CN104888866A - Silicon-magnesium compound carrier and preparation method thereof - Google Patents
Silicon-magnesium compound carrier and preparation method thereof Download PDFInfo
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- CN104888866A CN104888866A CN201510258411.5A CN201510258411A CN104888866A CN 104888866 A CN104888866 A CN 104888866A CN 201510258411 A CN201510258411 A CN 201510258411A CN 104888866 A CN104888866 A CN 104888866A
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Abstract
The invention relates to a catalyst carrier, and particularly relates to a silicon-magnesium compound carrier and a preparation method of the silicon-magnesium compound carrier. The silicon-magnesium compound carrier is a compound of silicon and aluminium oxides and magnesium carbonates and oxides, or takes a compound of silicon oxides and magnesium carbonates and oxides as a carrier. The ratio of Si: Al: Mg is 5-7: 0-3: 2-5. The preparation method is simple, and is high in activity and strength, and good in selectivity. According to the invention, the carrier is prepared via a coprecipitation method, and the specific surface area and fine pore volume of the carrier are increased.
Description
(1) technical field
The present invention relates to a kind of catalyst carrier, particularly a kind of silicon magnesium complexes carrier and preparation method thereof.
(2) background technology
Catalyst carrier, also known as carrier (support), is one of composition of loaded catalyst.Catalytic active component is supported on carrier surface, and carrier is mainly used in supporting active component, make catalyst have specific physical behavior, and carrier itself does not generally have catalytic activity.Majority carrier is the product in Catalyst, and conventional has alumina support, silica-gel carrier, absorbent charcoal carrier and some natural products as float stone, diatomite etc.At present, many employings pressure ball method or extrusion legal system obtain carrier mother bulb, then activated roasting and/or superheated steam expanding treatment obtain final catalyst carrier, the shortcoming of this technique is difficult to reach desirable pore diameter, specific area and pore volume less, thus cause carrier activity decrease and exchange volume reduce, when catalyzing and synthesizing product, the output of unit volume will be affected, and the consumption of carrier is increased.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides a kind of silicon magnesium complexes carrier and preparation method thereof.
The present invention is achieved through the following technical solutions:
A kind of silicon magnesium complexes carrier, is characterized in that: comprise the compound be made up of the oxide of the oxide of silicon, aluminium and the carbonate of magnesium and magnesium, or the compound be made up of the oxide of the oxide of silicon and the carbonate of magnesium and magnesium is carrier.
The preparation method of above-mentioned silicon magnesium complexes carrier, comprises the following steps:
(1) in beaker, add sodium silicate aqueous solution 1000ml and 20% ammoniacal liquor successively, be 9-11 by 20% ammoniacal liquor hierarchy of control pH value, under stirring, be warming up to 50-60 DEG C;
(2) the mixed solution 500ml adding magnesium nitrate or magnesium nitrate and aluminum nitrate in above-mentioned mixed liquor mixes, and adds 20% hydrochloric acid and system pH is adjusted to 4-6, then stir 1h after stirring 1h;
(3) after stirring and terminating, then after system pH is adjusted to 8 by the sal volatile adding 2mol/L in system, be warming up to 80-90 DEG C, stir 6 hours, then aging 40h is precipitated thing;
(4) dry after sediment filtration washing at 100-130 DEG C, in 400-600 DEG C of roasting 5 hours, pulverized 200 mesh sieves, obtained carrier.
Above-mentioned sodium silicate aqueous solution concentration is: in silica concentration for 40-58 gram of silica/rise sodium silicate aqueous solution.
The concentration of the magnesium nitrate added in above-mentioned steps (2) is: in magnesia concentration for 70-85 gram of magnesia/rise magnesium nitrate.
The concentration of the aluminum nitrate added in above-mentioned steps (2) is: in aluminium oxide concentration for 50-100 gram of aluminium oxide/liter.
Wherein, described carrier pore volume is 0.6-1.5 ml/g, and specific area is 55-130 m
2/ g.
In described carrier, the mass ratio of silicon, aluminium, magnesium is, silicon: aluminium: magnesium=5-7:0-3:2-5.
The invention has the beneficial effects as follows: the invention provides a kind of silicon magnesium complexes carrier, wherein Si:Al:Mg=5-7:0-3:2-5; Preparation method of the present invention is simple, and active high, and intensity is high, selective good; And the present invention adopts coprecipitation to obtain carrier, increase specific area and the pore volume of carrier.
(4) detailed description of the invention
Embodiment 1:
Add successively in a precipitation vessel in silica concentration be 44 grams of silica/liter sodium silicate aqueous solution (waterglass, as follows, Qingdao water glass plant product) 1000ml, with 20% ammoniacal liquor (Katyuan city chemical reagent factory product) hierarchy of control pH value for 10-11, after being warming up to 60 DEG C under stirring, add in magnesia concentration be 71.3 grams of magnesia/liter magnesium nitrate (Tianjin Yao Hua chemical reagent work product) solution 250ml and in aluminium oxide concentration be 99.7 grams of aluminium oxide/liter aluminum nitrate (Shenyang City's reagent one factory product) solution 250ml mixed liquor, stir at 45-60 DEG C after 1 hour, use 20% hydrochloric acid again adjusted to ph be 4-6, stir 1 hour, be after 8 with the sal volatile adjusted to ph of 2M, be warming up to 80-90 DEG C, continue stirring again 6 hours, then discharging, aging 40 hours, filtration washing, in 125 DEG C of oven dry.In 550 DEG C of roastings after 5 hours, through pulverizing 200 mesh sieves, obtained carrier S
a.
Embodiment 2:
Add successively in a precipitation vessel in silica concentration be 50.6 grams of silica/liter sodium metasilicate (Qingdao water glass plant product) aqueous solution 1000ml, with 20% ammoniacal liquor (Katyuan city chemical reagent factory product) hierarchy of control pH value for 10-11, after being warming up to 60 DEG C under stirring, add in magnesia concentration be 80.7 grams of magnesia/liter magnesium nitrate (Tianjin Yao Hua chemical reagent work product) solution 250ml and be 55.9 grams of aluminium oxide/rise aluminum nitrate (Shenyang City's reagent one factory product) solution 250ml mixed liquor in aluminium oxide concentration, stir at 45-60 DEG C after 1 hour, use 20% hydrochloric acid again adjusted to ph be 4-6, stir 1 hour, be after 8 with the sal volatile adjusted to ph of 2M, be warming up to 80-90 DEG C, continue stirring again 6 hours, then discharging, aging 40 hours, filtration washing, in 125 DEG C of oven dry.In 550 DEG C of roastings after 5 hours, through pulverizing 200 mesh sieves, obtained carrier S
b.
Embodiment 3:
Add successively in a precipitation vessel in silica concentration be 55.2 grams of silica/liter sodium metasilicate (Qingdao water glass plant product) aqueous solution 1000ml, with 20% ammoniacal liquor (Katyuan city chemical reagent factory product) hierarchy of control pH value for 10-11, after being warming up to 60 DEG C under stirring, add in magnesia concentration be 81.0 grams of magnesia/liter magnesium nitrate (Tianjin Yao Hua chemical reagent work product) solution 500ml, stir at 45-60 DEG C after 1 hour, use 20% hydrochloric acid again adjusted to ph be 4-6, stir 1 hour, be after 8 with the sal volatile adjusted to ph of 2M, be warming up to 80-90 DEG C, continue stirring again 6 hours, then discharging, aging 40 hours, filtration washing, in 125 DEG C of oven dry.In 550 DEG C of roastings after 5 hours, through pulverizing 200 mesh sieves, obtained carrier S
c.
The constituent content of carrier in table 1 various embodiments of the present invention
Claims (7)
1. a silicon magnesium complexes carrier, is characterized in that: comprise the compound be made up of the oxide of the oxide of silicon, aluminium and the carbonate of magnesium and magnesium, or the compound be made up of the oxide of the oxide of silicon and the carbonate of magnesium and magnesium is carrier.
2. the preparation method of silicon magnesium complexes carrier according to claim 1, it is characterized in that: comprise the following steps: (1) adds sodium silicate aqueous solution 1000ml and 20% ammoniacal liquor successively in precipitation vessel, be 9-11 by 20% ammoniacal liquor hierarchy of control pH value, under stirring, be warming up to 50-60 DEG C; (2) the mixed solution 500ml adding magnesium nitrate or magnesium nitrate and aluminum nitrate in above-mentioned mixed liquor mixes, and adds 20% hydrochloric acid and system pH is adjusted to 4-6, then stir 1h after stirring 1h; (3) after stirring and terminating, then after system pH is adjusted to 8 by the sal volatile adding 2mol/L in system, be warming up to 80-90 DEG C, stir 6 hours, then aging 40h, is precipitated thing; (4) dry after sediment filtration washing at 100-130 DEG C, in 400-600 DEG C of roasting 5 hours, pulverized 200 mesh sieves, obtained carrier.
3. silicon magnesium complexes carrier according to claim 2 and preparation method thereof, is characterized in that: described sodium silicate aqueous solution concentration is: in silica concentration for 40-58 gram of silica/rise sodium silicate aqueous solution.
4. silicon magnesium complexes carrier according to claim 2 and preparation method thereof, is characterized in that: the concentration of the magnesium nitrate added in described step (2) is: in magnesia concentration for 70-85 gram of magnesia/rise magnesium nitrate.
5. silicon magnesium complexes carrier according to claim 2 and preparation method thereof, is characterized in that: the concentration of the aluminum nitrate added in described step (2) is: in aluminium oxide concentration for 50-100 gram of aluminium oxide/liter.
6. silicon magnesium complexes carrier according to claim 2 and preparation method thereof, it is characterized in that: described carrier pore volume is 0.6-1.5 ml/g, specific area is 55-130 m
2/ g.
7. silicon magnesium complexes carrier according to claim 2 and preparation method thereof, is characterized in that: in described carrier, the mass ratio of silicon, aluminium, magnesium is, silicon: aluminium: magnesium=5-7:0-3:2-5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539598A (en) * | 2022-03-24 | 2022-05-27 | 慈溪市赞恩包装科技有限公司 | Preparation method of foam board with uniform particles |
Citations (3)
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|---|---|---|---|---|
| EP1422198A1 (en) * | 2001-07-27 | 2004-05-26 | Chiyoda Corporation | Porous 4 group metal oxide and method for preparation thereof |
| CN1907567A (en) * | 2006-08-16 | 2007-02-07 | 天津化工研究设计院 | Forming method for porous composite metallic oxide catalytic carrier |
| CN101613110A (en) * | 2008-12-16 | 2009-12-30 | 海南美大制药有限公司 | A kind of aluminum-magnesium silicate compound and synthetic method thereof |
-
2015
- 2015-05-20 CN CN201510258411.5A patent/CN104888866B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1422198A1 (en) * | 2001-07-27 | 2004-05-26 | Chiyoda Corporation | Porous 4 group metal oxide and method for preparation thereof |
| CN1907567A (en) * | 2006-08-16 | 2007-02-07 | 天津化工研究设计院 | Forming method for porous composite metallic oxide catalytic carrier |
| CN101613110A (en) * | 2008-12-16 | 2009-12-30 | 海南美大制药有限公司 | A kind of aluminum-magnesium silicate compound and synthetic method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 冯凌等: "共沉淀法合成三硅酸镁及其微观分析", 《北京科技大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114539598A (en) * | 2022-03-24 | 2022-05-27 | 慈溪市赞恩包装科技有限公司 | Preparation method of foam board with uniform particles |
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Effective date of registration: 20211201 Address after: 274000 west of north section of Huaxu road and north of Changcheng street, ChenWang sub district office, juancheng County, Heze City, Shandong Province Patentee after: JUANCHENG DINGSHENG CHEMICAL TECHNOLOGY Co.,Ltd. Address before: 274600 east of Fenghuang Road south of Chengpu Street juancheng County Heze City Shandong Province Patentee before: JUANCHENG RUIDING TECHNOLOGY Co.,Ltd. |
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Denomination of invention: Silicon magnesium composite carrier and preparation method thereof Effective date of registration: 20211221 Granted publication date: 20170616 Pledgee: Shandong juancheng Rural Commercial Bank Co.,Ltd. Pledgor: JUANCHENG DINGSHENG CHEMICAL TECHNOLOGY Co.,Ltd. Registration number: Y2021980015438 |
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