CN100395026C - Method for preparing porous solid alkali - Google Patents
Method for preparing porous solid alkali Download PDFInfo
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- CN100395026C CN100395026C CNB2006100128674A CN200610012867A CN100395026C CN 100395026 C CN100395026 C CN 100395026C CN B2006100128674 A CNB2006100128674 A CN B2006100128674A CN 200610012867 A CN200610012867 A CN 200610012867A CN 100395026 C CN100395026 C CN 100395026C
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Abstract
The present invention relates to a method for preparing porous solid alkali. Active carbon which is prepared from husks is processed for 2 to 4 hours at the temperature of 600 to 800 DEG C in vacuum, and the concentration of nitrate water solution is controlled between 2 and 6 mol/L. The active carbon with equal volume is added in nitrate solution, stirred for 0.5 to 1 hours or oscillated for 10 to 20 minutes by ultrasonic, and dried at the temperature of 100 to 150 DEG C. The dried product is protected by vacuum or nitrogen gas, baked for 4 to 6 hours at the temperature of 400 to 600 DEG C, and heated to 600-800 DEG C by 1 to 10 DEG C / minute at the air atmosphere, and the temperature keeps for 2 to 5 hours. The present invention has the advantages of simple operation, moderate preparation condition, low material cost, large specific surface area of the prepared products and high activity.
Description
Technical field
The invention belongs to a kind of preparation method of inoganic solids alkali, relate in particular to the preparation method of a kind of high-specific surface area, porous solid alkali.
Technical background
Solid base has high activity, high selectivity, reaction condition gentleness, product as catalyst and plurality of advantages such as is easy to separate, can be recycled, especially can make the serialization of reaction process process at fine chemicals aspect synthetic, strengthened the production capacity of equipment, bring into play more and more remarkable advantages, be expected to become eco-friendly catalysis material of new generation.The main direction that the inoganic solids base catalyst is simple because of its preparation, the base strength distribution is wide, Heat stability is good becomes the solid base development.Inoganic solids alkali mainly comprises metal oxide, hydration talcs anionic clay and load-type solid.Alkali metal and alkaline earth oxide are the important solid base catalysts of a class.The basic sites of this quasi-metal oxides is mainly derived from hydroxyl and the electronegative Lattice Oxygen that produces after the surperficial adsorbed water.Yet, relative solid acid catalyst, the solid base catalyst preparation is complicated, cost is higher, specific area is little, and its specific area strengthens with basic sites and remarkable the reduction simultaneously.
Though the hydrotalcite specific area is bigger, its base strength is not high, and also there is the more weak acidic site of a part in the surface, the most important thing is that the hydrotalcite heat endurance is relatively poor, when surpassing uniform temperature, the layer column structure of its uniqueness will subside and take place crystal transfer, cause specific area sharply to reduce.
Magnesia and calcium oxide be two classes the most common also be most important solid base.Calcium oxide belongs to super base, H-=26.5; Magnesia belongs to middle highly basic, and the two has been widely used in many base catalyzed reactions.Important defective of solid base catalyst is its less stable, to CO
2And H
2O is very responsive, touch air or moisture after, active sites is promptly poisoned.There are some researches show, in above two kinds of oxides, add the proper amount of rare-earth oxide, both can strengthen alkalescence, can also effectively improve the stability of solid base.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing good stability, specific area height, porous, inorganic solid base, thereby the mass-and heat-transfer effect of intensified response thing in catalyst improves activity of such catalysts.
The present invention adopts the activated carbon of shell preparation as template, by with corresponding presoma salt solution impregnation in suitable pretreated activated carbon, and in vacuum or inert atmosphere, heat and reduces nitrate formation oxide/activated carbon compound system; At last the activated carbon roasting is removed, obtain porous solid alkali.
Concrete preparation method of the present invention is as follows:
(6) specific area with the shell preparation is 1300～1400m
2The activated carbon of/g in a vacuum 600-800 ℃ handled 2-4 hour, remove in its surface and the duct and adsorb impurity;
(7) nitrate is dissolved in the deionized water, solution concentration is controlled at 2-6mol/L;
(8) the activated carbon equal-volume is added in the nitrate solution, stirred 0.5-1 hour, or adopted sonic oscillation 10-20 minute, in 100～150 ℃ of dryings;
(9) with dried product in vacuum or nitrogen protection, 400～600 ℃ of roasting temperatures 4～6 hours;
(10) product that (9) step was obtained is warmed up to 600～800 ℃ with 1-10 ℃/minute, constant temperature 2-5 hour under air atmosphere.
Aforesaid nitrate is the mixture of calcium nitrate, magnesium nitrate, calcium nitrate and lanthanum nitrate or the mixture of magnesium nitrate and lanthanum nitrate.
The present invention compared with prior art has following advantage:
1. simple to operate, preparation condition is gentle, controllability is good;
2. cost of material is cheap, wide material sources;
3. Zhi Bei product specific area is big, and is active high;
4. have certain universality, not only can be used to prepare a few class solid bases described in this patent, even can be generalized to other oxide system.
The specific embodiment
Embodiment 1
With activated carbon (the about 1300m of specific area
2/ g, pore volume 1ml/g) in a vacuum 600 ℃ handled 4 hours, remove in its surface and the duct and adsorb impurity.Take by weighing 10g magnesium nitrate (Mg (NO
3)
2.6H
2O), be dissolved in the 10g deionized water, be designated as solution A.Measure with the isopyknic activated carbon of solution A and be added in the solution A, stirred 30 minutes, above product was in 150 ℃ of dryings 5 hours.With dried product at nitrogen protection tubular type kiln roasting, temperature: 300 ℃, 4 hours time, at last above-mentioned product is warmed up to 700 ℃ with 5 ℃/minute under the air atmosphere in Muffle furnace, constant temperature 6 hours.Be removed up to activated carbon, stay the target product porous magnesia.
Embodiment 2
With activated carbon (the about 1300m of specific area
2/ g, pore volume are 1ml/g) in a vacuum 700 ℃ handled 2 hours, remove in its surface and the duct and adsorb impurity.Take by weighing 10g calcium nitrate (Ca (NO
3)
2.4H
2O), be dissolved in the 10g deionized water, be designated as solution B.Measure and the isopyknic activated carbon of solution B, be added in the solution B, stirred 20 minutes, solution is fully immersed in the duct of activated carbon.Above product was in 150 ℃ of dryings 5 hours.With dried product at nitrogen protection tubular type kiln roasting, temperature: 600 ℃, 4 hours time, make calcium nitrate be decomposed into calcium oxide.At last above-mentioned product is warmed up to 700 ℃ with 10 ℃/minute under the air atmosphere in Muffle furnace, constant temperature 5 hours.After removing activated carbon, stay target product porous calcium oxide.
Embodiment 3
(specific area is 1400m with activated carbon
2/ g, pore volume are 1ml/g) in a vacuum 800 ℃ handled 2 hours, remove in its surface and the duct and adsorb impurity.Take by weighing 7.8g magnesium nitrate (Mg (NO
3)
2.6H
2O) and 4.99g lanthanum nitrate (La (NO
3)
3.9H
2O), be dissolved in the 10g deionized water, be designated as solution C.Measure and the isopyknic activated carbon of solution C, be added in the solution C, adopted sonic oscillation 10 minutes.Above product was in 150 ℃ of dryings 3 hours.With dried product at the electron tubes type kiln roasting, temperature: 600 ℃, 4 hours time, make magnesium nitrate, lanthanum nitrate be decomposed into magnesia and lanthana.At last above-mentioned product is warmed up to 800 ℃ with 5 ℃/minute under the air atmosphere in Muffle furnace, constant temperature 2 hours.Activated carbon is removed, and stays the superpower solid base of target product porous magnesia/lanthana.
Embodiment 4
(specific area is 1350m with activated carbon
2/ g, pore volume are 1ml/g) in a vacuum 600 ℃ handled 3 hours, remove in its surface and the duct and adsorb impurity.Take by weighing 7.2g calcium nitrate (Ca (NO
3)
2.4H
2O) and 4.99g lanthanum nitrate (La (NO
3)
3.9H
2O), be dissolved in the 10g deionized water, be designated as solution D.Measure and the isopyknic activated carbon of solution D, be added in the solution D, sonic oscillation 20 minutes, above product was in 150 ℃ of dryings 5 hours.With dried product at the electron tubes type kiln roasting, temperature: 700 ℃, 4 hours time, make calcium nitrate, lanthanum nitrate be decomposed into calcium oxide, lanthana.At last above-mentioned product is warmed up to 700 ℃ with 10 ℃/minute under the air atmosphere in Muffle furnace, constant temperature 5 hours.Be removed up to activated carbon, stay target product porous calcium oxide/lanthana.
The pore structure of the various solid bases of table one and catalytic performance test result
Claims (2)
1. a method for preparing porous solid alkali is characterized in that comprising the steps:
(1) specific area with the shell preparation is 1300～1400m
2The activated carbon of/g in a vacuum 600-800 ℃ handled 2-4 hour, remove in its surface and the duct and adsorb impurity;
(2) nitrate is dissolved in the deionized water, solution concentration is controlled at 2-6mol/L;
(3) the activated carbon equal-volume is added in the nitrate solution, stirred 0.5-1 hour, or adopted sonic oscillation 10-20 minute, in 100～150 ℃ of dryings;
(4) with dried product in vacuum or nitrogen protection, 400～600 ℃ of roasting temperatures 4～6 hours;
(5) product that (4) step was obtained is warmed up to 600～800 ℃ with 1-10 ℃/minute, constant temperature 2-5 hour under air atmosphere.
2. a kind of method for preparing porous solid alkali as claimed in claim 1 is characterized in that described nitrate is the mixture of calcium nitrate, magnesium nitrate, calcium nitrate and lanthanum nitrate or the mixture of magnesium nitrate and lanthanum nitrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100128674A CN100395026C (en) | 2006-06-24 | 2006-06-24 | Method for preparing porous solid alkali |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100128674A CN100395026C (en) | 2006-06-24 | 2006-06-24 | Method for preparing porous solid alkali |
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|---|---|
| CN1868592A CN1868592A (en) | 2006-11-29 |
| CN100395026C true CN100395026C (en) | 2008-06-18 |
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|---|---|---|---|
| CNB2006100128674A Active CN100395026C (en) | 2006-06-24 | 2006-06-24 | Method for preparing porous solid alkali |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4746375A (en) * | 1987-05-08 | 1988-05-24 | General Electric Company | Activation of refractory metal surfaces for electroless plating |
| CN1460641A (en) * | 2003-06-06 | 2003-12-10 | 南京大学 | Mesopore solid alkali, mesopore functional material, its preparation method and application |
| CN1680514A (en) * | 2005-01-27 | 2005-10-12 | 清华大学 | Solid alkali catalyst, preparation and use thereof |
-
2006
- 2006-06-24 CN CNB2006100128674A patent/CN100395026C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4746375A (en) * | 1987-05-08 | 1988-05-24 | General Electric Company | Activation of refractory metal surfaces for electroless plating |
| CN1460641A (en) * | 2003-06-06 | 2003-12-10 | 南京大学 | Mesopore solid alkali, mesopore functional material, its preparation method and application |
| CN1680514A (en) * | 2005-01-27 | 2005-10-12 | 清华大学 | Solid alkali catalyst, preparation and use thereof |
Non-Patent Citations (2)
| Title |
|---|
| 磁性镁铝水滑石固体碱的制备与表征. 张海永等人.应用科技，第29卷第3期. 2002 |
| 磁性镁铝水滑石固体碱的制备与表征. 张海永等人.应用科技，第29卷第3期. 2002 * |
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|---|---|
| CN1868592A (en) | 2006-11-29 |
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