CN108101073A - A kind of preparation method of molecular sieve catalyst - Google Patents
A kind of preparation method of molecular sieve catalyst Download PDFInfo
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- CN108101073A CN108101073A CN201711448849.5A CN201711448849A CN108101073A CN 108101073 A CN108101073 A CN 108101073A CN 201711448849 A CN201711448849 A CN 201711448849A CN 108101073 A CN108101073 A CN 108101073A
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- molecular sieve
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/06—Preparation of isomorphous zeolites characterised by measures to replace the aluminium or silicon atoms in the lattice framework by atoms of other elements, i.e. by direct or secondary synthesis
- C01B39/065—Galloaluminosilicates; Group IVB- metalloaluminosilicates; Ferroaluminosilicates
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- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
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Abstract
The present invention relates to a kind of preparation methods of molecular sieve catalyst, and silicon source, silicon source, titanium source, molecular sieve, water are proportionally mixed, and mixture is reacted 30h in the case where temperature is 250 DEG C, pressure is 2MPa, obtains molecular sieve precursor liquid；The molecular sieve precursor liquid is washed, is filtered, is removed the foreign ion of molecular sieve surface, the molecular sieve after filtration washing is then added to the water stirring, slurry is made；Montmorillonite or kaolinite are added in into the slurry, continues agitation grinding 2h, obtains molecular sieve catalyst semi-finished product；Then it is spray-dried, obtains uniform particle sizes, the catalyst granules of drying, it is fired to obtain the molecular sieve catalyst.The step of this invention simplifies catalyst is prepared, avoids high-temperature roasting fashion material and the more situation of link floor type powder that discharges, improves product yield, the catalyst activity prepared is high, selective stable, extends the service life of catalyst, preparation method is simple, it is easy to operate, it is safe.
Description
Technical field
The present invention relates to catalyst preparation technical field, especially a kind of preparation method of molecular sieve catalyst.
Background technology
Molecular sieve catalyst has been applied successfully to a variety of chemical reaction processes due to its excellent catalytic performance.Existing
For in petrochemical industry, propylene is as a kind of important base stock for being only second to ethylene, for the production of many chemicals.
Molecular sieve catalytic agent producing process is divided into two steps, the i.e. system of molecular sieve semi-finished product used by methanol-to-olefins
Standby and finished catalyst preparation.The preparation of molecular sieve semi-finished product be by raw material according to a certain percentage under the conditions of specific template agent
Synthesis of molecular sieve precursor liquid through oven drying link and carries out high-temperature activation roasting after washing filtering, and product is mixed with water after roasting
Conjunction is ground mashing, until the molecular sieve in slurries is uniformly dispersed and granularity touches the mark requirement, is added in into slurries certain
The dispensing of amount continues to be ground to granularity qualification, obtains the molecular sieve catalyst semi-finished product of slurry.Then mist projection granulating is carried out to do
It is dry, obtain molecular sieve catalyst through high-temperature roasting.
This method preparation process is relatively cumbersome at present, excessively high to equipment requirement, and there are certain drawbacks, and what is prepared urges
Agent activity is not high enough, and selectivity is unstable, and service life is short, and very big inconvenience is brought to production.
The content of the invention
It is an object of the invention to provide a kind of preparation methods of molecular sieve catalyst, can simplify production process, reduce
Production cost extends the service life of catalyst, effectively improves the catalytic activity and selectivity of prepared molecular sieve catalyst,
Product yield is improved, reduces loss.
The object of the invention to solve the technical problems is realized using following technical scheme.
According to a kind of preparation method of molecular sieve catalyst proposed by the present invention, comprise the following steps：
(1) silicon source, silicon source, titanium source, molecular sieve, water are proportionally mixed, by mixture temperature be 250 DEG C, pressure
To react 30h under 2MPa, molecular sieve precursor liquid is obtained；
(2) the molecular sieve precursor liquid is washed, filtered, remove the foreign ion of molecular sieve surface, it then will filtering
Molecular sieve after washing is added to the water stirring and slurry is made；
(3) montmorillonite or kaolinite are added in into above-mentioned slurry, continues agitation grinding 2h, obtain molecular sieve catalyst half into
Product；
(4) above-mentioned molecular sieve catalyst semi-finished product are spray-dried, obtain uniform particle sizes, the catalyst particles of drying
Grain, it is then fired to obtain the molecular sieve catalyst.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
A kind of preparation method of foregoing molecular sieve catalyst, wherein, step (1) by silicon source, silicon source, titanium source, molecular sieve,
Water is according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is (1-2)：(0.8-1)： (0.5-1)：(2-4)：(40-45)
Ratio mixing.
A kind of preparation method of foregoing molecular sieve catalyst, wherein, the temperature of step (4) spray drying is 300-400
DEG C, the temperature of roasting is 700-800 DEG C.
A kind of preparation method of foregoing molecular sieve catalyst, wherein, the molecular sieve is X-type molecular sieve, Y types point
One or both of son sieve, ZSM type molecular sieves are mixed above.
A kind of preparation method of foregoing molecular sieve catalyst, wherein, the silicon source is aluminium oxide, and the silicon source is
Waterglass or Ludox, the titanium source are titanium sulfate or titanium tetrachloride.
The present invention has clear advantage and advantageous effect compared with prior art, by above-mentioned technical proposal, the present invention
A kind of preparation method of molecular sieve catalyst can reach comparable technological progress and practicability, and with the extensive profit in industry
With value, at least there are following advantages：
The step of this invention simplifies catalyst is prepared, avoid high-temperature roasting fashion material and discharging link floor type powder compared with
More situations improves product yield, and the catalyst activity prepared is high, selectivity is stablized, and extends the use of catalyst
In the service life, preparation method is simple, easy to operate, safe.
In conclusion a kind of preparation method of molecular sieve catalyst of the present invention technically has significant progress, and have
Apparent good effect is really a new and innovative, progressive, practical new design.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, special below to lift preferred embodiment, detailed description are as follows.
Specific embodiment
Further to illustrate the present invention to reach the technological means and effect that predetermined goal of the invention is taken, below in conjunction with
Preferred embodiment, to according to a kind of preparation method of molecular sieve catalyst proposed by the present invention, specific embodiment, structure,
Feature and its effect are described in detail as after.
The preparation method of the present invention is as follows：
(1) by silicon source, silicon source, titanium source, molecular sieve, water according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is
(1-2)：(0.8-1)：(0.5-1)：(2-4)：(40-45) ratio mixing, by mixture temperature be 250 DEG C, pressure is
30h is reacted under 2MPa, obtains molecular sieve precursor liquid；
(2) the molecular sieve precursor liquid is washed, filtered, remove the foreign ion of molecular sieve surface, it then will filtering
Molecular sieve after washing is added to the water stirring and slurry is made；
(3) montmorillonite or kaolinite are added in into above-mentioned slurry, continues agitation grinding 2h, obtain molecular sieve catalyst half into
Product；
(4) above-mentioned molecular sieve catalyst semi-finished product at 300-400 DEG C are spray-dried, obtain uniform particle sizes, does
Then dry catalyst granules obtains the molecular sieve catalyst through 700-800 DEG C of roasting 2h.
Preferably, the molecular sieve is more than one or both of X-type molecular sieve, Y type molecular sieve, ZSM type molecular sieves
Mixing, source of aluminium are aluminium oxide, and silicon source is waterglass or Ludox, and titanium source is titanium sulfate or titanium tetrachloride.
Embodiment 1
By silicon source, silicon source, titanium source, molecular sieve, water according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is 1：1：
0.8：3：42 ratio mixing, reacts 30h in the case where temperature is 250 DEG C, pressure is 2MPa by mixture, obtains molecular sieve forerunner
Liquid；The molecular sieve precursor liquid is washed, filters, removes the foreign ion of molecular sieve surface, it then will be after filtration washing
Molecular sieve is added to the water stirring and slurry is made；Montmorillonite is added in into above-mentioned slurry, continues agitation grinding 2h, obtains molecular sieve and urge
Agent semi-finished product；Above-mentioned molecular sieve catalyst semi-finished product at 350 DEG C are spray-dried, obtain uniform particle sizes, drying
Then catalyst granules obtains the molecular sieve catalyst through 780 DEG C of roasting 2h.
Embodiment 2
By silicon source, silicon source, titanium source, molecular sieve, water according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is 2：
0.8：0.5：4：45 ratio mixing, reacts 30h in the case where temperature is 250 DEG C, pressure is 2MPa by mixture, obtains molecular sieve
Precursor liquid；The molecular sieve precursor liquid is washed, is filtered, the foreign ion of molecular sieve surface is removed, then by filtration washing
Molecular sieve afterwards is added to the water stirring and slurry is made；Montmorillonite is added in into above-mentioned slurry, continues agitation grinding 2h, obtains molecule
Sieve catalyst semi-finished product；Above-mentioned molecular sieve catalyst semi-finished product at 300 DEG C are spray-dried, uniform particle sizes is obtained, does
Then dry catalyst granules obtains the molecular sieve catalyst through 700 DEG C of roasting 2h.
Embodiment 3
By silicon source, silicon source, titanium source, molecular sieve, water according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is 1：
0.9：1：2：40 ratio mixing, reacts 30h in the case where temperature is 250 DEG C, pressure is 2MPa by mixture, obtains molecular sieve forerunner
Liquid；The molecular sieve precursor liquid is washed, filters, removes the foreign ion of molecular sieve surface, it then will be after filtration washing
Molecular sieve is added to the water stirring and slurry is made；Kaolinite is added in into above-mentioned slurry, continues agitation grinding 2h, obtains molecular sieve and urge
Agent semi-finished product；Above-mentioned molecular sieve catalyst semi-finished product at 380 DEG C are spray-dried, obtain uniform particle sizes, drying
Then catalyst granules obtains the molecular sieve catalyst through 800 DEG C of roasting 2h.
Embodiment 4
By silicon source, silicon source, titanium source, molecular sieve, water according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is 2：1：
0.7：3：43 ratio mixing, reacts 30h in the case where temperature is 250 DEG C, pressure is 2MPa by mixture, obtains molecular sieve forerunner
Liquid；The molecular sieve precursor liquid is washed, filters, removes the foreign ion of molecular sieve surface, it then will be after filtration washing
Molecular sieve is added to the water stirring and slurry is made；Kaolinite is added in into above-mentioned slurry, continues agitation grinding 2h, obtains molecular sieve and urge
Agent semi-finished product；Above-mentioned molecular sieve catalyst semi-finished product at 400 DEG C are spray-dried, obtain uniform particle sizes, drying
Then catalyst granules obtains the molecular sieve catalyst through 740 DEG C of roasting 2h.
The above described is only a preferred embodiment of the present invention, not make limitation in any form to the present invention, though
So the present invention is disclosed above with preferred embodiment, however is not limited to the present invention, any to be familiar with this professional technology people
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, technical spirit according to the invention
To any simple modification, equivalent change and modification that above example is made, in the range of still falling within technical solution of the present invention.
Claims (5)
1. a kind of preparation method of molecular sieve catalyst, it is characterised in that comprise the following steps：
(1) silicon source, silicon source, titanium source, molecular sieve, water are proportionally mixed, by mixture temperature be 250 DEG C, pressure is
30h is reacted under 2MPa, obtains molecular sieve precursor liquid；
(2) the molecular sieve precursor liquid is washed, filtered, the foreign ion of molecular sieve surface is removed, then by filtration washing
Molecular sieve afterwards is added to the water stirring and slurry is made；
(3) montmorillonite or kaolinite are added in into above-mentioned slurry, continues agitation grinding 2h, obtains molecular sieve catalyst semi-finished product；
(4) above-mentioned molecular sieve catalyst semi-finished product are spray-dried, obtain uniform particle sizes, the catalyst granules of drying, so
The molecular sieve catalyst is obtained by roasting.
2. the preparation method of molecular sieve catalyst as described in claim 1, it is characterised in that step (1) is by silicon source, silicon source, titanium
Source, molecular sieve, water are according to Al2O3:SiO2:TiO2:Molecular sieve：H2The molar ratio of O is (1-2)：(0.8-1)：(0.5-1)：(2-
4)：The ratio mixing of (40-45).
3. the preparation method of molecular sieve catalyst as described in claim 1, it is characterised in that the temperature of step (4) spray drying
For 300-400 DEG C, the temperature of roasting is 700-800 DEG C.
4. the preparation method of molecular sieve catalyst as described in claim 1, it is characterised in that the molecular sieve is X-type molecule
One or both of sieve, Y type molecular sieve, ZSM type molecular sieves are mixed above.
5. the preparation method of molecular sieve catalyst as described in claim 1, it is characterised in that the silicon source be aluminium oxide, institute
The silicon source stated is waterglass or Ludox, and the titanium source is titanium sulfate or titanium tetrachloride.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013531A (en) * | 2019-11-15 | 2020-04-17 | 石家庄汉创环保科技有限公司 | Preparation method of titanium dioxide zeolite molecular sieve for adsorbing volatile organic pollutants |
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| CN101468806A (en) * | 2007-12-25 | 2009-07-01 | 中国石油化工股份有限公司 | ZSM-5 molecular sieve and process for preparing catalytic cracking catalyst containing the same |
| CN102614911A (en) * | 2012-02-23 | 2012-08-01 | 湘潭大学 | One-step molding method of titanium silicalite molecular sieve |
| CN102674389A (en) * | 2012-05-07 | 2012-09-19 | 华东师范大学 | Preparation method of titanium-containing nano-mordenite molecular sieve |
| CN103058223A (en) * | 2013-01-28 | 2013-04-24 | 神华集团有限责任公司 | Molecular sieve catalyst and preparation method thereof |
| WO2013086767A1 (en) * | 2011-12-15 | 2013-06-20 | 中国石油天然气股份有限公司 | Heavy oil catalytic cracking catalyst and preparation method therefor |
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2017
- 2017-12-27 CN CN201711448849.5A patent/CN108101073A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101468806A (en) * | 2007-12-25 | 2009-07-01 | 中国石油化工股份有限公司 | ZSM-5 molecular sieve and process for preparing catalytic cracking catalyst containing the same |
| WO2013086767A1 (en) * | 2011-12-15 | 2013-06-20 | 中国石油天然气股份有限公司 | Heavy oil catalytic cracking catalyst and preparation method therefor |
| CN102614911A (en) * | 2012-02-23 | 2012-08-01 | 湘潭大学 | One-step molding method of titanium silicalite molecular sieve |
| CN102674389A (en) * | 2012-05-07 | 2012-09-19 | 华东师范大学 | Preparation method of titanium-containing nano-mordenite molecular sieve |
| CN103058223A (en) * | 2013-01-28 | 2013-04-24 | 神华集团有限责任公司 | Molecular sieve catalyst and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013531A (en) * | 2019-11-15 | 2020-04-17 | 石家庄汉创环保科技有限公司 | Preparation method of titanium dioxide zeolite molecular sieve for adsorbing volatile organic pollutants |
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Application publication date: 20180601 |