CN113086999A - Novel preparation method of titanium modified activated alumina dry glue - Google Patents
Novel preparation method of titanium modified activated alumina dry glue Download PDFInfo
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- CN113086999A CN113086999A CN202110407110.XA CN202110407110A CN113086999A CN 113086999 A CN113086999 A CN 113086999A CN 202110407110 A CN202110407110 A CN 202110407110A CN 113086999 A CN113086999 A CN 113086999A
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 16
- 239000010936 titanium Substances 0.000 title claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000003292 glue Substances 0.000 title claims abstract description 9
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 17
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 16
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 16
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000032683 aging Effects 0.000 claims abstract description 12
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 28
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims 6
- 239000011148 porous material Substances 0.000 abstract description 23
- 230000007547 defect Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 4
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 6
- 239000000969 carrier Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/14—Aluminium oxide or hydroxide from alkali metal aluminates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention provides a new preparation method of titanium modified activated alumina dry glue, which comprises the following steps: step one, adding quantitative pure water into a reactor, and under the condition of stirring, carrying out parallel flow neutralization on a titanium tetrachloride water solution, an aluminum sulfate solution and a sodium metaaluminate solution to form gel; and step two, aging, washing, drying and crushing the finished product gelatinized in the step one to obtain the activated alumina. The invention has the beneficial effects that: in the preparation process, an inorganic titanium source with low price is adopted, so that the problem of wastewater treatment is reduced, and the preparation process adopts a conventional activated alumina preparation method, so that the process is simple and the cost is low. The prepared product titanium oxide is uniformly dispersed on the surface of the alumina, has better pore structure index, and overcomes the defects of uneven dispersion of elements, poorer pore structure and lower pore diameter of the conventional modified alumina.
Description
Technical Field
The invention relates to the field of preparation of alumina dry gel, in particular to a novel preparation method of titanium modified activated alumina dry gel.
Background
The active alumina is widely used as a common carrier material of the catalyst, but most of the catalysts are basically added with other basic elements to prepare carriers, such as Si, P, Ti, B, F and the like, and active components are loaded after the carriers are prepared, and the elements are added for the main purpose of adjusting the acidity and the pore structure of the catalyst or improving the distribution of the active components on the carriers and the interaction between the active components and the carriers.
The addition of such elements in the catalyst preparation process is likely to cause the problems of complex preparation process, uneven dispersion, difficult molding and the like.
Disclosure of Invention
The invention overcomes the defects in the prior art and provides a novel preparation method of titanium modified activated alumina dry glue.
The purpose of the invention is realized by the following technical scheme.
A new preparation raw material of titanium modified active alumina dry glue comprises a titanium tetrachloride aqueous solution and an aluminum source.
Preferably, the aluminum source is aluminum sulfate and sodium metaaluminate.
Preferably, the concentration of the aluminum oxide in the aluminum sulfate solution is 50-80g/L, and the acid-base ratio is 1.4-1.7.
Preferably, the concentration of the aluminum oxide in the aluminum sulfate solution is 65g/L, and the pH ratio is 1.55.
Preferably, the concentration of the aluminum oxide in the sodium metaaluminate solution is 150-220 g/L.
Preferably, the concentration of the aluminum oxide in the sodium metaaluminate solution is 180 g/L.
In the above aspect, it is preferable that the titanium oxide concentration in the titanium tetrachloride aqueous solution is 50 to 100 g/L.
In the above aspect, it is preferable that the titanium oxide concentration in the titanium tetrachloride aqueous solution is 70 g/L.
A new preparation method of titanium modified activated alumina dry gel comprises the following steps:
step one, adding quantitative pure water into a reactor, and under the condition of stirring, carrying out parallel flow neutralization on a titanium tetrachloride water solution, an aluminum sulfate solution and a sodium metaaluminate solution to form gel;
and step two, aging, washing, drying and crushing the finished product gelatinized in the step one to obtain the activated alumina.
Preferably, in the above scheme, the concentration of the aluminum oxide in the aluminum sulfate solution in the first step is 50-80g/L, and the pH ratio is 1.4-1.7.
Preferably, in the above scheme, the concentration of aluminum oxide in the aluminum sulfate solution in the first step is 65g/L, and the pH ratio is 1.55.
Preferably, in the first step, the concentration of alumina in the sodium metaaluminate solution is 150-220 g/L.
Preferably, in the above scheme, the concentration of alumina in the sodium metaaluminate solution in the first step is 180 g/L.
Preferably, in the above scheme, the titanium oxide concentration in the titanium tetrachloride aqueous solution in the first step is 50 to 100 g/L.
Preferably, in the above scheme, the titanium oxide concentration in the titanium tetrachloride aqueous solution in the first step is 70 g/L.
Preferably, the neutralization water amount in the first step is 10-50L per kilogram of aluminum oxide, the pH value of the gel is 5-10, and the neutralization temperature is 50-90 ℃.
Preferably, the aging time in the second step is 10-80min, and the aging pH value is 8-11.
Preferably, the aging time in the second step is 20min, and the aging pH value is 9.
Preferably, the drying temperature in the second step is 100-200 ℃.
Preferably, the drying temperature in the second step is 130 ℃.
Drawings
FIG. 1 is a BET-adsorption-test result chart;
FIG. 2 is an isotherm-line graph;
FIG. 3 is an isotherm-Log plot;
figure 4 BJH-adsorption-pore size distribution-graph.
The invention has the beneficial effects that:
in the preparation process, an inorganic titanium source with low price is adopted, so that the problem of wastewater treatment is reduced, and the preparation process adopts a conventional activated alumina preparation method, so that the process is simple and the cost is low. The prepared product titanium oxide is uniformly dispersed on the surface of the alumina, has better pore structure index, and overcomes the defects of uneven dispersion of elements, poorer pore structure and lower pore diameter of the conventional modified alumina.
The main physical and chemical property indexes of the product are that the content of titanium oxide is 15-25%, the pore volume is 0.8-1.0ml/g, the specific surface area is larger than 270-2The/g, average pore diameter is 10-15nm, can be used for preparing hydrotreating catalyst with larger pore diameter.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Firstly, preparation
A raw material for preparing titanium modified active alumina dry glue comprises a titanium tetrachloride aqueous solution and an aluminum source; preferably, the aluminum source is aluminum sulfate and sodium metaaluminate.
The concentration of aluminum oxide in the aluminum sulfate solution is 50-80g/L, and the acid-base ratio is 1.4-1.7; preferably, the concentration of aluminum oxide in the aluminum sulfate solution is 65g/L, and the pH ratio is 1.55.
Wherein the concentration of the aluminum oxide in the sodium metaaluminate solution is 150-220g/L, and preferably, the concentration of the aluminum oxide in the sodium metaaluminate solution is 180 g/L.
Wherein the concentration of titanium oxide in the titanium tetrachloride aqueous solution is 50-100g/L, and preferably the concentration of titanium oxide in the titanium tetrachloride aqueous solution is 70 g/L.
A new preparation method of titanium modified activated alumina dry gel comprises the following steps:
adding quantitative pure water into a reactor, adding a titanium tetrachloride aqueous solution, an aluminum sulfate solution and a sodium metaaluminate solution into the reactor in a parallel flow manner under the stirring condition, and neutralizing in the parallel flow manner to form gel; wherein the neutralization water amount is 10-50L per kilogram of aluminum oxide, the pH value of the gel is 5-10, the neutralization temperature is 50-90 ℃, and the optimal neutralization temperature is 75 ℃.
The concentration of aluminum oxide in the aluminum sulfate solution is 50-80g/L, and the acid-base ratio is 1.4-1.7; most preferably, the concentration of aluminum oxide in the aluminum sulfate solution is 65g/L, and the pH ratio is 1.55.
In the first step, the concentration of the aluminum oxide in the sodium metaaluminate solution is 150-220g/L, and preferably, the concentration of the aluminum oxide in the sodium metaaluminate solution is 180 g/L.
The titanium oxide concentration in the titanium tetrachloride aqueous solution is 50-100g/L, and the titanium oxide concentration in the titanium tetrachloride aqueous solution is 70 g/L.
And step two, aging, washing, drying and crushing the finished product gelatinized in the step one to obtain the activated alumina.
In the second step, the aging time is 10-80Min, and the optimal aging time is 20 Min; the aging pH is 8-11, preferably 9.
The drying temperature in the second step is 100-.
Secondly, analyzing the specific surface area and the pore diameter of the product
1. Specific surface area test of the product
(1) Test conditions
The weight of the product sample is 0.13420 g;
the product sample treatment: heating at 200 ℃ and vacuumizing for 2 hours;
the instrument model is as follows: V-Sorb 2800P specific surface area and pore size analyzer;
ambient temperature: 25 ℃;
the test method comprises the following steps: multipoint BET.
(2) Test results
The results of the adsorption test are shown in FIG. 1 in Table 1:
TABLE 1 test results of specific surface area of product
(3) The product specific surface area analysis of the invention is reported in table 2:
TABLE 2 specific Surface Area analysis report (Surface Area)
2. Product pore volume test
(1) Test conditions
The weight of the product sample is 0.13420 g;
the product sample treatment: heating at 200 ℃ and vacuumizing for 2 hours;
the instrument model is as follows: V-Sorb 2800P specific surface area and pore size analyzer;
ambient temperature: 25 ℃;
the test method comprises the following steps: and (4) the aperture.
(2) Test results
The results of the adsorption tests are shown in tables 3 and 4, as shown in FIGS. 2-4:
TABLE 3 pore volume analysis report
TABLE 4 pore size analysis report
In the preparation process, an inorganic titanium source with low price is adopted, so that the problem of wastewater treatment is reduced, and the preparation process adopts a conventional activated alumina preparation method, so that the process is simple and the cost is low. The prepared product titanium oxide is uniformly dispersed on the surface of the alumina, has better pore structure index, and overcomes the defects of uneven dispersion of elements, poorer pore structure and lower pore diameter of the conventional modified alumina.
The main physical and chemical property indexes of the product are that the content of titanium oxide is 15-25%, the pore volume is 0.8-1.0ml/g, the specific surface area is larger than 270-2Per g, average pore diameter of 10-15nm, can be usedThe preparation of the hydrotreating catalyst with larger pore diameter.
While one embodiment of the present invention has been described in detail, the description is only a preferred embodiment of the present invention and should not be taken as limiting the scope of the invention. All equivalent changes and modifications made within the scope of the present invention shall fall within the scope of the present invention.
Claims (9)
1. A raw material for preparing titanium modified activated alumina dry glue is characterized in that: comprises titanium tetrachloride aqueous solution and aluminum source.
2. The raw material for the new preparation of titanium modified activated alumina dry glue according to claim 1, characterized in that: the aluminum source is aluminum sulfate and sodium metaaluminate.
3. A new preparation method of titanium modified activated alumina dry glue is characterized by comprising the following steps: the method comprises the following steps:
step one, adding quantitative pure water into a reactor, and under the condition of stirring, carrying out parallel flow neutralization on a titanium tetrachloride water solution, an aluminum sulfate solution and a sodium metaaluminate solution to form gel;
and step two, aging, washing, drying and crushing the finished product gelatinized in the step one to obtain the activated alumina.
4. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 3 wherein: in the first step, the concentration of aluminum oxide in the aluminum sulfate solution is 50-80g/L, and the acid-base ratio of the aluminum sulfate solution is 1.4-1.7.
5. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 4 wherein: in the first step, the concentration of the aluminum oxide in the sodium metaaluminate solution is 150-220 g/L.
6. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 3 wherein: in the first step, the concentration of titanium oxide in the titanium tetrachloride aqueous solution is 50-100 g/L.
7. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 6 wherein: the neutralization water amount in the first step is 10-50L per kilogram of aluminum oxide, the pH value of the gel is 5-10, and the neutralization temperature is 50-90 ℃.
8. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 3 wherein: and the aging time in the second step is 10-80 min.
9. The novel process for preparing a titanium-modified activated alumina xerogel according to claim 3 wherein: the drying temperature in the second step is 100-200 ℃.
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| CN202110407110.XA CN113086999A (en) | 2021-04-15 | 2021-04-15 | Novel preparation method of titanium modified activated alumina dry glue |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273878A (en) * | 1999-05-18 | 2000-11-22 | 中国石油化工集团公司 | Process for preparing aluminium oxide-titanium oxide bicomponent |
| EP1403358A1 (en) * | 2002-09-27 | 2004-03-31 | ENI S.p.A. | Process and catalysts for deep desulphurization of fuels |
| CN1768945A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | Alumina support containing silicon and titanium and preparation method thereof |
| CN102218351A (en) * | 2011-04-20 | 2011-10-19 | 山东浩霖石油化工科技股份有限公司 | Titanium-containing amorphous silicon-aluminum dry gel and preparation method thereof |
| CN104475168A (en) * | 2014-11-12 | 2015-04-01 | 中国海洋石油总公司 | Preparation method of titanium-aluminum composite oxide with large specific surface and small aperture |
| CN105170193A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of large-aperture titanium-aluminum composite oxide |
-
2021
- 2021-04-15 CN CN202110407110.XA patent/CN113086999A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1273878A (en) * | 1999-05-18 | 2000-11-22 | 中国石油化工集团公司 | Process for preparing aluminium oxide-titanium oxide bicomponent |
| EP1403358A1 (en) * | 2002-09-27 | 2004-03-31 | ENI S.p.A. | Process and catalysts for deep desulphurization of fuels |
| CN1768945A (en) * | 2004-10-29 | 2006-05-10 | 中国石油化工股份有限公司 | Alumina support containing silicon and titanium and preparation method thereof |
| CN102218351A (en) * | 2011-04-20 | 2011-10-19 | 山东浩霖石油化工科技股份有限公司 | Titanium-containing amorphous silicon-aluminum dry gel and preparation method thereof |
| CN104475168A (en) * | 2014-11-12 | 2015-04-01 | 中国海洋石油总公司 | Preparation method of titanium-aluminum composite oxide with large specific surface and small aperture |
| CN105170193A (en) * | 2015-09-10 | 2015-12-23 | 中国海洋石油总公司 | Preparation method of large-aperture titanium-aluminum composite oxide |
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Application publication date: 20210709 |