CN103449484A - Method for continuously producing pseudoboehmite - Google Patents
Method for continuously producing pseudoboehmite Download PDFInfo
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- CN103449484A CN103449484A CN2013103740431A CN201310374043A CN103449484A CN 103449484 A CN103449484 A CN 103449484A CN 2013103740431 A CN2013103740431 A CN 2013103740431A CN 201310374043 A CN201310374043 A CN 201310374043A CN 103449484 A CN103449484 A CN 103449484A
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- boehmite
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Abstract
The invention discloses a method for continuously producing pseudoboehmite, belonging to the technical field of boehmite preparation. The method comprises the following steps: continuously adding a sodium metaaluminate solution into a reactor while introducing an air-carbon dioxide gas mixture, and forming a strong liquid flow of the sodium metaaluminate solution to be thoroughly mixed with the carbon dioxide gas; controlling the flow rates of the gas mixture and the sodium metaaluminate solution to control the temperature of the slurry generated by reaction at 25-55 DEG C and the pH value at 9.5-11; and after the slurry passes through a pipeline with a plurality of U-shaped bends, aging the slurry, filtering, washing with water, and drying to obtain the pseudoboehmite. The pseudoboehmite prepared by the method has the characteristics of large specific area and pore volume, reasonable peptization, continuous production, simple technique, high production efficiency, stable product quality, low equipment investment, reliable operation, low energy consumption, low labor intensity and the like, is convenient to operate and maintain, and is especially suitable for producing common pseudoboehmite, superfine aluminum hydroxide or aluminum oxide.
Description
Technical field
The present invention relates to aluminium standby technical field, particularly a kind of method of continuous production pseudo-boehmite made of stones.
Background technology
Pseudo-boehmite claims again monohydrate alumina, false boehmite, nontoxic, tasteless, odorless, white colloidal (wet product) or powder (dry product), crystalline phase purity is high, peptization performance good, and cohesiveness is strong, have the characteristics such as specific surface is high, pore volume is large, it is thixotropy gel containing aquosity.
The production method of pseudo-boehmite has multiple: the current external normal aluminium alcoholates method that adopts, and the high and pore structure of quality product is easy to control, but production cost is high, has environmental pollution; At present domestic most economical, most widely used be acid system or alkaline process.The production method of industrial pseudo-boehmite mainly comprises following three kinds:
(1) neutralization of aluminium salt and alkali:
AlCl
3+3NH
3OH——>Al(OH)
3+3NH
4Cl
(2) the replacement(metathesis)reaction method of aluminium salt and sodium metaaluminate:
Al
2(SO
4)
3+6NaAlO
2＋12H
2O——>8Al(OH)
3＋3Na
2SO
4
(3) sodium metaaluminate and sour neutralization, as carborization:
2NaAlO
2＋CO
2＋3H
2O——>2Al(OH)
3＋Na
2CO
3
Wherein, the process that carborization is produced pseudo-boehmite is as follows: the industrial sodium aluminate solution of low-temperature and low-concentration of take is raw material, passes into fast high concentration CO
2gas, as in precipitation agent and plastic, is controlled the pH value of plastic temperature and terminal, then, through intensification, aging, washing, drying, obtains common pseudo-boehmite product.
Carborization prepares pseudo-boehmite can rely on alumina producer, and raw material sources are extensive, production cost is low, and the waste liquid in production can recycle in the returning alumina Production Flow Chart, substantially without waste material, discharges, and environmental pollution is little, is widely used thus.But the process that carborization prepares pseudo-boehmite mostly is interruption production, facility investment is large, personnel labor intensity is large, productivity is low, and the quality product fluctuation is large.
Summary of the invention
The interruption production for preparing pseudo-boehmite in order to solve existing carborization, labour intensity is large, productivity is low, and the problem such as the quality product fluctuation is large, the invention provides a kind of method of continuous production pseudo-boehmite, comprising:
Sodium aluminate solution is joined in reaction unit continuously, and the mixed gas of air and carbonic acid gas is passed in described reaction unit, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide; Control the flow of mixed gas and sodium aluminate solution, the slurry temperature that reaction is generated is 25～55 ℃, and the pH value is 9.5～11; The slip of reaction gained is delivered to ageing tank by having the curved pipeline of a plurality of u-shapeds, and that slip carries out is aging, filter, be washed to neutrality and drying treatment, obtains pseudo-boehmite.
The alumina concentration of described sodium aluminate solution is 15～80g/L.
Described slip through overaging, the step of filtering, be washed to neutrality and drying treatment specifically comprises:
Slip enters ageing tank and heats up after containing the curved pipeline of a plurality of u-shapeds, controls aging temperature and is not less than 90 ℃;
By the slurry filtration after aging intensification, filter cake is washed to neutrality;
Filter cake after washing is carried out to drying treatment.
The drying temperature of described drying treatment is 100～120 ℃.
The percent by volume of described carbon dioxide in gas mixture is 30%～100%, and the pressure of described mixed gas is 0.1MPa～0.3MPa.
The flow ratio of described mixed gas and sodium aluminate solution is 10～100.
The characteristics such as method of the present invention has continuous production, technique is simple, production efficiency is high, constant product quality, facility investment are few, simple and convenient operation and maintenance, reliable, energy consumption low and labour intensity is little, be specially adapted to the production of common pseudo-boehmite or ultrafine aluminium hydroxide, aluminum oxide.The prepared pseudo-boehmite by the inventive method, specific surface area is large, pore volume, peptization are reasonable.
The accompanying drawing explanation
Fig. 1 is the method flow diagram of the continuous production pseudo-boehmite of the embodiment of the present invention.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further described.
Referring to Fig. 1, the embodiment of the present invention provides a kind of method of continuous production pseudo-boehmite, and the method comprises the steps:
Step 101: join continuously in reaction unit by sodium aluminate solution, and the mixed gas of air and carbonic acid gas is passed in this reaction unit, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble;
In the present embodiment, the alumina concentration of sodium aluminate solution is 15～80g/L; The percent by volume of carbon dioxide in gas mixture is 30%～100%, and the pressure of mixed gas is 0.1MPa～0.3MPa;
Step 102: control the flow ratio of mixed gas and sodium aluminate solution 10～100, the slurry temperature that reaction is generated is 25～55 ℃, and the pH value is 9.5～11, stops plastic;
Step 103: the slip that will react gained is by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slip through overaging, filter, be washed to neutrality and drying treatment, obtain pseudo-boehmite.
In the present embodiment, slip by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank and heat up, is controlled to aging temperature and is not less than 90 ℃; By the slurry filtration after aging intensification, filter cake is washed to neutrality; Again the filter cake after washing is carried out to drying treatment, drying temperature is 100～120 ℃, finally obtains pseudo-boehmite.
Method for the continuous production pseudo-boehmite of more clearly setting forth the embodiment of the present invention, further illustrate below by several typical Application Examples.
Embodiment 1
The sodium aluminate solution that is 15.3g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 30%, the pressure of mixed gas is 0.1MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 10, and the slurry temperature that reaction is generated is that 25 ℃ and pH value are 9.5 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 90 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 100 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 2
The sodium aluminate solution that is 23.5g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 40%, the pressure of mixed gas is 0.12MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 30, and the slurry temperature that reaction is generated is that 30 ℃ and pH value are 9.5 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 95 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 102 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 3
The sodium aluminate solution that is 35.3g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 50%, the pressure of mixed gas is 0.15MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 40, and the slurry temperature that reaction is generated is that 35 ℃ and pH value are 10 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 100 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 102 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 4
The sodium aluminate solution that is 43.1g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 60%, the pressure of mixed gas is 0.2MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 50, and the slurry temperature that reaction is generated is that 40 ℃ and pH value are 10 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 98 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 110 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 5
The sodium aluminate solution that is 51.9g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 70%, the pressure of mixed gas is 0.25MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 60, and it is 11 o'clock with the pH value that the slurry temperature that reaction is generated is 45 ℃, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 97 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 115 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 6
The sodium aluminate solution that is 67.4g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 80%, the pressure of mixed gas is 0.3MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 80, and the slurry temperature that reaction is generated is that 50 ℃ and pH value are 11 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 93 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 120 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Embodiment 7
The sodium aluminate solution that is 78.83g/L by alumina concentration joins in reaction unit by pump continuously, pass into the mixed gas of air and carbonic acid gas, the percent by volume of carbon dioxide in gas mixture is 100%, the pressure of mixed gas is 0.3MPa, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide, produce many and fine and smooth bubble; The flow ratio of controlling mixed gas and sodium aluminate solution is 100, and the slurry temperature that reaction is generated is that 55 ℃ and pH value are 10.5 o'clock, stops plastic; By the slip of reaction gained, by sufficiently long and have the curved pipeline of a plurality of u-shapeds and be delivered to ageing tank, slurry heats up in ageing tank, and aging temperature is 94 ℃; By the slurry filtration after aging, filter cake is washed to neutrality; Filter cake after washing is carried out to drying and processing, and bake out temperature is 120 ℃, finally obtains common pseudo-boehmite product, and its physico-chemical property sees the following form 1.
Table 1
| Character | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Peptization, % | 97.1 | 96.1 | 95.6 | 97.5 | 96.4 | 98.1 | 96.9 |
| Specific surface, m 2/g | 289.02 | 341.3 | 345.43 | 298.44 | 325.81 | 356.66 | 394.52 |
| Pore volume, ml/L | 0.33 | 0.31 | 0.31 | 0.36 | 0.30 | 0.31 | 0.32 |
As can be seen from Table 1, the prepared pseudo-boehmite by the method for the present embodiment, specific surface area is large, pore volume, peptization are reasonable.The analysis of pore volume and specific surface area in table 1, can adopt the low temperature liquid nitrogen absorption method to complete.(annotate: in common pseudo-boehmite quality standard Q/Chalco A020-2004, peptization>=95%, specific surface>=250m
2/ g, pore volume>=0.3ml/L)
The present embodiment joins sodium aluminate solution in reaction unit continuously with pump, sufficiently long and there is the curved transport pipe of a plurality of u-shapeds and guaranteed fully carrying out of carburizing reagent, overcome pseudo-boehmite and be interrupted the defect of producing, there is continuous production, the characteristics such as technique is simple, facility investment is few, simple and convenient operation and maintenance, reliable, energy consumption is low and labour intensity is little, improved the work production rate, stablize quality product, be specially adapted to the production of common pseudo-boehmite or ultrafine aluminium hydroxide, aluminum oxide.
Above-described specific embodiment; purpose of the present invention, technical scheme and beneficial effect are further described; institute is understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any modification of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (6)
1. a method of producing continuously pseudo-boehmite, is characterized in that, comprising:
Sodium aluminate solution is joined in reaction unit continuously, and the mixed gas of air and carbonic acid gas is passed in described reaction unit, make sodium aluminate solution form powerful liquid stream and fully mix with carbon dioxide; Control the flow of mixed gas and sodium aluminate solution, the slurry temperature that reaction is generated is 25～55 ℃, and the pH value is 9.5～11; By the reaction gained slip be delivered to ageing tank by thering is the curved pipeline of a plurality of u-shapeds, slip through overaging, filter, be washed to neutrality and drying treatment, obtain pseudo-boehmite.
2. the method for continuous production pseudo-boehmite as claimed in claim 1, is characterized in that, the alumina concentration of described sodium aluminate solution is 15～80g/L.
3. the method for continuous production pseudo-boehmite as claimed in claim 1, is characterized in that, described slip through overaging, the step of filtering, be washed to neutrality and drying treatment specifically comprises:
Slip is passed into to ageing tank and heat up, control aging temperature and be not less than 90 ℃;
By the slurry filtration after aging intensification, filter cake is washed to neutrality;
Filter cake after washing is carried out to drying treatment.
4. the method for continuous production pseudo-boehmite as claimed in claim 3, is characterized in that, the drying temperature of described drying treatment is 100～120 ℃.
5. the method for continuous production pseudo-boehmite as claimed in claim 1, is characterized in that, the percent by volume of described carbon dioxide in gas mixture is 30%～100%, and the pressure of described mixed gas is 0.1MPa～0.3MPa.
6. the method for continuous production pseudo-boehmite as claimed in claim 1, is characterized in that, the flow ratio of described mixed gas and sodium aluminate solution is 10～100.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104959091A (en) * | 2015-06-08 | 2015-10-07 | 辽宁石油化工大学 | Carbonization synthesis system and application of same in preparation of pseudo-boehmite, and preparation method for pseudo-boehmite |
| CN104973613A (en) * | 2015-06-25 | 2015-10-14 | 厦门大学 | Method for continuously producing aluminum oxide by using carbonation method |
| CN105600812A (en) * | 2015-12-24 | 2016-05-25 | 江苏晶晶新材料有限公司 | Method for preparing high-viscosity and superfine pseudo boehmite coating adhesive |
| CN107200339A (en) * | 2017-05-31 | 2017-09-26 | 广西壮族自治区化工研究院 | A kind of method for preparing boehmite |
| CN111377466A (en) * | 2018-12-27 | 2020-07-07 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite and alumina prepared by same |
| CN113461408A (en) * | 2021-07-22 | 2021-10-01 | 杭州智华杰科技有限公司 | Method for improving strength of activated alumina balls |
| CN114426297A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Method for continuously preparing pseudoboehmite |
| CN114506865A (en) * | 2020-10-29 | 2022-05-17 | 中国石油化工股份有限公司 | Aluminum hydroxide and method for preparing aluminum hydroxide by carbonization method |
| CN115724448A (en) * | 2022-11-21 | 2023-03-03 | 岳阳慧璟新材料科技有限公司 | Process method for preparing pseudo-boehmite by continuous carbonization |
| CN115974113A (en) * | 2022-12-23 | 2023-04-18 | 中科催化新技术(大连)股份有限公司 | Method for synthesizing high-peptization pseudo-boehmite by taking carbon dioxide as raw material |
| CN116395723A (en) * | 2023-03-09 | 2023-07-07 | 中铝山东新材料有限公司 | Pseudo-boehmite for hydrocracking and preparation method thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104959091A (en) * | 2015-06-08 | 2015-10-07 | 辽宁石油化工大学 | Carbonization synthesis system and application of same in preparation of pseudo-boehmite, and preparation method for pseudo-boehmite |
| CN104973613A (en) * | 2015-06-25 | 2015-10-14 | 厦门大学 | Method for continuously producing aluminum oxide by using carbonation method |
| CN105600812A (en) * | 2015-12-24 | 2016-05-25 | 江苏晶晶新材料有限公司 | Method for preparing high-viscosity and superfine pseudo boehmite coating adhesive |
| CN107200339A (en) * | 2017-05-31 | 2017-09-26 | 广西壮族自治区化工研究院 | A kind of method for preparing boehmite |
| CN111377466A (en) * | 2018-12-27 | 2020-07-07 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite and alumina prepared by same |
| CN111377466B (en) * | 2018-12-27 | 2022-09-09 | 中国石油化工股份有限公司 | Preparation method of pseudo-boehmite and alumina prepared by same |
| CN114426297A (en) * | 2020-10-29 | 2022-05-03 | 中国石油化工股份有限公司 | Method for continuously preparing pseudoboehmite |
| CN114506865A (en) * | 2020-10-29 | 2022-05-17 | 中国石油化工股份有限公司 | Aluminum hydroxide and method for preparing aluminum hydroxide by carbonization method |
| CN114426297B (en) * | 2020-10-29 | 2023-07-28 | 中国石油化工股份有限公司 | Method for continuously preparing pseudo-boehmite |
| CN114506865B (en) * | 2020-10-29 | 2023-10-10 | 中国石油化工股份有限公司 | Method for preparing aluminum hydroxide by aluminum hydroxide and carbonization method |
| CN113461408A (en) * | 2021-07-22 | 2021-10-01 | 杭州智华杰科技有限公司 | Method for improving strength of activated alumina balls |
| CN115724448A (en) * | 2022-11-21 | 2023-03-03 | 岳阳慧璟新材料科技有限公司 | Process method for preparing pseudo-boehmite by continuous carbonization |
| CN115974113A (en) * | 2022-12-23 | 2023-04-18 | 中科催化新技术(大连)股份有限公司 | Method for synthesizing high-peptization pseudo-boehmite by taking carbon dioxide as raw material |
| CN116395723A (en) * | 2023-03-09 | 2023-07-07 | 中铝山东新材料有限公司 | Pseudo-boehmite for hydrocracking and preparation method thereof |
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