothermal method for preparing series of special-shaped graded pseudo-boehmite |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4120943A (en) * | 1973-04-06 | 1978-10-17 | Asahi Kasei Kogyo Kabushiki Kaisha | Process for producing pseudo-boehmite |
| CN1884082A (en) * | 2006-06-22 | 2006-12-27 | 武汉理工大学 | Method for preparing pseudo-boehmite with large pore volume and high specific surface area |
| CN101704538A (en) * | 2009-11-13 | 2010-05-12 | 武汉理工大学 | Hydrothermal method for preparing series of special-shaped graded pseudo-boehmite |
Non-Patent Citations (1)
| Title |
|---|
| 张蕾等."拟薄水铝石制备技术的研究进展".《山东化工》.2018,第47卷(第14期),第64、69页. * |
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