GB2315430A - Mixed oxide catalyst support - Google Patents
Mixed oxide catalyst support Download PDFInfo
- Publication number
- GB2315430A GB2315430A GB9701614A GB9701614A GB2315430A GB 2315430 A GB2315430 A GB 2315430A GB 9701614 A GB9701614 A GB 9701614A GB 9701614 A GB9701614 A GB 9701614A GB 2315430 A GB2315430 A GB 2315430A
- Authority
- GB
- United Kingdom
- Prior art keywords
- porous composite
- composite oxide
- making
- gel
- oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-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
- B01J21/12—Silica and alumina
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/036—Precipitation; Co-precipitation to form a gel or a cogel
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Catalysts (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
A method for making a porous composite oxide, which includes the steps of: (a) preparing a solution including a silicon oxide source and a solution including an aluminium oxide source; (b) slowly pouring one of the solutions from step (a) into the other solution while stirring; (c) adding hydrochloric acid to the mixed solution prepared in step (b)to obtain a sol and then adding sodium hydroxide to the sol to obtain a gel; and (d) reacting the silicon oxide source and aluminium oxide source in the gel at high temperature and high pressure. The porous composite oxide so formed has an abundance of fine pores and a relatively uniform distribution of pore sizes, making it suitable for use as a carrier or catalytic support.
Description
METHOD OF MAKING A POROUS COMPOSITE OXIDE
The present invention relates to a method of making a porous composite oxide and, more particularly, to a method of making a porous composite oxide for use as a carrier, in which an abundance of fine pores is formed and the distribution of pore sizes is relatively uniform.
Current progress in chemical-related industries has been accompanied by the development of various catalysts. In general, the use of catalysts is essential for chemical reactions involving synthesis, decomposition or rearrangement of substances and such catalysts usually comprise particles of metal or other compounds. Various methods for handling a catalyst may be used but, most typically, a carrier or support is impregnated with the catalyst. A carrier or support suitable for impregnation with catalyst particles must be non-reactive itself and should have an abundance of fine pores. The latter are required because, in order to promote effective catalysis of a reaction, it is necessary to ensure that there is sufficient space for contact between the catalytic components and the reactants. Suitable carriers include silica, alumina, aluminosilicate, zeolite and activated carbon, of which aluminosilicate is especially widely used because of its range of pore sizes.
For more vigorous catalytic reactions, carriers which can further increase contact area between the reactants and the catalyst are required. Generally, aluminosilicate is made by dissolving a soluble aluminium oxide source and a soluble silicon oxide source and then heating the resultant solution. However, aluminosilicate prepared by this method does not have a sufficient number of pores for impregnation with catalyst particles. A pore formed in a carrier provides a space for impregnation with catalyst particles, in which a catalytic reaction can occur, and, consequently, the catalytic reaction cannot be performed effectively, if there are insufficient pores. Accordingly, a carrier having a large number of pores is required.
Furthermore, large numbers of pores of various diameters must be uniformly distributed throughout the carrier, in order to facilitate impregnation with different catalytic particles. However, the pore sizes of aluminosilicate made by conventional methods are not uniformly distributed. It is an object of the present invention to overcome some of the aforementioned disadvantages.
Accordingly, in a first aspect of the invention there is provided a method of making a porous composite oxide for use as a catalytic support, which comprises forming a sol from an intimate mixture of at least two oxideforming materials, forming a gel from said sol, and heating said gel to form said composite oxide.
In a second aspect of the invention, there is provided a porous composite oxide obtained or obtainable by a method according to the invention in its first aspect.
In a third aspect of the invention, there is provided a porous composite oxide for use as a catalytic support having an abundance of fine pores and a substantially uniform distribution of pore sizes.
In a fourth aspect of the invention, there is provided a catalyst supported on a porous composite oxide according to the invention in its second or third aspects.
In a fifth aspect of the invention, there is provided a method for making a porous composite oxide comprising the steps of:
(a) preparing a solution including a silicon oxide source and a solution including an aluminium oxide source;
(b) slowly pouring one of said solutions from step (a) into the other solution while stirring;
(c) adding hydrochloric acid to the mixed solution prepared in said step (b) to obtain a sol and then adding sodium hydroxide to said sol to obtain a gel; and
(d) reacting said silicon oxide source and aluminium oxide source in said gel at high temperature and high pressure.
Preferred embodiments of the invention in any of its various aspects are as described below and as defined in the subclaims.
The advantages of present invention and the manner in which it may be performed will become more apparent from the following detailed description with reference to the attached drawings, in which:
FIG. 1 is a graph showing the relationship between pore volume and pore size of three porous composite oxides prepared according to the present invention; and
FIG. 2 is a graph showing the relationship between pore volume and pore size of a porous composite oxide prepared according to a conventional method.
In an especially preferred embodiment of the present invention described hereafter, hydrochloric acid and sodium or ammonium hydroxide are used in a method of making an aluminosilicate, to form numerous pores of various sizes which are evenly distributed. It should be understood, however, that the present invention is not limited to the preparation of aluminosilicates but also includes the preparation of other composite oxides that are suitable for use as catalytic supports. Moreover, the present invention is not limited to the use of hydrochloric acid and sodium or ammonium hydroxide to form the sol and gel intermediates, respectively, but also includes the use of other acids or bases and other chemical or physical means for achieving these transitions.
In a first step, a soluble silicon oxide source and a soluble aluminium oxide source are separately dissolved in water. A silicate, particularly sodium silicate, is used as the preferred silicon oxide source. Also, an aluminate, particularly sodium aluminate, is used as the preferred aluminium oxide source. Since the solubility of the silicon oxide source may be low in water at room temperature, it is preferable to heat the aqueous solution in order to dissolve the silicon oxide source. The temperature required may vary depending on the solubility and properties of the specific compounds used, however, a temperature range of 5o60 C is generally preferred.
After aqueous solutions of the silicon oxide source and the aluminium oxide source have been prepared, the two solutions are mixed. At this stage, the amounts of the silicon oxide source and aluminium oxide source are preferably controlled, such that the mole ratio of silicon to aluminium is in the range of 1 to 3. At the same time, in order to ensure even mixing of the silicon oxide source and the aluminium oxide source, one of the solutions is preferably added to the other solution, whilst simultaneously heating and stirring the solution.
When the two solutions are completely mixed, hydrochloric acid is added until a sol is obtained. Then, sodium hydroxide is added and the resultant mixture left for a predetermined period, resulting in a change from the sol to a gel. During this step, the sodium hydroxide stimulates active and uniform reaction between the silicon oxide source and the aluminium oxide source.
Preferably, the hydrochloric acid and sodium hydroxide are used in dilute solution and the pH of the resultant solution is maintained at a range of 3-1 2.
Finally, the gel is heated to give an aluminosilicate having abundant fine pores. The heating step is preferably performed for 1-10 hours at 100-300 C at a pressure of 100-1,200 psi, although a temperature range of 100-150"C at a pressure of 100-200 psi is especially preferred.
The present invention will now be described in more detail and by way of illustration only with reference to the following specific examples.
Example 1
First, 98.4 g of sodium silicate (Na2 SiO3) was completely dissolved in 150ml of distilled water at 55 C. Also, 152.5 g of sodium aluminate (NaA102) was dissolved in 700ml of distilled water. Then, the sodium aluminate solution was slowly poured into the sodium silicate solution. During the mixing process, the mixed solution was continuously heated at 55"C whilst being stirred. After the two solutions were completely mixed, 6N HCl was added until the reactant mixture became transparent. Then, 6N NaOH was added to the transparent solution until the pH of the solution reached 10, and the resultant solution left for 60 minutes to obtain a gel. The gel was placed into a reaction chamber and dried at 100 C at a pressure of 100 psi. After 1 hour, the resultant precipitate was filtered using a vacuum filter and then dried at 100 C for 24 hours to obtain aluminosilicate in powder form.
The surface area and the relationship between pore volume and pore size of the powder so obtained were measured. It was found that the BET surface was 135 m2/g and the distribution of pore sizes was relatively uniform (see graph a of FIG. 1).
Example 2
Aluminosilicate in powder form was prepared by the same method as described in Example 1, except that 6N NaOH was added to adjust the pH of the solution to 7 and the reaction was performed at 1500C and 150 psi.
The surface area and the relationship between pore volume and pore size of the powder so obtained were measured. It was found that the BET surface area was 135 m2/g and the distribution of pore sizes was relatively uniform (see graph b of FIG. 1).
Example 3
Aluminosilicate in powder form was prepared by the same method as described in Example 1, except that 6N NaOH was added to adjust the pH of the solution to 3 and the reaction was performed at 265"C and 1,100 psi.
The surface area and the relationship between pore volume and pore size of the powder so obtained were measured. It was found that the BET surface area was 135 m2/g and the degree of distribution of pores according to the size of the pores was uniform throughout (see graph c of FIG. 1).
Comparative Example
Aluminosilicate in powder form was prepared by the same method as described in Example 1, except that HCl and NaOH were not used. Then, the BET surface area and the distribution of pore sizes with respect to the powder so obtained were measured. The BET surface area was found to be less than 3.3 m2/g, whilst the distribution of pore sizes was not uniform.
It can be seen from the results of the above examples and the comparative example that the BET surface area of the aluminosilicate prepared according to the present invention is greater than 100 m2/g, whilst that prepared by the conventional method is less than 3.3 m2/g. Also, in respect of distribution of pore sizes, the aluminosilicate according to the present invention has a relatively uniform distribution of pore volume to pore size (see FIG. 1), whilst that of the conventional aluminosilicate is not uniform (see FIG. 2).
In conclusion, therefore, the porous composite oxides prepared according to the present invention have an abundance of fine pores and a relatively uniform distribution of pore sizes, thus making them especially suitable for use as catalytic carriers or supports.
Claims (33)
1. A method of making a porous composite oxide for use as a catalytic support, which comprises forming a sol from an intimate mixture of at least two oxide-forming materials, forming a gel from said sol, and heating said gel to form said composite oxide.
2. A method as claimed in daim 1, wherein said intimate mixture is prepared by mixing separate solutions of at least two oxide-forming materials.
3. A method as claimed in claim 2, wherein at least one of said solutions is heated prior to or during mixing.
4. A method as claimed in claims 2 or 3, wherein said intimate mixture is a homogeneous solution.
5. A method as claimed in claims 2 or 3, wherein said intimate mixture is a suspension.
6. A method as claimed in claim 5, wherein said suspension is treated to form a homogeneous solution, prior to formation of said sol.
7. A method as claimed in claim 6, wherein said homogeneous solution is formed upon addition of mineral acid to said suspension.
8. A method as claimed in any one of the preceding claims, wherein said sol is formed at low pH.
9. A method as claimed in any one of the preceding daims, wherein said gel is formed upon addition of dilute alkali to said sol.
10. A method as claimed in claimed in claim 9, wherein said gel is formed at pH 3-12.
11. A method as claimed in any one of the preceding claims, wherein said gel is heated at high temperature and high pressure to form said composite.
12. A method as claimed in claim 11, wherein said gel is heated at a temperature of 100-3000C and a pressure of 100-1200 psi.
13. A method as daimed in claim 12, wherein said gel is heated at a temperature of 100-1500C and a pressure of 100-200 psi.
14. A method as claimed in any one of the preceding claims, wherein said porous composite oxide is an aluminosilicate.
15. A method as claimed in claim 14, wherein said intimate mixture comprises a silicon oxide-forming material and an aluminium oxide-forming material.
16. A method as claimed in claim 15, wherein the mole ratio of silicon to aluminium in said intimate mixture is approximately 1:3.
17. A method as claimed in claims 15 or 16, wherein said silicon oxideforming material is a silicate, preferably sodium silicate.
18. A method as claimed in claims 15, 16 or 17, wherein said aluminium oxide-forming material is an aluminate, preferably sodium ruminate.
19. A porous composite oxide obtained by a method according to any one of the preceding claims.
20. A porous composite oxide for use as a catalytic support having an abundance of fine pores and a substantially uniform distribution of pore sizes.
21. A porous composite oxide as claimed in claims 19 or 20 having a BET surface area of at least 100 m2/g.
22. A porous composite oxide as claimed in claim 21 having a BET surface area of at least 135 m2/g.
23. A porous composite oxide substantially as hereinbefore described in
Examples 1-3.
24. A catalyst supported on a porous composite oxide according to any one of claims 19-23.
25. A method for making a porous composite oxide comprising the steps of:
(a) preparing a solution including a silicon oxide source and a solution including an aluminium oxide source;
(b) slowly pouring one of said solutions from step (a) into the other solution while stirring;
(c) adding hydrochloric acid to the mixed solution prepared in said step (b) to obtain a sol and then adding sodium hydroxide to said sol to obtain a gel; and
(d) reacting said silicon oxide source and aluminium oxide source in said gel at high temperature and high pressure.
26. A method for making a porous composite oxide as claimed in daim 25, wherein the mole ratio of silicon to aluminium of said mixed solution is 1-3.
27. A method of making a porous composite oxide as claimed in claims 25 or 26, wherein said silicon oxide source is a silicate.
28. A method for making a porous composite oxide as claimed in claim 27, wherein said silicate is sodium silicate.
29. A method for making a porous composite oxide as claimed in any of claims 25-28, wherein said aluminium oxide source is an aluminate.
30. A method for making a porous composite oxide as claimed in claim 29, wherein said aluminate is sodium aluminate.
31. A method for making a porous composite oxide as claimed in any one of claims 25-30, wherein said sodium hydroxide is added until the pH of the sol reaches 3-12.
32. A method for making a porous composite oxide as claimed in any one of claims 25-31, wherein the reaction is performed at a temperature of 100-300 C and a pressure of 100;1,200 psi.
33. A method for making a porous composite oxide as claimed in claim 32, wherein said temperature is 100-150 C and said pressure is 100-200 psi.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1019960029309A KR100195111B1 (en) | 1996-07-19 | 1996-07-19 | Method for manufacturing porous composite oxide |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| GB9701614D0 GB9701614D0 (en) | 1997-03-19 |
| GB2315430A true GB2315430A (en) | 1998-02-04 |
| GB2315430B GB2315430B (en) | 1999-04-07 |
Family
ID=19466849
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB9701614A Expired - Fee Related GB2315430B (en) | 1996-07-19 | 1997-01-27 | Method of making a porous composite oxide |
Country Status (6)
| Country | Link |
|---|---|
| JP (1) | JP2928189B2 (en) |
| KR (1) | KR100195111B1 (en) |
| CN (1) | CN1074303C (en) |
| BR (1) | BR9701084A (en) |
| GB (1) | GB2315430B (en) |
| IT (1) | IT1289954B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055891A (en) * | 2012-12-03 | 2013-04-24 | 天津大学 | Method for preparing nano porous titanium dioxide thin film doped with Pd by constant voltage dealloying method on amorphous alloy stripe |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI279848B (en) | 2004-11-04 | 2007-04-21 | Ind Tech Res Inst | Structure and method for forming a heat-prevented layer on plastic substrate |
| CN101388414B (en) * | 2004-11-05 | 2011-01-26 | 财团法人工业技术研究院 | Heat resistance construction on plastic substrate |
| KR100761452B1 (en) | 2006-11-06 | 2007-10-04 | 한양대학교 산학협력단 | Method for manufacturing cement having minute particle by chemical synthesis and method for manufacturing concrete using thereof |
| KR101142398B1 (en) * | 2009-08-17 | 2012-05-08 | (주)한천자원 | Manufacturing method of molding coal using coal dust |
| CN114763543A (en) | 2021-01-15 | 2022-07-19 | 百瑞全球有限公司 | Membranous immobilized cell, polypeptide, oligopeptide or protein and preparation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1413874A (en) * | 1973-01-10 | 1975-11-12 | Atlantic Richfield Co | Process for hydrotreating high nitrogen feedstocks and a catalyst for use therein |
| GB1525811A (en) * | 1975-04-08 | 1978-09-20 | Grace W R & Co | High activity amorphous silica-alumina catalyst |
| EP0340868A1 (en) * | 1988-05-06 | 1989-11-08 | ENIRICERCHE S.p.A. | Catalytically active silica and alumina gel and process for preparing it |
| GB2276486A (en) * | 1993-02-25 | 1994-09-28 | Ronald William Bennett | Combined clamp/tuning means for a guitar string |
| WO1994026790A1 (en) * | 1993-05-17 | 1994-11-24 | Solvay S.A. | Catalyst support, method for making a precursor gel for a catalyst support |
| EP0659478A1 (en) * | 1993-12-22 | 1995-06-28 | ENIRICERCHE S.p.A. | Process for preparing amorphous, catalytically active silico-aluminas |
| US5436681A (en) * | 1994-04-12 | 1995-07-25 | Michaels; Brian A. | Apparatus and method for screening individuals for ametropic conditions |
| WO1996009117A1 (en) * | 1994-09-22 | 1996-03-28 | F. Hoffmann-La Roche Ag | Heterogeneous catalysts |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4181532A (en) * | 1975-10-22 | 1980-01-01 | United Kingdom Atomic Energy Authority | Production of colloidal dispersions |
| US4559321A (en) * | 1985-01-28 | 1985-12-17 | Shell Oil Company | Process for producing wide pore catalyst supports |
| JPH0655276B2 (en) * | 1990-02-28 | 1994-07-27 | 富田製薬株式会社 | Method for producing ammonium ion-selective adsorbent |
| BE1008640A7 (en) * | 1994-09-14 | 1996-07-02 | Messadek Jallal | Silica-alumina xerogel preparation methods |
-
1996
- 1996-07-19 KR KR1019960029309A patent/KR100195111B1/en not_active IP Right Cessation
-
1997
- 1997-01-27 GB GB9701614A patent/GB2315430B/en not_active Expired - Fee Related
- 1997-02-21 IT IT97MI000382A patent/IT1289954B1/en active IP Right Grant
- 1997-02-26 BR BR9701084A patent/BR9701084A/en not_active IP Right Cessation
- 1997-02-28 CN CN97103418A patent/CN1074303C/en not_active Expired - Fee Related
- 1997-03-17 JP JP9063635A patent/JP2928189B2/en not_active Expired - Fee Related
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1413874A (en) * | 1973-01-10 | 1975-11-12 | Atlantic Richfield Co | Process for hydrotreating high nitrogen feedstocks and a catalyst for use therein |
| GB1525811A (en) * | 1975-04-08 | 1978-09-20 | Grace W R & Co | High activity amorphous silica-alumina catalyst |
| EP0340868A1 (en) * | 1988-05-06 | 1989-11-08 | ENIRICERCHE S.p.A. | Catalytically active silica and alumina gel and process for preparing it |
| GB2276486A (en) * | 1993-02-25 | 1994-09-28 | Ronald William Bennett | Combined clamp/tuning means for a guitar string |
| WO1994026790A1 (en) * | 1993-05-17 | 1994-11-24 | Solvay S.A. | Catalyst support, method for making a precursor gel for a catalyst support |
| EP0659478A1 (en) * | 1993-12-22 | 1995-06-28 | ENIRICERCHE S.p.A. | Process for preparing amorphous, catalytically active silico-aluminas |
| US5436681A (en) * | 1994-04-12 | 1995-07-25 | Michaels; Brian A. | Apparatus and method for screening individuals for ametropic conditions |
| WO1996009117A1 (en) * | 1994-09-22 | 1996-03-28 | F. Hoffmann-La Roche Ag | Heterogeneous catalysts |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055891A (en) * | 2012-12-03 | 2013-04-24 | 天津大学 | Method for preparing nano porous titanium dioxide thin film doped with Pd by constant voltage dealloying method on amorphous alloy stripe |
Also Published As
| Publication number | Publication date |
|---|---|
| ITMI970382A1 (en) | 1998-08-21 |
| KR100195111B1 (en) | 1999-06-15 |
| JPH1036111A (en) | 1998-02-10 |
| CN1074303C (en) | 2001-11-07 |
| CN1171295A (en) | 1998-01-28 |
| IT1289954B1 (en) | 1998-10-19 |
| KR980009114A (en) | 1998-04-30 |
| GB2315430B (en) | 1999-04-07 |
| GB9701614D0 (en) | 1997-03-19 |
| JP2928189B2 (en) | 1999-08-03 |
| BR9701084A (en) | 1998-12-15 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PCNP | Patent ceased through non-payment of renewal fee |
Effective date: 20050127 |