CN103159243A - Method for producing active alumina by common aluminum-containing compound - Google Patents
Method for producing active alumina by common aluminum-containing compound Download PDFInfo
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- CN103159243A CN103159243A CN2013100723133A CN201310072313A CN103159243A CN 103159243 A CN103159243 A CN 103159243A CN 2013100723133 A CN2013100723133 A CN 2013100723133A CN 201310072313 A CN201310072313 A CN 201310072313A CN 103159243 A CN103159243 A CN 103159243A
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- common aluminum
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Abstract
The invention relates to a method for producing active alumina by a common aluminum-containing compound, which comprises the following steps: adding deionized water while stirring, placing monobasic acid, ammonium nitrate, hexadecyl trimethyl ammonium chloride or ammonium bromide, triton 100, one of span-80 or span-20, one of tween-80 or tween-20 surfactant, and common aluminum-containing compound waste material in a high pressure reaction vessel with a polytetrafluoroethylene lining; wherein, by taking the aluminium in the common aluminum-containing compound waste material, the mol ratio of each components is 50-100: 0.01-0.1: 0.01-3.5: 0.005-0.12: 1; sealing the reaction vessel and heating to 130-220 DEG C, reacting for 1-48 hours at constant temperature for 1-48 hours, stopping heating and cooling to less than 90 DEG C and discharging the material, washing the solid by deionized water for three times, drying the washed solid material at 120 DEG C to make the analysis and detection qualified; placing in a muffle furnace for roasting, and performing ball milling for 0-2 hours to prepare the active alumina.
Description
Technical field
The present invention relates to the method that the common aluminum contained compound of a kind of use is produced activated alumina.
Background technology
Aluminum oxide is to use a kind of raw material very widely, and development trend is mainly reflected in the preparation technology of developing low-cost, environmental protection at present, and the distribution of particle sizes of aluminum oxide is controlled, and improves the chemical reactivity of aluminum oxide.Particularly when aluminum oxide was used for the catalyzer preparation field, its purity and chemical reactivity were just even more important.Generally speaking, oxide of high activity aluminium production alkali process process steps is many, and processing condition are strict, and water consumption is large, and environmental issue is serious.Organic alkoxide isoreactivity intermediate hydrolysis method must be raw material with high-purity metallic aluminium, and good product performance, purity are high.It is raw material that CN1394807A adopts wrought aluminum, adopts the aluminium powder hydrolysis, and then roasting prepares the aluminum oxide of high-purity different crystalline phases.A technical characterictic of these techniques is the active high of product, if but high to the purity requirement of product, must improve production cost with high-purity raw materials such as alkoxide, limited the widespread use of this type of technology.CN1429771A adopts the physical mixed method to reduce the content of impurity.This method is high to the dilution ingredient requirement, and range of application is narrow.
Summary of the invention
The object of the invention is to overcome the problem that prior art exists, the method for producing activated alumina with common aluminum contained compound is provided, utilize the technique of hydrothermal treatment consists associating roasting to control granularity and the activity of product.
Technical scheme of the present invention is: the method that the common aluminum contained compound of a kind of use is produced activated alumina, and concrete steps are as follows:
(1) add deionized water in reactor, start to stir and add successively again monoprotic acid, ammonium nitrate, cats product palmityl trimethyl ammonium chloride or cetyl trimethylammonium bromide, nonionogenic tenside triton x-100, Arlacel-80, Arlacel-20, tween-80, a kind of in tween 20, the common aluminum contained compound waste material of aluminium content 〉=24.35wt% is measured in the autoclave that is placed in respectively with teflon lined in aluminium on demand; Mol ratio between aforementioned each component is followed successively by: 50～100:0.01～0.1:0.01～3.5:0.005～0.12:1;
(2) after closed reactor, be warming up to 130～220 ℃, isothermal reaction 1～48 hour, stopped heating when then being cooled to below 90 ℃, is emitted material, removes supernatant liquid, uses deionized water wash solid three times;
(3) oven dry of the solid materials after washing in 120 ℃ again; Repeating step is (2) one to three times in case of necessity, until the detection of oven dry solid analysis is qualified, and aluminium content 〉=99.8wt%; Then,
(4) step (3) oven dry solid is placed in retort furnace, in 350～750 ℃ of roastings 0.5～6 hour; Material after roasting was processed 0～2 hour with ball mill, made activated alumina.
The method that the common aluminum contained compound of above-mentioned a kind of use is produced activated alumina, its described monoprotic acid is hydrochloric acid, nitric acid, acetic acid or formic acid.
The method that the common aluminum contained compound of above-mentioned a kind of use is produced activated alumina, its described common aluminum contained compound is aluminium hydroxide, aluminum oxide or aluminium salt or its waste material.
The present invention have following marked improvement and positively effect as follows:
1, product purity is high.
2, raw material is cheap and easy to get, and utilizing described common aluminum contained compound (aluminium hydroxide, aluminum oxide or aluminium salt or its waste material) is raw material, the preparation high value added product, to realize the reasonable comprehensive utilization of resource, technological process is simple, good reproducibility, economic benefit are obvious especially.
3, product can be for the preparation of the catalyzer of the molecular sieve that contains aluminium, preparing dimethyl ether from methanol, alumina supporter etc.
4, the present invention utilizes the method for the explained hereafter activated alumina of hydrothermal treatment consists associating roasting, along with the difference of hydrothermal treatment consists condition, can adopt the differing temps roasting, thereby can control granularity and the activity of product.Product is during for the preparation of the SAPO-34 molecular sieve, is that the SAPO-34 molecular sieve initial activity that makes of raw material is high than adopting pseudo-boehmite under identical preparation condition.And adopt molecular sieve decomposition induction time in methanol to olefins reaction that activated alumina of the present invention makes to shorten 32 minutes, the selectivity that ethene adds propylene is high by 0.6%
Embodiment
The invention will be further described below by specific embodiment, but be not to be limitation of the invention.
Embodiment 1～7
The deionized water that adds requirement in the 10L autoclave with teflon lined, start stirring rake, drop into successively again monoprotic acid, ammonium nitrate, palmityl trimethyl ammonium chloride or cetyl trimethylammonium bromide, TritonX-100, Arlacel-80 or Arlacel-20, a kind of in tween-80 or tween 20 tensio-active agent; The common aluminum contained compound of aluminium content 〉=24.35wt% is in aluminium; The mol ratio of above each component is followed successively by 50～100:0.01～0.1:0.01～3.5:0.005～0.12:1;After closed reactor, be warming up to T1 ℃, constant temperature t1 hour, separate and remove supernatant liquid, solid deionized water wash three times.Repeat in case of necessity hydrothermal treatment consists, centrifugation and washing step n time.With the solid materials after washing in 120 ℃ of oven dry, until that solid detects is qualified, aluminium content 〉=99.8wt%; With being placed in retort furnace, in T2 ℃ of roasting t2 hour.Material after roasting was processed t3 hour with ball mill, formulated activated alumina.
The method that the common aluminum contained compound of above-mentioned a kind of use is produced activated alumina, its described monoprotic acid is hydrochloric acid, nitric acid, acetic acid or formic acid.
The method that the common aluminum contained compound of above-mentioned a kind of use is produced activated alumina, its described common aluminum contained compound is aluminium hydroxide, aluminum oxide or aluminium salt or its waste material.
The attached table 1 of concrete technology parameter " activated alumina synthesis condition table "; Product performance see Table 2, " activated alumina performance table ".
Embodiment 8(The application that the activated alumina that makes with the present invention prepares the SAPO-34 molecular sieve
)
The synthetic autoclave that uses with teflon lined.Under agitation condition, add successively 2196g deionized water, 458g activated alumina, 1194g phosphoric acid (H in container
3PO
4Massfraction 85%), stir 1h, add 1134g deionized water, 255g silicon sol (SiO
2Massfraction 29%), stir 2h, add at last 1134g deionized water and 478g Diisopropylamine.Room temperature stirs 5h again.Stop stirring static 24 hours.Begin to heat up, with 1 ℃ of intensification in every 2 minutes, rise to the slurries that 200 ℃ of lower crystallization obtained containing the SAPO-34 molecular sieve in 24 hours, slurries obtain the SAPO-34 molecular sieve through centrifuge washing, drying, roasting.Be the aluminium source with adopting pseudo-boehmite, the SAPO-34 molecular sieve for preparing under similarity condition relatively, molecular sieve output increases, and adopts molecular sieve decomposition induction time in methanol to olefins reaction that activated alumina of the present invention makes to shorten 32 minutes, and the selectivity that ethene adds propylene is high by 0.6%.
Embodiment 9(application that the activated alumina that makes with the present invention prepares the SAPO-34 molecular sieve)
The synthetic autoclave that uses with teflon lined.Under agitation condition, add successively 2196g deionized water, 458g activated alumina, 1194g phosphoric acid (H in container
3PO
4Massfraction 85%), stir 1h, add 1134g deionized water, 255g silicon sol (SiO
2Massfraction 29%), stir 2h, add at last 1134g deionized water and 89g diethylamine and 423g triethylamine.Room temperature stirs 5h again.Stop stirring static 24 hours.Begin to heat up, with 1 ℃ of intensification in every 2 minutes, rise to the slurries that 200 ℃ of lower crystallization obtained containing the SAPO-34 molecular sieve in 24 hours, slurries obtain the SAPO-34 molecular sieve through centrifuge washing, drying, roasting.Be the aluminium source with adopting pseudo-boehmite, the SAPO-34 molecular sieve for preparing under similarity condition relatively, molecular sieve output increases, and adopts molecular sieve decomposition induction time in methanol to olefins reaction that activated alumina of the present invention makes to shorten 32 minutes, and the selectivity that ethene adds propylene is high by 0.65%.
Embodiment 9(activated alumina that makes with the present invention prepares the SAPO-11 molecular sieve)
The synthetic autoclave that uses with teflon lined.Under agitation condition, add successively 2430g deionized water, 469g activated alumina, 1153g phosphoric acid (H in container
3PO
4Massfraction 85%), stir 1h, add 315g deionized water, 621g silicon sol (SiO
2Massfraction 29%), stir 2h, add at last 315g deionized water and 809g di-n-propylamine.Room temperature stirs 5h again.Stop stirring static 24 hours.Begin to heat up, with 1 ℃ of intensification in every 2 minutes, rise to the slurries that 200 ℃ of lower crystallization obtained containing the SAPO-11 molecular sieve in 48 hours, slurries obtain the SAPO-11 molecular sieve through centrifuge washing, drying, roasting.
Embodiment 10(activated alumina that makes with the present invention prepares the SAPO-5 molecular sieve)
The synthetic autoclave that uses with teflon lined.Under agitation condition, add successively 2430g deionized water, 500g activated alumina, 1384g phosphoric acid (H in container
3PO
4Massfraction 85%), stir 1h, add 630g deionized water and 910g triethylamine.Room temperature stirs 5h again.Stop stirring static 24 hours.Begin to heat up, with 1 ℃ of intensification in every 2 minutes, rise to the slurries that 175 ℃ of lower crystallization obtained containing the AlPO-5 molecular sieve in 24 hours, slurries obtain the AlPO-5 molecular sieve through centrifuge washing, drying, roasting.
Embodiment 11(activated alumina that the present invention makes is used for the preparing dimethyl ether from methanol evaluation result)
With in embodiment 1-7 through the solid of 120 ℃ of oven dry, 620 ℃ of roastings 3 hours.Powder is crossed 60-80 mesh sieve through compressing tablet after pulverizing, carry out the preparing dimethyl ether from methanol evaluation.Temperature of reaction is 268 ℃, and pressure is 0.75MPa, and air speed is 2800h
-1, the per pass conversion of methyl alcohol is 78%, the selectivity of dme is 99.1%.
Embodiment 12(activated alumina that the present invention makes is for the preparation of the carrier of catalyzer)
With in embodiment 1～7 through the solid of 120 ℃ of oven dry, 620 ℃ of roastings 3 hours.Powder is through the tabletting machine granulation.The specific surface area of particle is 296m
2/ g, pore volume are that 0.86mL/g, pressure measurement intensity are 161N/cm.Result shows, this activated alumina is suitable for the carrier of Kaolinite Preparation of Catalyst.
Subordinate list 1 composite reactive alumina technology of the present invention condition table look-up
Subordinate list 2 activated alumina performance tables
Claims (3)
1. method of producing activated alumina with common aluminum contained compound, concrete steps are as follows:
(1) stir under with deionized water, monoprotic acid, ammonium nitrate, cats product palmityl trimethyl ammonium chloride or cetyl trimethylammonium bromide, nonionogenic tenside triton x-100, Arlacel-80, Arlacel-20, tween-80, a kind of in tween 20, the common aluminum contained compound of aluminium content 〉=24.35wt% is measured in the autoclave that is placed in respectively with teflon lined in aluminium on demand; Mol ratio between aforementioned each component is followed successively by: 50～100:0.01～0.1:0.01～3.5:0.005～0.12:1;
(2) after closed reactor, be warming up to 130～220 ℃, isothermal reaction 1～48 hour, stopped heating when then being cooled to below 90 ℃, is emitted material, removes supernatant liquid, uses deionized water wash solid three times;
(3) oven dry of the solid materials after washing in 120 ℃ again; Repeating step is (2) one to three times in case of necessity, until the detection of oven dry solid analysis is qualified, and aluminium content 〉=99.8wt%; Then,
(4) solid after step (3) oven dry is placed in retort furnace, in 350～750 ℃ of roastings 0.5～6 hour; Material after roasting was processed 0～2 hour with ball mill, made activated alumina.
2. the common aluminum contained compound of a kind of use according to claim 1 is produced the method for activated alumina, and its described monoprotic acid is hydrochloric acid, nitric acid, acetic acid or formic acid.
3. the common aluminum contained compound of a kind of use method of producing activated alumina according to claim 1, its described common aluminum contained compound is aluminium hydroxide, aluminum oxide, aluminium salt or its waste material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104971779A (en) * | 2014-04-09 | 2015-10-14 | 中国石油化工股份有限公司 | Hydrogenation catalyst and application thereof |
| CN104971693A (en) * | 2014-04-09 | 2015-10-14 | 中国石油化工股份有限公司 | Aluminum moulded material containing nonionic surfactant, preparation and application thereof |
| CN106830033A (en) * | 2017-03-22 | 2017-06-13 | 华东理工大学 | A kind of preparation method of porous flake nano aluminium oxide |
| CN111807393A (en) * | 2020-07-17 | 2020-10-23 | 青岛科技大学 | Method for improving compatibility of aluminum hydroxide |
| CN115518971A (en) * | 2021-06-25 | 2022-12-27 | 中国石油化工股份有限公司 | Method for secondary utilization of MTO waste catalyst |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104971779A (en) * | 2014-04-09 | 2015-10-14 | 中国石油化工股份有限公司 | Hydrogenation catalyst and application thereof |
| CN104971693A (en) * | 2014-04-09 | 2015-10-14 | 中国石油化工股份有限公司 | Aluminum moulded material containing nonionic surfactant, preparation and application thereof |
| CN104971693B (en) * | 2014-04-09 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of aluminum oxide article shaped containing nonionic surface active agent and its preparation and application |
| CN104971779B (en) * | 2014-04-09 | 2017-08-22 | 中国石油化工股份有限公司 | A kind of hydrogenation catalyst and its application |
| CN106830033A (en) * | 2017-03-22 | 2017-06-13 | 华东理工大学 | A kind of preparation method of porous flake nano aluminium oxide |
| CN111807393A (en) * | 2020-07-17 | 2020-10-23 | 青岛科技大学 | Method for improving compatibility of aluminum hydroxide |
| CN115518971A (en) * | 2021-06-25 | 2022-12-27 | 中国石油化工股份有限公司 | Method for secondary utilization of MTO waste catalyst |
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Application publication date: 20130619 |