CN102730726B - Method for preparing boehmite powder by using esterification reaction hydrothermal method - Google Patents
Method for preparing boehmite powder by using esterification reaction hydrothermal method Download PDFInfo
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- CN102730726B CN102730726B CN201210227534.9A CN201210227534A CN102730726B CN 102730726 B CN102730726 B CN 102730726B CN 201210227534 A CN201210227534 A CN 201210227534A CN 102730726 B CN102730726 B CN 102730726B
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Abstract
The invention provides a method and a device for preparing boehmite powder by using an esterification reaction hydrothermal method, which belongs to the field of chemical production technology. Organic acid, organic alcohol, urea and aluminum salt are mixed to react for 6-24 hours when the temperature of the water is 120-200 DEG C. The mixture is cooled naturally to room temperature after reaction. The upper liquid layer is poured out to be reserved as an esterification product. The white precipitate at the bottom and small amount of solution are centrifugally separated, washed by 95% ethanol and absolute ethyl alcohol and placed in a vacuum oven to be dried for 4-8 hours under 80-100 DEG C; The preparation of boehmite ultrafine powder is completed in a liquid phase for only one time. And the water generated by the esterification reaction is used to hydrolyze urea slowly. The reaction with aluminum salt is conducted under hydrothermal condition without additive. The post-treatment process is simple and the morphology of the product is regular. Consuming water generated by the esterification reaction through the hydrolysis of urea can promote the equilibrium movement of the esterification reaction, accelerate the progress of esterification reaction and shorten the reaction time.
Description
Technical field
The invention belongs to chemical production technical field, relate in particular to a kind of method and device that utilizes esterification hydrothermal method to prepare boehmite powder.
Background technology
Boehmite claims again boehmite, and outward appearance presents white powder, and molecular formula is γ-AlOOH.The significant application value of boehmite is after calcining, to prepare industrial broad-spectrum alumina powder jointedly, and its outstanding advantages one is that before and after calcining, the pattern of boehmite remains unchanged, and can obtain easily the alumina product identical with boehmite pattern.The 2nd, owing to comparing from molecular structure, boehmite can be regarded aluminium hydroxide (Al (OH) as
3) lose the product of a part water, so from boehmite, through calcining, prepare aluminum oxide, in energy consumption, be starkly lower than the method for calcinations of aluminum hydroxide.In sum, first preparing the boehmite of different-shape, is the final alumina powder jointed shortcut of corresponding pattern that obtains.So boehmite is also referred to as the presoma of aluminum oxide.
Adopt aluminium salt, Tai-Ace S 150 for example, aluminum nitrate, aluminum chloride etc., under urea exists, by hydro-thermal reaction, can obtain boehmite powder.But due to hydrothermal method long reaction time, need maintain for a long time higher temperature of reaction, the energy consumption of producing separately boehmite powder is relatively high.Esterification refers to utilizes Organic Alcohol and organic acid reaction, when making ester, generate a class reaction of water molecules, follow the generation of ester, can realize slowly and evenly discharging of water molecules, the water that if esterification can be generated, for the hydrolysis of urea, and then under hydrothermal condition, react with aluminium salt, can expect when obtaining esterification product, the little and uniform boehmite powder of by-product granularity.Meanwhile, the consumption of water, can also promote the balance of esterification to move, and is conducive to shorten reaction time of esterification.In the reaction time, can obtain organic esterified product and inorganic superfine powder body simultaneously, be conducive to the comprehensive utilization of energy, energy-saving effect is obvious.
Summary of the invention
The invention provides a kind of method and device that utilizes esterification hydrothermal method to prepare boehmite powder, be intended to solve that prior art provides by aluminium salt, urea, prepares the deficiency of boehmite powder method by hydro-thermal reaction.There is hydrothermal method long reaction time in current preparation method, need maintain for a long time higher temperature of reaction, and the energy consumption of producing separately boehmite powder is relatively high, the problem that production efficiency is low.
The object of the present invention is to provide a kind of method of utilizing esterification hydrothermal method to prepare boehmite powder, the method comprises the following steps:
Organic acid and Organic Alcohol mix, and add a certain amount of urea and aluminium salt, make material A;
The compactedness of material A is controlled to 67-80%, and hydrothermal temperature is controlled at 120-200 ℃, adds hydrothermal reaction kettle reaction 6-24 hour;
After having reacted, stop heating, naturally cool to room temperature, upper liquid layer is poured out, as esterification products, retain;
With the rotating speeds of 4000 revs/min, the white precipitate of bottom and a small amount of solution are carried out to centrifugation, with 95% ethanol and absolute ethanol washing, and be placed in the vacuum drying oven inner drying 4-8 hour of 80-100 ℃, obtain boehmite superfine powder.
Further, with the rotating speeds of 4000 revs/min, the white precipitate of bottom and a small amount of solution are carried out after centrifugation, first use 95% washing with alcohol three times, then use absolute ethanol washing three times.
Further, the aluminium salt in the method can adopt Tai-Ace S 150, aluminum nitrate or aluminum chloride.
Further, the organic acid in the method and Organic Alcohol, can be monoprotic acid, monohydroxy-alcohol, can be also binary and poly-basic organic acid and Organic Alcohol.
Another object of the present invention is to provide a kind of device that utilizes esterification hydrothermal method to prepare boehmite powder, this device comprises:
Be used for heating hydrothermal reaction kettle, make material in hydrothermal reaction kettle reach and maintain the electric heating constant-temperature blowing drying box of the temperature of reaction of appointment;
For holding the centrifuge tube of precipitated product;
Whizzer for centrifugation precipitated product;
Vacuum drying oven for centrifugal rear sample drying.
Further, described hydrothermal reaction kettle consists of inner bag, steel sleeve and fitting nut, and inner bag is used for holding reaction mass, and steel sleeve and fitting nut are used for sealing inner container, and guarantee the material in inner bag, in reaction process, do not reveal.
Further, the inner bag in described hydrothermal reaction kettle adopts tetrafluoroethylene material to make.
Further, the inner bag in described hydrothermal reaction kettle is positioned in steel sleeve; By tightening fitting nut, the inner bag in hydrothermal reaction kettle can be sealed in steel sleeve; By loosening fitting nut, the inner bag in hydrothermal reaction kettle can be taken out in steel sleeve.
Method and the device that utilizes esterification hydrothermal method to prepare boehmite powder provided by the invention, joins organic acid and Organic Alcohol in the inner bag in hydrothermal reaction kettle, adds a certain amount of urea and aluminium salt, obtains material A; The compactedness of material A in hydrothermal reaction kettle is controlled at 67-80%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 120-200 ℃, reaction 6-24 hour; After having reacted, stop heating, naturally cool to room temperature, the inner bag upper liquid layer in hydrothermal reaction kettle is poured out, as esterification products, retain; By the white precipitate of bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol, then use absolute ethanol washing, make between product particle loose, and be placed in the vacuum drying oven inner drying 4-8 hour of 80-100 ℃, obtain boehmite superfine powder; Owing to preparing the reaction of boehmite superfine powder, in liquid phase, once complete, and utilize the water molecules that esterification produces to carry out slow hydrolyze urea, and then under hydrothermal condition, with aluminium reactant salt, prepare boehmite, do not need to use additive, last handling process is simple, the product pattern rule of preparation, is uniformly dispersed; By hydrolysis of urea, consume the water molecules that esterification generates, can also promote the balance of esterification to move, the progress of enhance esterification, Reaction time shorten, has stronger propagation and employment and is worth.
Accompanying drawing explanation
Fig. 1 is that the esterification hydrothermal method of utilizing that the embodiment of the present invention provides is prepared the realization flow figure of the method for boehmite powder;
Fig. 2 is that the esterification hydrothermal method of utilizing that the embodiment of the present invention provides is prepared the structured flowchart of the device of boehmite powder.
In figure: 21, hydrothermal reaction kettle; 22, electric heating constant-temperature blowing drying box; 23, whizzer; 24, centrifuge tube; 25, vacuum drying oven.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is described in further detail.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, and be not used in restriction invention.
The esterification hydrothermal method of utilizing that Fig. 1 shows the embodiment of the present invention to be provided is prepared the realization flow of the method for boehmite powder.
The method comprises the following steps:
In step S101, organic acid and Organic Alcohol mix, and add a certain amount of urea and aluminium salt, make material A;
In step S102, the compactedness of material A is controlled to 67-80%, hydrothermal temperature is controlled at 120-200 ℃, adds hydrothermal reaction kettle reaction 6-24 hour;
In step S103, after having reacted, stop heating, naturally cool to room temperature, pour out upper liquid layer, as esterification products, retain;
In step S104, with the rotating speeds of 4000 revs/min, the white precipitate of bottom and a small amount of solution are carried out to centrifugation, use successively 95% ethanol and absolute ethanol washing, and be placed in the vacuum drying oven inner drying 4-8 hour of 80-100 ℃, obtain boehmite superfine powder.
In embodiments of the present invention, with the rotating speeds of 4000 revs/min, the white precipitate of bottom and a small amount of solution are carried out after centrifugation, first use 95% washing with alcohol three times, then use absolute ethanol washing three times.
In embodiments of the present invention, the aluminium salt in the method can adopt Tai-Ace S 150, aluminum nitrate or aluminum chloride.
In embodiments of the present invention, the organic acid in the method and Organic Alcohol, can be monoprotic acid, monohydroxy-alcohol, can be also binary and poly-basic organic acid and Organic Alcohol.
The esterification hydrothermal method of utilizing that Fig. 2 shows the embodiment of the present invention to be provided is prepared the structure of the device of boehmite powder.For convenience of explanation, only show part related to the present invention.
This device comprises: hydrothermal reaction kettle 21, electric heating constant-temperature blowing drying box 22, whizzer 23, centrifuge tube 24, vacuum drying oven 25;
Hydrothermal reaction kettle 21 consists of inner bag, steel sleeve and fitting nut, and inner bag is used for holding reaction mass, and steel sleeve and fitting nut are used for sealing inner container, and guarantee the material in inner bag, in reaction process, do not reveal; Electric drying oven with forced convection 22 is for heating hydrothermal reaction kettle 21, makes material in inner bag reach and maintain the temperature of reaction of appointment; Centrifuge tube 24 is for holding precipitated product, and whizzer 23 is for centrifugation precipitated product; Vacuum drying oven 25 is dry for centrifugal rear sample.
In embodiments of the present invention, the inner bag in hydrothermal reaction kettle 21 adopts tetrafluoroethylene material to make.
In embodiments of the present invention, the inner bag in hydrothermal reaction kettle 21 is positioned in steel sleeve.
In embodiments of the present invention, by tightening fitting nut, the inner bag in hydrothermal reaction kettle can be sealed in steel sleeve.
In embodiments of the present invention, by loosening fitting nut, the inner bag in hydrothermal reaction kettle can be taken out in steel sleeve.
In embodiments of the present invention, hydrothermal reaction kettle 21 is positioned in electric drying oven with forced convection 22 and heats.
In embodiments of the present invention, centrifuge tube 24 is arranged on whizzer 23.
Below in conjunction with drawings and the specific embodiments, application principle of the present invention is further described.
As shown in Figures 1 and 2, embodiment 1: first, the dehydrated alcohol of 30ml (0.5mol) Glacial acetic acid and 45ml is joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.5mol, 9 grams, consider the solubleness of Tai-Ace S 150 in water, and suitably leave surplus, therefore add the Tai-Ace S 150 of 0.004 mole and the urea of 0.015 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 75%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 150 ℃, react 24 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 8 hours of 80 ℃, obtain boehmite superfine powder,
Embodiment 2: first, the dehydrated alcohol of 30ml (0.5mol) Glacial acetic acid and 50ml is joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.5mol, 9 grams, consider the solubleness of aluminum nitrate in water, and suitably leave surplus, therefore add the aluminum nitrate of 0.01 mole and the urea of 0.02 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 80%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 180 ℃, react 18 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 7 hours of 90 ℃, obtain boehmite superfine powder,
Embodiment 3: first, the dehydrated alcohol of 30ml (0.5mol) Glacial acetic acid and 50ml is joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.5mol, 9 grams, consider the solubleness of aluminum chloride in water, and suitably leave surplus, therefore add the aluminum chloride of 0.015 mole and the urea of 0.03 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 80%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 160 ℃, react 12 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 6 hours of 100 ℃, obtain boehmite superfine powder,
Embodiment 4: first, the dehydrated alcohol of 45ml (0.6mol) propionic acid and 35ml is joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.6mol, 10.8 grams, consider the solubleness of aluminum chloride in water, and suitably leave surplus, therefore add the aluminum chloride of 0.02 mole and the urea of 0.04 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 80%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 150 ℃, react 24 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 8 hours of 80 ℃, obtain boehmite superfine powder,
Embodiment 5: first, 37ml (0.4mol) butanic acid and 38ml propyl carbinol are joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.4mol, 7.2 grams, consider the solubleness of aluminum nitrate in water, and suitably leave surplus, therefore add the aluminum nitrate of 0.01 mole and the urea of 0.02 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 75%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 180 ℃, react 18 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 7 hours of 80 ℃, obtain boehmite superfine powder,
Embodiment 6: first, the isopropylcarbinol of 30ml (0.5mol) Glacial acetic acid and 50ml is joined in the inner bag in hydrothermal reaction kettle 21, the present embodiment esterification theoretical water output is 0.5mol, 9 grams, consider the solubleness of Tai-Ace S 150 in water, and suitably leave surplus, therefore add the Tai-Ace S 150 of 0.004 mole and the urea of 0.015 mole, compactedness in hydrothermal reaction kettle 21 is controlled at 80%, sealing hydrothermal reaction kettle 21, be placed in electric heating constant-temperature blowing drying box 22, hydrothermal temperature is controlled to 160 ℃, react 12 hours, after finishing, reaction naturally cools to room temperature, finally open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain, then, by the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in vacuum drying oven 25 inner drying 6 hours of 90 ℃, can obtain boehmite superfine powder.
The esterification hydrothermal method of utilizing that the embodiment of the present invention provides is prepared method and the device of boehmite powder, and organic acid and Organic Alcohol are joined in the inner bag in hydrothermal reaction kettle 21, adds a certain amount of urea and aluminium salt, obtains material A; The compactedness of material A in hydrothermal reaction kettle 21 is controlled at 67-80%, and sealing hydrothermal reaction kettle 21, is placed in electric heating constant-temperature blowing drying box 22, and hydrothermal temperature is controlled to 120-200 ℃, reaction 6-24 hour; After having reacted, stop heating, naturally cool to room temperature, open hydrothermal reaction kettle 21, inner bag upper liquid layer is poured out, as esterification products, retain; By the white precipitate of bottom and a small amount of solution, pour in centrifuge tube 24, put into whizzer 23, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol, then use absolute ethanol washing, make between product particle loose, and be placed in the vacuum drying oven 25 inner drying 4-8 hour of 80-100 ℃, obtain boehmite superfine powder; Owing to preparing the reaction of boehmite superfine powder, in liquid phase, once complete, and utilize the water molecules that esterification produces to carry out slow hydrolyze urea, and then under hydrothermal condition, with aluminium reactant salt, prepare boehmite, do not need to use additive, last handling process is simple, the product pattern rule of preparation, is uniformly dispersed; By hydrolysis of urea, consume the water molecules that esterification generates, can also promote the balance of esterification to move, the progress of enhance esterification, Reaction time shorten, has stronger propagation and employment and is worth.
These are only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, be equal to and replace and improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. utilize esterification hydrothermal method to prepare a method for boehmite powder, it is characterized in that, by following steps, formed:
The dehydrated alcohol of 30mL 0.5mol Glacial acetic acid and 45mL is joined in the inner bag of hydrothermal reaction kettle, add the Tai-Ace S 150 of 0.004 mole and the urea of 0.015 mole;
The compactedness of hydrothermal reaction kettle inner bag is controlled at 75%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 150 ℃, reacts 24 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
By the white precipitate of inner bag bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol three times, then use absolute ethanol washing three times, make between product particle loose, and be placed in the vacuum drying oven inner drying 8 hours of 80 ℃, obtain boehmite superfine powder.
2. the method for utilizing esterification hydrothermal method to prepare boehmite powder as claimed in claim 1, is characterized in that, following steps, consists of:
The dehydrated alcohol of 30mL 0.5mol Glacial acetic acid and 50mL is joined in the inner bag of hydrothermal reaction kettle, add the aluminum nitrate of 0.01 mole and the urea of 0.02 mole;
Compactedness in hydrothermal reaction kettle inner bag is controlled at 80%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 180 ℃, reacts 18 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
Then, by the white precipitate of inner bag bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in the vacuum drying oven inner drying 7 hours of 90 ℃, obtain boehmite superfine powder.
3. the method for utilizing esterification hydrothermal method to prepare boehmite powder as claimed in claim 1, is characterized in that, following steps, consists of:
The dehydrated alcohol of 30mL 0.5mol Glacial acetic acid and 50mL is joined in the inner bag of hydrothermal reaction kettle, add the aluminum chloride of 0.015 mole and the urea of 0.03 mole;
The compactedness of hydrothermal reaction kettle inner bag is controlled at 80%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 160 ℃, reacts 12 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
By the white precipitate of bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol three times, then use absolute ethanol washing three times, make between product particle loose, and be placed in the vacuum drying oven inner drying 6 hours of 100 ℃, obtain boehmite superfine powder.
4. the method for utilizing esterification hydrothermal method to prepare boehmite powder as claimed in claim 1, is characterized in that, following steps, consists of:
The dehydrated alcohol of 45mL 0.6mol propionic acid and 35mL is joined in the inner bag of hydrothermal reaction kettle, add the aluminum chloride of 0.02 mole and the urea of 0.04 mole;
The compactedness of hydrothermal reaction kettle inner bag is controlled at 80%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 150 ℃, reacts 24 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
By the white precipitate of inner bag bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol three times, then use absolute ethanol washing three times, make between product particle loose, and be placed in the vacuum drying oven inner drying 8 hours of 80 ℃, obtain boehmite superfine powder.
5. the method for utilizing esterification hydrothermal method to prepare boehmite powder as claimed in claim 1, is characterized in that, following steps, consists of:
The dehydrated alcohol of 37mL0.4mol butanic acid and 38mL is joined in the inner bag of hydrothermal reaction kettle, add the aluminum nitrate of 0.01 mole and the urea of 0.02 mole;
Compactedness in hydrothermal reaction kettle inner bag is controlled at 75%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 180 ℃, reacts 18 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
Then, by the white precipitate of inner bag bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, with the rotating speed centrifugation of 4000 revs/min, with after 95% washing with alcohol three times, use again absolute ethanol washing three times, make between product particle loosely, and be placed in the vacuum drying oven inner drying 7 hours of 80 ℃, obtain boehmite superfine powder.
6. the method for utilizing esterification hydrothermal method to prepare boehmite powder as claimed in claim 1, is characterized in that, following steps, consists of:
The isopropylcarbinol of 30mL0.5mol Glacial acetic acid and 50mL is joined in the inner bag of hydrothermal reaction kettle, add the Tai-Ace S 150 of 0.004 mole and the urea of 0.015 mole;
The compactedness of hydrothermal reaction kettle inner bag is controlled at 80%, and sealing hydrothermal reaction kettle, is placed in electric heating constant-temperature blowing drying box, and hydrothermal temperature is controlled to 160 ℃, reacts 12 hours;
After reaction finishes, naturally cool to room temperature, open hydrothermal reaction kettle, inner bag upper liquid layer is poured out, as esterification products, retain;
By the white precipitate of bottom and a small amount of solution, pour in centrifuge tube, put into whizzer, rotating speed centrifugation with 4000 revs/min, with after 95% washing with alcohol three times, then use absolute ethanol washing three times, make between product particle loose, and be placed in the vacuum drying oven inner drying 6 hours of 90 ℃, obtain boehmite superfine powder.
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| DE10332775A1 (en) * | 2003-07-17 | 2005-02-17 | Sasol Germany Gmbh | Process for the preparation of boehmitic clays with a high a-transformation temperature |
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| 佚名.《全国中等物资学校试用教材 化工原材料》.《全国中等物资学校试用教材 化工原材料》.中国物资出版社,1988,(第1版),第181页. |
| 佚名.《全国中等物资学校试用教材 化工原材料》.《全国中等物资学校试用教材 化工原材料》.中国物资出版社,1988,(第1版),第181页. * |
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