CN103120857B - The solid-liquid separating method of nano material - Google Patents
The solid-liquid separating method of nano material Download PDFInfo
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- CN103120857B CN103120857B CN201110369159.7A CN201110369159A CN103120857B CN 103120857 B CN103120857 B CN 103120857B CN 201110369159 A CN201110369159 A CN 201110369159A CN 103120857 B CN103120857 B CN 103120857B
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Abstract
The present invention relates to a kind of solid-liquid separating method of nano material, mainly solve the problem of nano material filter process complexity in prior art.Slurries containing nano material are obtained meter Sized Materials by spraying dry by adopting by the present invention; Wherein spray drying condition is: atomizing disk rotating speed 1000 ~ 20000 revs/min, hot-air enters spray drying tower tower body temperature 100 ~ 300 DEG C, the technical scheme that hot-air draws spray drying tower tower body temperature 50 ~ 200 DEG C preferably resolves this problem, can be used in the industrial solid-liquid separation of produced of nano material.
Description
Technical field
The present invention relates to a kind of solid-liquid separating method of nano material.
Background technology
General particle size is called nano material between the material of 1 ~ 100 nanometer, because it has large specific area, usually occurs " nano effect ", has a wide range of applications field.The surface atom number of nano molecular sieve sharply increases with the minimizing of particle size with the ratio of body phase total atom number, thus nano molecular sieve is become have the new material of unique catalytic performance.Nano molecular sieve is compared bulky grain molecular sieve and is had the higher micropore diffusion speed of larger Extra specific surface area sum, improve catalyst utilization rate, strengthen large Molecular Cloning ability, reduce deep reaction, improve selective and reduce in coking and deactivation etc. and all show superior performance, be therefore subject to extensive research.But nano molecular sieve particle is too little, is difficult to be separated with mother liquor, filters in the preparation and reclaim difficulty, thus hinder the commercial Application of nano molecular sieve.
Point out in " Microporous and Mesoporous Materials, 25 (1998): 59-74 ", nano-beta molecular sieve slurries are stable suspension, and sinking speed is extremely slow, 1 year also can not sedimentation layering even if placed.The document proposes first molecular sieve pulp to be diluted with water to low viscosity and low ph value, then adopts high speed centrifugation partition method to reclaim the method for molecular sieve solid, under rotating speed 16000 revs/min, operates 90 minutes.The method centrifugal rotational speed is high, and molecular sieve treating capacity is little, and disengaging time is long, and process is complicated, thus cannot be applied to large-scale industrial production.
Adopt sol-gel process by nano molecular sieve and SiO in patent ZL02100379.3
2or Al
2o
3or SiO
2/ Al
2o
3be prepared into nano molecular sieve compound.The method makes nanometer molecular sieve slurry directly mix with the colloidal sol of carrier without filtration, avoids filter process the most difficult in nano molecular sieve preparation.But the method adds SiO
2or Al
2o
3or SiO
2/ Al
2o
3, makes the composition of obtained nano molecular sieve solid there occurs change, not only can not obtain pure nano molecular sieve, and process is complicated.
The method of molecular sieve filtration disclosed in patent ZL97112269.5 is, after the small crystal grain NaY molecular sieve slurries of less than 0.5 micron mix with water, ammonium salt and a kind of acidic silicasol, slurry pH value is adjusted to average grain 2.8 ~ 3.5, then filters.Equally, the method makes the composition of obtained nano molecular sieve solid there occurs change, not only can not obtain pure nano molecular sieve, and process is complicated.
The method of molecular sieve filtration disclosed in patent ZL03122854.2 is in molecular sieve pulp, add alkaline medium, non-electrical medium and water, and process is complicated.
In sum, there is the shortcoming of process complexity in conventional art.
Summary of the invention
Technical problem to be solved by this invention is the problem of conventional art process complexity, provides a kind of solid-liquid separating method of new nano material.The method has easy, feature fast.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind of solid-liquid separating method of nano material, and the slurries containing nano material are obtained meter Sized Materials by spraying dry; Wherein spray drying condition is: atomizing disk rotating speed 1000 ~ 20000 revs/min, and hot-air enters spray drying tower tower body temperature 100 ~ 300 DEG C, and hot-air draws spray drying tower tower body temperature 50 ~ 200 DEG C.
In technique scheme, atomizing disk rotating speed is 5000 ~ 15000 revs/min, and hot-air enters spray drying tower tower body temperature 130 ~ 260 DEG C, and hot-air draws spray drying tower tower body temperature 80 ~ 160 DEG C.Preferred version of the present invention is regulate the described pH value containing the slurries of nano material to be 6 ~ 8.In described slurries, the solid-weight content preferable range of nano material is 5 ~ 50%, and more preferably scope is 10 ~ 30%.Described nano material preferred version is nano molecular sieve, and more preferably scheme is nano material is nanometer Y molecular sieve, nano-beta molecular sieve, nano wire optical molecule sieve, nanometer ZSM molecular sieve, nanometer SAPO molecular sieve, nanometer SBA molecular sieve or nanometer MCM molecular sieve.
In the inventive method, can by regulating the pH value of slurries to containing adding pH value regulator in the slurries of nano material.PH value regulator can be selected according to the pH value of slurries, if slurry pH value < 6, then selects alkaline pH adjusting agent; As slurry pH value > 8, then select acidic ph modifier.Described alkaline pH adjusting agent is at least one in ammoniacal liquor, sodium hydrate aqueous solution, potassium hydroxide aqueous solution, aqueous sodium carbonate or wet chemical.Described acidic ph modifier is at least one in aqueous hydrochloric acid solution, aqueous solution of nitric acid, aqueous sulfuric acid, oxalic acid aqueous solution, aqueous citric acid solution or the benzoic acid aqueous solution.
Adopt the inventive method, not only can reach the object of Separation of Solid and Liquid, and can by regulating slurry solids weight content, hot-air turnover tower body temperature, atomizing disk rotating speed, regulate size and the shape of obtained solid, complete the shaping of fluid catalyst, achieve good technique effect.
Below by embodiment, the present invention is further elaborated.
Detailed description of the invention
[embodiment 1]
According to document CN200810043303.6[embodiment 1] method of preparing ZSM-5 obtains 50 grams of slurries, and slurry pH value is 13, adds 1.5 mol/L salpeter solutions, and pH is 8, then adds water, and in last slurries, ZSM-5 weight content is 21%.Under agitation, slurries are input to atomizing disk by feed pipe by pump, atomizing disk rotating speed 5000 revs/min, hot-air enters tower body temperature 200 DEG C, and hot-air draws tower body temperature 100 DEG C, and both can obtain nano material solid, its grain size is 460 nanometers.
[embodiment 2]
According to document CN201110045540.8[embodiment 11] method of preparing ZSM-11 obtains 50 grams of slurries, and slurry pH value is 13, adds 1 mol/L citric acid solution, and pH is 8, then adds water, and in last slurries, ZSM-11 weight content is 15%.Under agitation, slurries are input to atomizing disk by feed pipe by pump, atomizing disk rotating speed 10000 revs/min, hot-air enters tower body temperature 220 DEG C, and hot-air draws tower body temperature 140 DEG C, and both can obtain nano material solid, its grain size is 100 nanometers.
[embodiment 3]
According to document ZL00107486.5[embodiment 1] method of preparing beta-molecular sieve obtains 50 grams of slurries, and slurry pH value is 13, adds 1 mol/L oxalic acid solution, and pH is 7, then adds water, and in last slurries, beta-molecular sieve weight content is 24%.Under agitation, slurries are input to atomizing disk by feed pipe by pump, atomizing disk rotating speed 12000 revs/min, hot-air enters tower body temperature 220 DEG C, and hot-air draws tower body temperature 120 DEG C, and both can obtain nano material solid, its grain size is 50 nanometers.
Claims (1)
1. a solid-liquid separating method for nano material, 40% Ludox, sodium metaaluminate, 4-propyl bromide TPABr, sodium chloride, NaOH and water are mixed, wherein in mixture, the mol ratio of each raw material is: SiO
2/ Al
2o
3=76.90, H
2o/SiO
2=50.83, NaCl/SiO
2=0.68, NaOH/SiO
2=0.15, TPABr/SiO
2=0.40, stir 20 minutes, load in reactor, 170 DEG C dynamically, 200 revs/min, crystallization three days; Crystallization product chilling, to filter, be washed to pH value be 8, dry 12 hours in 120 DEG C, obtained 50 grams of ZMS-5 molecular sieve pulps, wherein molecular sieve average crystal grain diameter is 0.5 micron, slurry pH value is 13, adds 1.5 mol/L salpeter solutions, and pH is 8, add water again, in last slurries, ZSM-5 weight content is 21%; Under agitation, slurries are input to atomizing disk by feed pipe by pump, atomizing disk rotating speed 5000 revs/min, hot-air enters tower body temperature 200 DEG C, and hot-air draws tower body temperature 100 DEG C, and both can obtain nano material solid, its grain size is 460 nanometers.
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| CN103120857B true CN103120857B (en) | 2015-08-12 |
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| CN104436723B (en) * | 2014-12-02 | 2016-05-04 | 四川绵竹川润化工有限公司 | A kind of dry gentle powder integral process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032498A (en) * | 1987-10-16 | 1989-04-26 | 中国石油化工总公司石油化工科学研究院 | The preparation of semi-synthetic fluidized cat catalytic cracking catalyst |
| US7819977B2 (en) * | 2004-02-19 | 2010-10-26 | Syram Belgium nv | Spray-dried starch hydrolysate agglomerate product and method for preparing a spray-dried starch hydrolysate agglomerate product |
| CN102371168A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Preparation method of fluid catalyst |
| CN102371166A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Preparation method of binder-free ZSM-5 fluidized bed catalyst |
| CN102371167A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Fluidized bed catalyst and its preparation method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005056184A1 (en) * | 2003-11-24 | 2005-06-23 | Exxonmobil Chemical Patents Inc. | Spray drying molecular sieve catalyst |
-
2011
- 2011-11-18 CN CN201110369159.7A patent/CN103120857B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032498A (en) * | 1987-10-16 | 1989-04-26 | 中国石油化工总公司石油化工科学研究院 | The preparation of semi-synthetic fluidized cat catalytic cracking catalyst |
| US7819977B2 (en) * | 2004-02-19 | 2010-10-26 | Syram Belgium nv | Spray-dried starch hydrolysate agglomerate product and method for preparing a spray-dried starch hydrolysate agglomerate product |
| CN102371168A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Preparation method of fluid catalyst |
| CN102371166A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Preparation method of binder-free ZSM-5 fluidized bed catalyst |
| CN102371167A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Fluidized bed catalyst and its preparation method |
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