CN110441465A - A kind of anthraquinone hydrogenation catalyst selective evaluation device and evaluation method - Google Patents
A kind of anthraquinone hydrogenation catalyst selective evaluation device and evaluation method Download PDFInfo
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- CN110441465A CN110441465A CN201910661914.5A CN201910661914A CN110441465A CN 110441465 A CN110441465 A CN 110441465A CN 201910661914 A CN201910661914 A CN 201910661914A CN 110441465 A CN110441465 A CN 110441465A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
Abstract
The invention discloses a kind of anthraquinone hydrogenation catalyst selective evaluation device and evaluation methods, evaluating apparatus, it include: reactor, it is vertical to place, it is internal filled with catalyst layer, and the both ends of catalyst layer are separately filled with inert filler layer, and the outer wall of reactor is provided with collet, collet is connect with thermal water source, and the bottom of reactor is provided with sample tap；Flow container is recycled, one end is connected to the bottom of reactor, and the other end is connect with the top of reactor by pump, recycles and be provided with exhaust outlet at the top of flow container；Hydrogen cylinder is connect with the top of reactor；Source nitrogen is connect with the top of reactor.The evaluating apparatus preferably can accurately detect, evaluate the selectivity of catalyst.
Description
Technical field
The invention belongs to catalyst activity assessment technique fields, and in particular to a kind of anthraquinone hydrogenation catalyst selective evaluation
Device and evaluation method.
Background technique
Disclosing the information of the background technology part, it is only intended to increase understanding of the overall background of the invention, without certainty
It is considered as recognizing or implying in any form that information composition has become existing skill well known to persons skilled in the art
Art.
Currently, industrial Hydrogen Peroxide Production generallys use anthraquinone hydrogenation technique, palladium catalyst is the core of this technique production.Anthracene
Quinone working solution carries out hydrogenation reaction under the catalytic action of palladium catalyst and generates hydrogen anthraquinone, and hydrogen anthraquinone is further aoxidized and be can be prepared by
Hydrogen peroxide.In anthraquinone hydrogenation reaction process, it can make anthraquinone that degradation occur with certain side reaction and generate degradation product, degradation product
Generate number with the selectivity of palladium catalyst have direct relation.But the inventors have found that choosing for such catalyst at present
Select the evaluating apparatus and evaluation method that performance evaluation there is no.
Summary of the invention
For above-mentioned the technical problems existing in the prior art, the object of the present invention is to provide a kind of anthraquinone hydrogenation catalysts
Selective evaluation device and evaluation method.The evaluating apparatus preferably can accurately detect, evaluate the selectivity of catalyst.
In order to solve the above technical problems, the technical solution of the present invention is as follows:
A kind of anthraquinone hydrogenation catalyst selective evaluation device, comprising:
Reactor, vertical to place, internal to be filled with catalyst layer, the both ends of catalyst layer are separately filled with inert filler
Layer, the outer wall of reactor are provided with collet, and collet is connect with thermal water source, and the bottom of reactor is provided with sample tap；
Flow container is recycled, one end is connected to the bottom of reactor, and the other end is connect by pump with the top of reactor, recycles
Exhaust outlet is provided at the top of flow container；
Hydrogen cylinder is connect with the top of reactor；
Source nitrogen is connect with the top of reactor.
Source nitrogen is passed through nitrogen into reactor, and the air displacement in reactor is gone out, with guarantee subsequent reactions safety,
It goes on smoothly.
Hydrogen cylinder provides hydrogen feed to be passed through hydrogen in reactor for anthraquinone hydrogenation reaction.
Reactor is vertically placed, wherein being filled with catalyst layer, can extend stop of the reaction system in catalyst layer
Time improves the reacting dose of single cycle.
Reactor is vertically placed, the lower section connection circulation flow container of reactor, after each circular response of reaction solution, is received
Collect in circulation flow container, is passed through the hydrogen in reactor in the top vent discharge of circulation flow container, then will recycle flow container again
In reaction solution circulation be pumped into reactor, continue to react with quantitative hydrogen, carry out subsequent cycle reaction.Using this kind
Structure can guarantee pressure remained steady when each circular response in reactor, and have enough hydrogen to participate in reaction.In addition,
After due to each circular response, directly reaction solution is discharged into circulation flow container, it is ensured that every section in the secondary circular response
The reaction time of reaction solution is equal, and the result to guarantee every sub-sampling is identical as the extent of reaction after the secondary circular response.
Inert filler layer is filled respectively at the both ends of catalyst layer, convenient for the fixation to catalyst, prevents the stream of catalyst
It loses.
It is filled with hot water into the collet of reactor outer wall, to guarantee the constant temperature reacted in reactor.
In some embodiments, liquid valve is provided in the connecting pipe between the reactor and circulation flow container.It adjusts
The aperture of liquid valve, the residence time of adjustable reaction solution in the reactor.
Further, the bottom of the circulation flow container is provided with drain pipe, is provided with valve on drain pipe.End of reaction
Afterwards, the reaction solution of reaction system can be discharged by drain pipe.
In some embodiments, the pump is diaphragm pump.Diaphragm pump is also known as pneumatic diaphragm pump or Pneumatic double diaphragm pump, is
Pump is separated into not connected two parts with elastic film, anti-corrosive rubber or elastic sheet metal, respectively by one kind of reciprocating pump
It is to be conveyed region existing for liquid and movable post.The ipsilateral medium that reciprocates through of movable post is transmitted on diaphragm, makes diaphragm
Also make reciprocal operation, sucked and be discharged through ball shutter by conveying liquid to realize, movable post is not contacted with the liquid of conveying, can
To effectively prevent reaction solution to be polluted by movable post.
In some embodiments, pressure reducing valve is provided in the connecting pipe between the hydrogen cylinder and reactor.
Further, valve is provided on the connecting line between pressure reducing valve and reactor.Aperture is adjusted, to adjust hydrogen
Flow velocity.
In some embodiments, it is provided with pressure sensor in the reactor, pressure sensor is connect with pressure gauge.
Pressure sensor can detecte the pressure in reactor, and show internal pressure by pressure gauge, convenient for control hydrogen
The intake of gas.
In some embodiments, the height of the reactor is 40-50cm, internal diameter 18-22mm.
Further, the height of catalyst layer be 20-30cm, inert filler layer with a thickness of 2-5cm.
Further, the inert filler is glass marble.
A kind of anthraquinone hydrogenation catalyst selective evaluation method, includes the following steps:
Prepared anthraquinone reaction solution is added in circulating storage tank；
It is passed through nitrogen into reactor, inside reactor is replaced, displaced air prevents logical hydrogen after-explosion danger
Danger；
Diaphragm pump is opened, the anthraquinone reaction solution in circulating storage tank is continuously pumped at the top of reactor, while to reaction
It is passed through hydrogen in device, opens the exhaust outlet at the top of circulating storage tank, flows the hydrogen in reactor；
Liquid after each circular response is pooled in circulating storage tank；
It is sampled analysis every setting time, until circular response stops reacting after a certain period of time, when according to overall reaction
The total reduction of interior anthraquinone and the number of circular response calculate the degradation amount that reaction solution single flows through catalyst layer, thus
To the selectivity of catalyst.
In some embodiments, hydrogen is passed through into reactor, maintaining the pressure in reactor is 0.18-0.22Mpa.
The invention has the benefit that
It is heat medium using circulating hot water, is directly heated by collet, reactor temperature is controlled in optimum response
Temperature, temperature control ± 0.1 DEG C, and precision is high.
Working solution is measured using accurate measurement pump, system run all right.
The evaluating apparatus is easy to operate, and data stabilization is reproducible, can effectively measure anthraquinone degradation rate, reflection catalysis
Agent selects performance superiority and inferiority.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation are not constituted an undue limitation on the present application for explaining the application.
Fig. 1 is the selective evaluation apparatus structure schematic diagram of the embodiment of the present invention.
Wherein, 1, hydrogen cylinder, 2, pressure reducing valve, 3, valve, 4, pressure gauge, 5, reactor, 6, liquid valve, 7, circulation flow container,
8, liquid feed valve, 9, diaphragm pump, 10, drain pipe, 11, sample tap, 12, exhaust outlet, 13, thermostatic circulation bath.
Specific embodiment
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Embodiment:
As shown in Figure 1, a kind of anthraquinone hydrogenation catalyst selective evaluation device, comprising:
Reactor 5, vertical to place, internal to be filled with catalyst layer, the both ends of catalyst layer are separately filled with inertia and fill out
The bed of material, the outer wall of reactor are provided with collet, and collet is connect with thermal water source, and the material of collet is S304, are passed through into collet
Heat medium is water or conduction oil etc..
The bottom of reactor 5 is provided with sample tap 11；The height of reactor 5 is 45cm, internal diameter 20mm.Catalyst layer
Height be 20-30cm, inert filler layer with a thickness of 2-5cm.Inert filler is glass marble, and the diameter of glass marble is
Pressure sensor is provided in reactor, pressure sensor is connect with pressure gauge 4.
Flow container 7, material S304 are recycled, one end is connected to the bottom of reactor 5, and the other end passes through pump and reactor
5 top connection, the top of circulation flow container 7 are provided with exhaust outlet 12；In connecting pipe between reactor 5 and circulation flow container 7
It is provided with liquid valve 6, the bottom of circulation flow container 7 is provided with drain pipe 10, is provided with valve on drain pipe 10.The pump is diaphragm
The range of pump 9, diaphragm pump is 0-3L/h, and flow is adjustable, is recycled into reactor 5 for working solution.Diaphragm pump 9 and circulation flow container
Liquid feed valve 8 is provided in connecting pipe between 7.
Hydrogen cylinder 1 is connect with the top of reactor 5；It is provided with and subtracts in connecting pipe between hydrogen cylinder 1 and reactor 5
Pressure valve 2 is provided with valve 3 on the connecting line between pressure reducing valve 2 and reactor 5.Hydrogen cylinder 1 is used to provide hydrogen for hydrogenation
Gas gas source, while maintaining system pressure.
Source nitrogen is connect with the top of reactor.
Anthraquinone hydrogenation catalyst selective evaluation method, includes the following steps:
1, it by reactor flange suitable for reading, is addedGlass marble, bed of material 2cm.That evaluates needed for adding urges
Agent 60g, catalyst bed of material 30cm.It addsGlass marble, bed of material 3cm prevents catalyst from loosening.
2, reactor jacket is connected to thermostatic circulation bath.Circulator bath circulating pump is opened, heating response device is to required
Temperature maintains reactor temperature invariable.
3, anthraquinone working solution 600ml is prepared to obtain by reactor addition suitable for reading, opens valve 6 and 12, makes treatment fluid flow
To circulation liquid storage tank.
4, gas circuit is connected, first system is replaced with nitrogen.Valve 8 is opened, diaphragm pump 9 is opened and conveys working solution
To reactor, working solution essence reactor is back to circulation flow container and realizes circulation.
5, gas cylinder 1 is opened, valve 3 makes hydrogen enter reactor, maintains reactor pressure in 0.2Mpa.Crack valve
12, make the hydrogen discharge for entering circulation flow container, maintains hydrogen flowing in reactor.
6, valve 11 is opened every 1h to be sampled.6 hours stopping evaluation responses being carried out to reaction.
7, general anthraquinone amount in every sub-sampling sample working solution is analyzed, by working solution additive amount and diaphragm pump feed speed,
Calculate working solution cycle-index.Working solution single pass bed degradation amount is calculated by 6h general anthraquinone reduction amount and cycle-index,
To obtain catalyst choice.
Selectivity=(general anthraquinone amount ÷ cycle-index before general anthraquinone amount ÷ reacts after 1- reaction) × 100%.
The foregoing is merely preferred embodiment of the present application, are not intended to limit this application, for the skill of this field
For art personnel, various changes and changes are possible in this application.Within the spirit and principles of this application, made any to repair
Change, equivalent replacement, improvement etc., should be included within the scope of protection of this application.
Claims (10)
1. a kind of anthraquinone hydrogenation catalyst selective evaluation device, it is characterised in that: include:
Reactor, vertical to place, internal to be filled with catalyst layer, the both ends of catalyst layer are separately filled with inert filler layer,
The outer wall of reactor is provided with collet, and collet is connect with thermal water source, and the bottom of reactor is provided with sample tap；
Flow container is recycled, one end is connected to the bottom of reactor, and the other end is connect by pump with the top of reactor, recycles flow container
Top be provided with exhaust outlet；
Hydrogen cylinder is connect with the top of reactor；
Source nitrogen is connect with the top of reactor.
2. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: the reactor with
Liquid valve is provided in connecting pipe between circulation flow container；
Further, the bottom of the circulation flow container is provided with drain pipe, is provided with valve on drain pipe.
3. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: the pump is diaphragm
Pump.
4. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: the hydrogen cylinder with
Pressure reducing valve is provided in connecting pipe between reactor；
Further, valve is provided on the connecting line between pressure reducing valve and reactor.
5. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: in the reactor
It is provided with pressure sensor, pressure sensor is connect with pressure gauge.
6. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: the reactor
Height is 40-50cm, internal diameter 18-22mm.
7. anthraquinone hydrogenation catalyst selective evaluation device according to claim 6, it is characterised in that: the height of catalyst layer
Degree be 20-30cm, inert filler layer with a thickness of 2-5cm.
8. anthraquinone hydrogenation catalyst selective evaluation device according to claim 1, it is characterised in that: the inert filler
For glass marble.
9. a kind of anthraquinone hydrogenation catalyst selective evaluation method, characterized by the following steps:
Prepared anthraquinone reaction solution is added in circulating storage tank；
It is passed through nitrogen into reactor, inside reactor is replaced；
Diaphragm pump is opened, the anthraquinone reaction solution in circulating storage tank is continuously pumped at the top of reactor, while into reactor
It is passed through hydrogen, the exhaust outlet at the top of circulating storage tank is opened, flows the hydrogen in reactor；
Liquid after each circular response is pooled in circulating storage tank；
It is sampled analysis every setting time, until circular response stops reacting after a certain period of time, according in total reaction time
The total reduction of anthraquinone and the number of circular response calculate reaction solution single and flow through the degradation amount of catalyst layer, to be urged
The selectivity of agent.
10. anthraquinone hydrogenation catalyst selective evaluation method according to claim 9, it is characterised in that: into reactor
It is passed through hydrogen, maintaining the pressure in reactor is 0.18-0.22Mpa.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0596938B1 (en) * | 1991-07-31 | 1998-10-07 | Kemira Oy | Process for the preparation of hydrogen peroxide |
| CN1673069A (en) * | 2005-03-11 | 2005-09-28 | 天津大学 | Operation process for hydrogenation reaction of anthraquinone work liquid during hydrogen perioxide production |
| CN101177246A (en) * | 2007-11-02 | 2008-05-14 | 山东百川汇通化工科技有限公司 | Method for producing oxydol by dihydrodiketoanthracene method |
| CN106430108A (en) * | 2016-10-10 | 2017-02-22 | 中国石油大学(北京) | System and method for preparing hydrogen peroxide through anthraquinone method under supergravity condition |
| CN106629622A (en) * | 2017-03-02 | 2017-05-10 | 中触媒新材料股份有限公司 | Hydrogenation method and hydrogenation device for oxanthranol-containing working solution |
| CN106629618A (en) * | 2017-01-03 | 2017-05-10 | 河北美邦工程科技股份有限公司 | Fluidized bed hydrogenation reaction and separation process and device for producing hydrogen peroxide by virtue of anthraquinone method |
| CN206627487U (en) * | 2017-03-27 | 2017-11-10 | 中触媒新材料股份有限公司 | A kind of evaluating apparatus of anthraquinone producing hydrogen peroxide hydrogenation catalyst |
| CN208003919U (en) * | 2017-12-19 | 2018-10-26 | 鲁西催化剂有限公司 | A kind of anthraquinone hydrogenation catalyst evaluating apparatus |
-
2019
- 2019-07-22 CN CN201910661914.5A patent/CN110441465A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0596938B1 (en) * | 1991-07-31 | 1998-10-07 | Kemira Oy | Process for the preparation of hydrogen peroxide |
| CN1673069A (en) * | 2005-03-11 | 2005-09-28 | 天津大学 | Operation process for hydrogenation reaction of anthraquinone work liquid during hydrogen perioxide production |
| CN101177246A (en) * | 2007-11-02 | 2008-05-14 | 山东百川汇通化工科技有限公司 | Method for producing oxydol by dihydrodiketoanthracene method |
| CN106430108A (en) * | 2016-10-10 | 2017-02-22 | 中国石油大学(北京) | System and method for preparing hydrogen peroxide through anthraquinone method under supergravity condition |
| CN106629618A (en) * | 2017-01-03 | 2017-05-10 | 河北美邦工程科技股份有限公司 | Fluidized bed hydrogenation reaction and separation process and device for producing hydrogen peroxide by virtue of anthraquinone method |
| CN106629622A (en) * | 2017-03-02 | 2017-05-10 | 中触媒新材料股份有限公司 | Hydrogenation method and hydrogenation device for oxanthranol-containing working solution |
| CN206627487U (en) * | 2017-03-27 | 2017-11-10 | 中触媒新材料股份有限公司 | A kind of evaluating apparatus of anthraquinone producing hydrogen peroxide hydrogenation catalyst |
| CN208003919U (en) * | 2017-12-19 | 2018-10-26 | 鲁西催化剂有限公司 | A kind of anthraquinone hydrogenation catalyst evaluating apparatus |
Non-Patent Citations (1)
| Title |
|---|
| 姚冬龄: "蒽醌法生产过氧化氢工艺中活性氧化铝的应用", 《无机盐工业》 * |
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