CN105478100A - Method for preparing silicon-containing gamma-Al2O3 microsphere - Google Patents

Method for preparing silicon-containing gamma-Al2O3 microsphere Download PDF

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Publication number
CN105478100A
CN105478100A CN201510781628.4A CN201510781628A CN105478100A CN 105478100 A CN105478100 A CN 105478100A CN 201510781628 A CN201510781628 A CN 201510781628A CN 105478100 A CN105478100 A CN 105478100A
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hours
grams
deionized water
stir
bead
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CN201510781628.4A
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唐靖岚
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Wuxi Qingyang Machinery Manufacturing Co Ltd
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Wuxi Qingyang Machinery Manufacturing Co Ltd
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Priority to CN201510781628.4A priority Critical patent/CN105478100A/en
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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Abstract

A disclosed method for preparing silicon-containing gamma-Al2O3 microsphere comprises stirring 200 g of Al(OH)3 powder and proper amount of deionized water to form a slurry, and controlling the liquid-solid mass ratio to be 3-10; adding 10 mL of diluted nitric acid with the volume ratio of 1:3, 10-15 g of urea and a predetermined amount of a sodium silicate solution, and enabling the silicon content in the solution is 0.30% by mass of dry aluminium oxide, stirring for 5 h, adding 40-50 g of kerosene and 5 g of fatty alcohol polyoxyethylene ether, stirring for 5 h, and dropping in an oil-ammonia column to form spheres; and solidifying the wet spheres in ammonia water with the mass concentration of 5% for 2 h, then filtering, flushing with deionized water for 6 times, drying at 80 DEG C for 4 h, drying at 100 DEG C for 2 h, and roasting at 800 DEG C for 3 h, so as to obtain the silicon-containing gamma-Al2O3 microsphere. The silicon-containing gamma-Al2O3 microsphere can be used as a catalyst for preparing propylene through dehydrogenation of propane, and possesses better effect compared with aluminium microspheres containing other elements.

Description

A kind ofly prepare siliceous γ-Al 2o 3the method of bead
Technical field
The present invention relates to and a kind ofly prepare siliceous γ-Al 2o 3the method of bead.
Background technology
The reaction of preparing propylene by dehydrogenating propane is by balance controlled, and for making reaction carry out to dehydrogenation direction, need improve reaction temperature and reduce pressure, high reaction temperature often causes the sintering of platinum group metal catalyst with hydrogenation/dehydrogenation function and a large amount of carbon deposit.The stability of propane dehydrogenation catalyst and selective can be increased substantially by introducing IVA race metal and alkali metal or alkaline-earth metal.In actual applications, along with the lengthening of catalyst service time, need to carry out regeneration process to catalyst, namely by the carbon deposit in high-temperature roasting removing catalyst, recover the performance of catalyst.
In order to realize catalyst performance preferably, must improve aluminum oxide micro-sphere wherein, particularly in the catalyst of preparing propylene by dehydrogenating propane, microballoon of the prior art all well can not realize catalytic action,
Summary of the invention
In order to solve the problems of the technologies described above, the present invention proposes a kind of method that preparation method is specially the bead of the siliceous aluminium oxide of preparation, and its concrete technical scheme is as follows:
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 3-10, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 10-15 gram of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 40-50 gram of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Wherein preferred technical scheme is:
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 8, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 12 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 45 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 2, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 10 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 40 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 10, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 15 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 50 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Advantage of the present invention: the bead prepared by said method is applied to propane to be prepared in propylene catalyst and achieve good effect, and following instance investigates the regenerating stability of catalyst.Coke burning regeneration is the carbon deposit passed on air roasting removing catalyst at 560 DEG C, then at 600 DEG C with hydrogen reducing, recover the activity of catalyst.Catalyst after regeneration is evaluated, and finds that conversion of propane and Propylene Selectivity all achieve unexpected technique effect.
Detailed description of the invention
Embodiment 1
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 2, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 10 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 40 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 2
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 4, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 12 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 45 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 3
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 10, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 15 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 50 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 4
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 8, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 14 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 42 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 5
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 10, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 11 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 40 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 6
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 2, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 15 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 50 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 7
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 2, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 13 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 49 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.
Embodiment 8
A kind ofly prepare siliceous γ-Al 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and appropriate amount of deionized water stir pulp, Gu liquid/mass ratio is 7, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 14 grams of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 49.2 grams of kerosene and 5 grams of AEOs stir 5 hours, in oil ammonia column, drip ball forming.Wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filters, and with deionized water rinsing 6 times, 80 DEG C dryings 4 hours, 100 DEG C of dryings, 12 hours, 800 DEG C roastings 3 hours, obtained siliceous γ-Al 2o 3bead.

Claims (1)

1. prepare siliceous γ-Al for one kind 2o 3the method of bead, obtains as follows: get 200 grams of AL (OH) 3powder and deionized water and stirring pulp, Gu liquid/mass ratio is 3-10, adding 10 ml volumes ratios is the dust technology of 1: 3, the sodium silicate solution of 10-15 gram of urea and scheduled volume, the relative butt aluminium oxide of the silicon content in solution is made to be 0.30 quality %, stir 5 hours, add 40-50 gram of kerosene and 5 grams of AEOs stir 5 hours, ball forming is dripped in oil ammonia column, wet bulb solidifies 2 hours in the ammoniacal liquor of 5 quality %, then filter, with deionized water rinsing 6 times, 80 DEG C of dryings 4 hours, 100 DEG C of dryings 12 hours, 800 DEG C of roastings 3 hours, obtain siliceous γ-Al 2o 3bead.
CN201510781628.4A 2015-11-13 2015-11-13 Method for preparing silicon-containing gamma-Al2O3 microsphere Pending CN105478100A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1465438A (en) * 2002-06-27 2004-01-07 中国石油化工股份有限公司 Spherical aluminium oxide carrier material and preparation process thereof
CN1686812A (en) * 2005-04-29 2005-10-26 邓少彬 Method for producing alumina
CN1958457A (en) * 2006-10-27 2007-05-09 北京化工大学 Round alumina of containing silicon, and preparation method
US20140274818A1 (en) * 2012-06-26 2014-09-18 Brownwood Clay Holdings, Llc Spherical pellets containing common clay particulate material useful as a proppant in hydraulic fracturing of oil and gas wells

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1465438A (en) * 2002-06-27 2004-01-07 中国石油化工股份有限公司 Spherical aluminium oxide carrier material and preparation process thereof
CN1686812A (en) * 2005-04-29 2005-10-26 邓少彬 Method for producing alumina
CN1958457A (en) * 2006-10-27 2007-05-09 北京化工大学 Round alumina of containing silicon, and preparation method
US20140274818A1 (en) * 2012-06-26 2014-09-18 Brownwood Clay Holdings, Llc Spherical pellets containing common clay particulate material useful as a proppant in hydraulic fracturing of oil and gas wells

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
唐博合金等: "含硅氧化铝催化剂的制备及性质", 《上海工程技术大学学报》 *

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Application publication date: 20160413