CN104888816A - Aluminum trichloride-immobilized catalyst boiling bed production apparatus and preparation technology thereof - Google Patents
Aluminum trichloride-immobilized catalyst boiling bed production apparatus and preparation technology thereof Download PDFInfo
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- CN104888816A CN104888816A CN201510227304.6A CN201510227304A CN104888816A CN 104888816 A CN104888816 A CN 104888816A CN 201510227304 A CN201510227304 A CN 201510227304A CN 104888816 A CN104888816 A CN 104888816A
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- alcl
- gas
- bed reactor
- fluidized bed
- supported catalyst
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Abstract
The invention relates to an aluminum trichloride-immobilized catalyst production apparatus and a preparation technology thereof. especially relates to an aluminum trichloride-immobilized catalyst boiling bed production apparatus and a preparation technology thereof. A technical scheme of the present invention is characterized in that N2 gas is introduced in a CCl4 storage tank through a N2 flowmeter, N2 is taken as a carrying gas for carrying the CCl4 saturated vapor into an AlCl3 generator, AlCl3 gas is generated by reacting with Al2O3, AlCl3 gas is introduced in to a boiling bed reactor through a cooler, and is immobilized with a suspension carrier in the boiling bed; a gas internal circulation method is employed in the boiling bed reactor, so that AlCl3 is cycled in the boiling bed, and is fully contacted with carrier particles for reacting, N2 gas containing a few of AlCl3 passes through an AlCl3 collector, and is washed to remove the residual AlCl3 and then is discharged into atmosphere; and aluminum trichloride-immobilized catalyst is recovered for storage. The apparatus is easy for industrial production, equipment corrosion, environmental pollution and difficult separating with products can be effectively solved, and the method has the advantages of low reaction temperature, high immobilization rate and uniform supporting.
Description
Technical field
The present invention relates to aluminium trichloride solid-supported catalyst process units composition and preparation technology field, particularly a kind of aluminium trichloride solid-supported catalyst ebullated bed process units and preparation technology.
Background technology
Alchlor is as Fu-Ke catalysts; there is purposes widely; it is one of the catalyst of chemical industry, petroleum refining and pharmacy; it reveals excellent catalytic performance to the reaction table of alkylation, acyl group, alkane isomerization, cracking and polymerization; but the comparatively strong and aftertreatment technology more complicated of the corrosivity of this catalyst; with product separation difficulty and use produce a large amount of waste water cause environmental pollution, unbecoming with the theory of cleaner production, its application is restricted day by day.
In order to address this problem, people start AlCl always
3immobilized, at maintenance AlCl
3under the prerequisite of good characteristic, it is made to be transformed into environment amenable catalyst.AlCl
3immobilized research had made great progress at nearly 30 years, invent multiple aluminium trichloride solid-supported catalyst preparation technology both at home and abroad, as patent of invention: USP2.927.087(1960), USP4.306.105(1981), CN 1324690A(2001), CN1939590A(2007), CN102247885(2011), CN03894225A(2014) etc.
The common feature of above-mentioned patented technology is by gaseous state AlCl
3use N
2the catalyst carrier being carried to fixed bed is carried out immobilized.Because fixed bed exists some problems: as solid particle poor heat transfer, bed temperature is uneven, AlCl
3diffusion difficulty on fixed bed carrier, hot-spot causes hydroxyl loss and the change of carrier crystalline form etc., and therefore cause catalyst prod to support low, product quality can not be guaranteed, and therefore the supported catalyst technology of fixed bed is difficult to suitability for industrialized production.
For the problems referred to above, the invention provides a kind of ebullated bed process units and preparation technology of aluminium trichloride solid-supported catalyst, for realizing the suitability for industrialized production of aluminium trichloride solid-supported catalyst.With this device and the supported AlCl of technique
3catalyst can not only effectively solve equipment corrosion, environmental pollution and with the problem such as product separation difficulty, and the AlCl supported
3for nanostructured, have low, the immobilized rate of reaction temperature high, support the advantage such as evenly.The extensive use of aluminium trichloride solid-supported catalyst, by the huge economic benefit of generation and environmental benefit, meets the requirement of current recycling economy development.
Summary of the invention
The object of this invention is to provide a kind of can the ebullated bed process units of suitability for industrialized production aluminium trichloride solid-supported catalyst and preparation technology.
For overcoming prior art problem, the invention provides a kind of aluminium trichloride solid-supported catalyst ebullated bed process units, comprising N
2flowmeter, CCl
4storage tank, AlCl with heater
3generator, cooler, fluidized bed reactor and AlCl
3collector; N
2flowmeter and CCl
4storage tank connects, CCl
4storage tank and AlCl
3generator connects, AlCl
3generator is connected with cooler, and cooler is connected with bottom fluidized bed reactor, fluidized bed reactor top and AlCl
3collector connects; Fluidized bed reactor comprises: cyclone separator, inner circulating tube, catalyst discharging opening, immobilized ebullated bed; Immobilized ebullated bed is arranged on the bottom of fluidized bed reactor, cyclone separator is arranged at fluidized bed reactor top, inner circulating tube one end is connected with cyclone separator, and the other end causes fluidized bed reactor inner bottom part, and catalyst discharging opening is positioned on fluidized bed reactor sidewall; Heater is inductive heater; Immobilized ebullated bed comprises impeller, motor, sieve aperture cone Compound Distribution plate, and impeller and motor connect, and sieve aperture cone Compound Distribution plate is arranged on above impeller; Below impeller, thermostat is set; The structure of sieve aperture cone Compound Distribution plate comprises cone and sieve aperture, and some cones are distributed on Compound Distribution plate, and distribute around cone some sieve apertures; Cyclone separator and inner circulating tube form AlCl
3gas internal circulation system.
The invention provides a kind of aluminium trichloride solid-supported catalyst ebullated bed process for producing, process is N
2through N
2flowmeter enters CCl
4in storage tank, with N
2for CCl is carried in carrier gas
4saturated vapor enters AlCl
3in generator, with Al
2o
3add thermal response and generate AlCl
3gas, AlCl
3gas enters in fluidized bed reactor, carries out immobilized with the suspending carrier in ebullated bed, immobilized rear collection AlCl
3solid-supported catalyst.In fluidized bed reactor, adopt gas Inner eycle method, make AlCl
3at ebullated bed Inner eycle, haptoreaction abundant with carrier granular, containing a small amount of AlCl
3n
2gas, through AlCl
3collector, then remove residual AlCl by washing
3air is entered after gas; Al
2o
3the temperature adding thermal response is 400 ~ 500
oc.
The invention has the beneficial effects as follows: the ebullated bed process units and the preparation technology that the invention provides a kind of aluminium trichloride solid-supported catalyst, adopt N
2direct gas carries CCl
4method, can reduce cost of equipment and the maintenance cost of measuring pump, and tolerance is uniform and stable, operation and maintenance is convenient.Cone and sieve aperture Compound Distribution plate, can ensure that the solid particle of different size is all in suspended state in ebullated bed space, avoids the deposition of oversized particles and cross short grained effusion, making AlCl
3obtain immobilized preferably on the carrier particles.Adopt inductive heater temperature control, the problem that particulate matter poor heat transfer, temperature distributing disproportionation are even can be solved.Have the advantages that heating quality is even, firing rate is fast, power is large, temperature adjusting precision is high.AlCl
3gas can be recycled in fluidized bed reactor.AlCl can be improved
3the service efficiency of gas, improves the immobilized rate of carrier.
The present invention is for realizing the suitability for industrialized production of aluminium trichloride solid-supported catalyst.With this device and the supported AlCl of technique
3catalyst can not only effectively solve equipment corrosion, environmental pollution and with the problem such as product separation difficulty, and the AlCl supported
3for nanostructured, have low, the immobilized rate of reaction temperature high, support the advantage such as evenly.
Accompanying drawing explanation
Fig. 1 is a kind of schematic diagram of aluminium trichloride solid-supported catalyst ebullated bed process units;
Fig. 2 is the top view of sieve aperture cone Compound Distribution plate structure.
In figure: 1, N
2flowmeter, 2, CCl
4storage tank, 3, AlCl
3generator, 4, inductive heater, 5, cooler, 6, thermostat, 7, sieve aperture cone Compound Distribution plate, 8, fluidized bed reactor, 9, cyclone separator, 10, inner circulating tube, 11, catalyst discharging opening, 12, impeller, 13, motor, 14, A lCl
3collector, 15, cone, 16, sieve aperture, 17, entrance.
Detailed description of the invention
Implementation process of the present invention is further illustrated below in conjunction with accompanying drawing.Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
0.5 Kg γ-Al is loaded in fluidized bed reactor
2o
3(60-80 order) carrier, preferred diplopore γ-Al
2o
3(60-80 order), high pure nitrogen passes through N
2flowmeter (1) enters CCl with the flow of 0.4 L/min
4basin (2), N
2carry CCl
4gas, enters AlCl through pipeline
3generator (3).AlCl
3generator (3) is built with γ-Al
2o
31.0 Kg, by being enclosed within AlCl
3inductive heater (4) control AlCl on generator (3)
3reaction temperature in generator (3) reaches 450
oc.CCl
4with Al
2o
3reaction generates AlCl
3gas, after condenser (5) cooling, enter fluidized bed reactor (8) bottom, thermostat (6) temperature of fluidized bed reactor (8) bottom controls 300
oc.
The air-flow produced by motor (13) impeller (12) High Rotation Speed is by AlCl
3gas passes through through thermostat (6) and cone sieve aperture Compound Distribution plate (7), with the γ-Al suspended
2o
3(60-80 order) carrier fully contacts and carries out immobilized reaction.Gas Inner eycle method is adopted, i.e. still unreacted AlCl in fluidized bed reactor (8)
3enter cyclone separator (9) from cyclone separator side wall entrance (17), be separated through cyclone separator (9), still unreacted AlCl
3enter inner circulating tube (10), return to fluidized bed reactor (8) bottom through thermostat (6), the air-flow produced by motor (13) impeller (12) High Rotation Speed is again by AlCl
3by cone sieve aperture Compound Distribution plate (7), enter fluidized bed reactor and carrier granular carries out immobilized reaction, iterative cycles like this.React operation of stopping after 1 hour.Finished catalyst after immobilized is released by catalyst discharging opening (11), finished catalyst sealed storage.After testing, AlCl in solid-supported catalyst
3loading reach 6.2%.
Finally containing a small amount of AlCl
3n
2gas, through AlCl
3collector (14), is thoroughly removing residual AlCl by washing
3after enter air.
Claims (9)
1. an aluminium trichloride solid-supported catalyst ebullated bed process units, is characterized in that: comprise N
2flowmeter, CCl
4storage tank, AlCl with heater
3generator, cooler, fluidized bed reactor and AlCl
3collector; N
2flowmeter and CCl
4storage tank connects, CCl
4storage tank and AlCl
3generator connects, AlCl
3generator is connected with cooler, and cooler is connected with bottom fluidized bed reactor, fluidized bed reactor top and AlCl
3collector connects; Fluidized bed reactor comprises: cyclone separator, inner circulating tube, catalyst discharging opening, immobilized ebullated bed; Immobilized ebullated bed is arranged on the bottom of fluidized bed reactor, cyclone separator is arranged at fluidized bed reactor top, inner circulating tube one end is connected with cyclone separator, and the other end causes fluidized bed reactor inner bottom part, and catalyst discharging opening is positioned on fluidized bed reactor sidewall.
2. a kind of aluminium trichloride solid-supported catalyst ebullated bed process units according to claim 1, is characterized in that: described heater is inductive heater.
3. a kind of aluminium trichloride solid-supported catalyst ebullated bed process units according to claim 1, is characterized in that: described immobilized ebullated bed comprises impeller, motor, sieve aperture cone Compound Distribution plate; Impeller is connected with motor, and sieve aperture cone Compound Distribution plate is arranged on above impeller.
4. a kind of aluminium trichloride solid-supported catalyst ebullated bed process units according to claim 3, is characterized in that: arrange thermostat below described impeller.
5. a kind of aluminium trichloride solid-supported catalyst ebullated bed process units according to claim 3, it is characterized in that: the structure of described sieve aperture cone Compound Distribution plate comprises cone and sieve aperture, some cones are distributed on Compound Distribution plate, and distribute around cone some sieve apertures.
6. a kind of aluminium trichloride solid-supported catalyst ebullated bed process units according to claim 1, is characterized in that: described cyclone separator and inner circulating tube form AlCl
3gas internal circulation system.
7. an aluminium trichloride solid-supported catalyst ebullated bed process for producing, is characterized in that: N
2through N
2flowmeter enters CCl
4in storage tank, with N
2for CCl is carried in carrier gas
4saturated vapor enters AlCl
3in generator, with Al
2o
3add thermal response and generate AlCl
3gas, AlCl
3gas enters in fluidized bed reactor, carries out immobilized with the suspending carrier in ebullated bed, immobilized rear collection AlCl
3solid-supported catalyst.
8. a kind of aluminium trichloride solid-supported catalyst ebullated bed process for producing according to claim 7, is characterized in that: in fluidized bed reactor, adopt gas Inner eycle method, make AlCl
3at fluidized bed reactor Inner eycle, with carrier granular haptoreaction, containing a small amount of AlCl
3n
2gas, through AlCl
3collector, then remove residual AlCl by washing
3air is entered after gas.
9. a kind of aluminium trichloride solid-supported catalyst ebullated bed process for producing according to claim 7, is characterized in that: Al
2o
3the temperature adding thermal response is 400 ~ 500
oc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510227304.6A CN104888816B (en) | 2015-05-07 | 2015-05-07 | A kind of aluminium trichloride solid-supported catalyst ebullated bed process units |
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|---|---|---|---|
| CN201510227304.6A CN104888816B (en) | 2015-05-07 | 2015-05-07 | A kind of aluminium trichloride solid-supported catalyst ebullated bed process units |
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| Publication Number | Publication Date |
|---|---|
| CN104888816A true CN104888816A (en) | 2015-09-09 |
| CN104888816B CN104888816B (en) | 2017-04-05 |
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ID=54022020
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510227304.6A Expired - Fee Related CN104888816B (en) | 2015-05-07 | 2015-05-07 | A kind of aluminium trichloride solid-supported catalyst ebullated bed process units |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517238A (en) * | 2016-12-07 | 2017-03-22 | 四川润和催化新材料股份有限公司 | Equipment for preparing Y type molecular sieve with low sodium and high silica-alumina ratio and preparation method |
| CN106861562A (en) * | 2017-03-25 | 2017-06-20 | 上海复榆新材料科技有限公司 | A kind of reaction unit for preparing Si hydrophobic Y zeolite adsorbents high |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324690A (en) * | 2000-05-19 | 2001-12-05 | 中国石油化工集团公司 | preparation of fixed and carried aluminium trichloride catalyst |
| US20030019789A1 (en) * | 2000-03-20 | 2003-01-30 | Ho-Jun Kwak | Method and system for continuously preparing gasoline, kerosene and diesel oil from waste plastics |
| CN1556080A (en) * | 2003-12-31 | 2004-12-22 | 大连理工大学 | Method of producing poly alpha olefine oil using alpha olefine as raw material |
-
2015
- 2015-05-07 CN CN201510227304.6A patent/CN104888816B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030019789A1 (en) * | 2000-03-20 | 2003-01-30 | Ho-Jun Kwak | Method and system for continuously preparing gasoline, kerosene and diesel oil from waste plastics |
| CN1324690A (en) * | 2000-05-19 | 2001-12-05 | 中国石油化工集团公司 | preparation of fixed and carried aluminium trichloride catalyst |
| CN1556080A (en) * | 2003-12-31 | 2004-12-22 | 大连理工大学 | Method of producing poly alpha olefine oil using alpha olefine as raw material |
Non-Patent Citations (1)
| Title |
|---|
| 刘宝春等: "利用沸腾床反应器制备碳纳米管", 《催化学报》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106517238A (en) * | 2016-12-07 | 2017-03-22 | 四川润和催化新材料股份有限公司 | Equipment for preparing Y type molecular sieve with low sodium and high silica-alumina ratio and preparation method |
| CN106517238B (en) * | 2016-12-07 | 2019-01-18 | 四川润和催化新材料股份有限公司 | It is a kind of to prepare equipment and preparation method of the low-Na and high-Si aluminium than Y type molecular sieve |
| CN106861562A (en) * | 2017-03-25 | 2017-06-20 | 上海复榆新材料科技有限公司 | A kind of reaction unit for preparing Si hydrophobic Y zeolite adsorbents high |
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| Publication number | Publication date |
|---|---|
| CN104888816B (en) | 2017-04-05 |
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Granted publication date: 20170405 Termination date: 20200507 |