CN103769245A - Magnetically-stabilized separation sleeving use method of catalyst - Google Patents
Magnetically-stabilized separation sleeving use method of catalyst Download PDFInfo
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- CN103769245A CN103769245A CN201210405120.0A CN201210405120A CN103769245A CN 103769245 A CN103769245 A CN 103769245A CN 201210405120 A CN201210405120 A CN 201210405120A CN 103769245 A CN103769245 A CN 103769245A
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Abstract
The invention belongs to the technical field of catalyst application and relates to a magnetically-stabilized separation sleeving use method of a catalyst. According to the method, a magnetic kettle sleeve is designed and sleeves the bottom of a reactor, through a magnetic force, catalyst particles are stabilized and collision between the solid particles is reduced in stirring, and after the reaction, catalyst particle settlement is accelerated and the catalyst particles are stably adsorbed on the bottom of the reactor so that a catalyst loss is reduced and solid-liquid separation is realized. After sleeving use, in an N2 protective atmosphere, the material is extruded by technical N2 so that air contact oxidation of the catalyst is avoided. The method is suitable for catalysts containing magnetic conductive metals such as iron, cobalt and nickel. The method can obviously reduce or avoid catalyst loss, reduce supplement frequency and supplement amount of the catalyst in industrial production and prolong a catalyst service life. The catalyst treated by the method can be separated from the reaction system after the reaction. The method simplifies a product purification process and is conducive to catalyst recovery and treatment.
Description
Technical field
The invention belongs to catalyst applied technical field, be specifically related to a kind of catalyst magnetic and surely separate using method.
Background technology
In autoclave hydrogenation process at intermittence, often because handling material makes catalyst exposure oxidized inactivation in air; Simultaneously in tank reactor high-pressure hydrogenation process, Gu because violent mechanical agitation makes the mutual intense impact of liquid------gas three-phase, easily cause the fragmentation of catalyst granules, broken particulate runs off in a large number in separation process, both cause catalyst loss, caused again environmental pollution.How reducing or avoid the loss of catalyst, is one of major issue facing in catalyst use, the separation processes such as Raney's nickel.
Summary of the invention
The object of the invention is for the problems referred to above, surely separate using method and proposed a kind of catalyst magnetic.
Main technical schemes of the present invention: designed magnetic still cover, be enclosed within Polycondensation Reactor and Esterification Reactor, by magnetic force rugged catalyst particle, reduce and between solid particle, collide in whipping process, the sedimentation of accelerator activator particle when reaction finishes, and more stably inhale at the bottom of still, reduce catalyst loss, realize Separation of Solid and Liquid.
The steady separation sleeve of catalyst magnetic, with in examination journey, is once applied mechanically end, logical N
2protection, and utilize technique N
2material is extruded, avoid the oxidation of catalyst ingress of air.
Magnetic still cover is according to Polycondensation Reactor and Esterification Reactor shape fabricating, and as required, magnetic material can be electromagnet or other permanent magnet.
This bright autoclave intermittent reaction device that is applicable to, and use the catalyst of the magnetic conductive metals such as iron content, cobalt, nickel.
The present invention can significantly reduce or avoid catalyst loss, reduces catalyst and fills into number of times and quantity, extending catalyst service life in industrial production.And catalyst easily separates with reaction system after reaction finishes, simplify purifying products technique, be conducive to the recycling of catalyst.The final recovery of catalyst can be filtered joint by arranging in liquid phase discharge pipe, and auxiliary magnetic field, in nitrogen stream, filters, and can fully reclaim catalyst.
Accompanying drawing explanation
Fig. 1 is embodiment of the present invention reactor and each block diagram.
1-gas phase feed inlet and outlet, 2-flange, 3-agitator, 4-liquid phase feed inlet and outlet, 5-liquid phase material, 6-catalyst, 7-magnetic still cover.
The specific embodiment
The test of applying mechanically of preparing 4-ADPA below by 4 nitrodiphenyl amine hydrogenating reduction illustrates the present invention.
Embodiment:
The present embodiment as shown in Figure 1, have on autoclave-gas phase feed inlet and outlet 1, flange 2, agitator 3, liquid phase feed inlet and outlet 4, has liquid phase material 5 and catalyst 6 in autoclave, install magnetic still cover 7 additional at autoclave outer bottom.
In still, add successively p-nitrodiphenylamine, solvent and catalyst, after enclosed high pressure still, successively logical nitrogen, hydrogen, displacement gas reactor.Logical hydrogen starts stirring to certain pressure, is warming up to uniform temperature, and reaction is terminal to not inhaling hydrogen.Stop stirring, cooling, sedimentation 15min.According to catalyst amount, suitably adjust liquid-phase tube and go out open height, after completing with catalyst sedimentation, the mouth of pipe is as the criterion above remaining on catalyst layer, after having reacted, passes into N
2extrude liquid phase material, allow a little liquid phase material residual.Remove by filter a small amount of entrained catalyst, analyze p-nitrodiphenylamine and mutual-amido two polyaniline content in filtrate, calculate conversion ratio and selective.Again feed intake and apply mechanically test next time.
Comparative example:
In autoclave, add successively p-nitrodiphenylamine, solvent and catalyst, after enclosed high pressure still, successively logical nitrogen, hydrogen, displacement gas reactor.Logical hydrogen starts stirring to certain pressure, is warming up to uniform temperature, and reaction is terminal to not inhaling hydrogen.Stop stirring, cooling, sedimentation 15min.According to catalyst amount, suitably adjust liquid-phase tube and go out open height, after completing with catalyst sedimentation, the mouth of pipe is as the criterion above remaining on catalyst layer, after having reacted, passes into N
2extrude liquid phase material, allow a little liquid phase material residual.Remove by filter a small amount of entrained catalyst, analyze p-nitrodiphenylamine and mutual-amido two polyaniline content in filtrate, calculate conversion ratio and selective.Again feed intake and apply mechanically test next time.
Process conditions:
P-nitrodiphenylamine condensation liquid 100mL, catalyst 15g, reaction temperature is controlled at below 80 ℃, reaction pressure 0.5～1.5MPa, initial pressure is 0.5MPa.Solvent is industrial methanol (99%), and consumption is to be 1:1 reaction time 60min with p-nitrodiphenylamine condensation liquid volume ratio.
Carry out difference by above-described embodiment and comparative example and apply mechanically experiment contrast, apply mechanically experimental result as shown in the table:
The different using method experiment of table 1 contrast
As can be seen from the above table, under condition, increase along with applying mechanically number of times, hydrogenation conversion reduces gradually, applies mechanically after 10 times, adopts one group of magnetic still cover to apply mechanically experiment hydrogenation conversion 98.6%, does not add one group of hydrogenation conversion 95.4% of magnetic still cover.Have suffered in the process of applying mechanically, hydrogenation conversion is clear and definite downward trend, and mutual-amido two polyaniline yield remains on more than 95%.
Above two groups of experimental techniques are applied mechanically after 10 times, adopt magnetic still cover group residual catalyst 14.2g, and catalyst recovery yield 94.6%, does not add magnetic still cover group residual catalyst 11.5g, and 76.6%, two group of experiment catalyst loss gap of catalyst recovery yield is obvious.
This invention can significantly increase catalyst and apply mechanically number of times, reduces catalyst and fills into number of times and quantity, extending catalyst service life in industrial production.And catalyst is easy to separate with reaction system after reaction finishes, and can reach the more than 94.6% of addition to the recovery of catalyst, facilitates the post processing of catalyst.
Claims (5)
1. a catalyst magnetic surely separates using method, it is characterized in that being enclosed within Polycondensation Reactor and Esterification Reactor with magnetic still cover, in reaction, by magnetic force, catalyst is stablized, reduce collision, the sedimentation of accelerator activator particle when reaction finishes, magnetic still cover is stably inhaled in Polycondensation Reactor and Esterification Reactor, reduces catalyst loss, realizes Separation of Solid and Liquid.
2. catalyst magnetic as claimed in claim 1 surely separates using method, it is characterized in that magnetic still cover is according to Polycondensation Reactor and Esterification Reactor shape fabricating, and magnetic material is electromagnet or other permanent magnet.
3. catalyst magnetic as claimed in claim 1 surely separates using method, it is characterized in that reaction finishes discharging and utilizes N
2material is extruded, pass through N
2protection, avoids the oxidation of catalyst ingress of air.
4. catalyst magnetic as claimed in claim 1 surely separates using method, it is characterized in that for autoclave intermittent reaction device.
5. catalyst magnetic as claimed in claim 1 surely separates using method, it is characterized in that the magnetic conductive metal catalyst for comprising iron content, cobalt, nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210405120.0A CN103769245A (en) | 2012-10-23 | 2012-10-23 | Magnetically-stabilized separation sleeving use method of catalyst |
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| CN201210405120.0A CN103769245A (en) | 2012-10-23 | 2012-10-23 | Magnetically-stabilized separation sleeving use method of catalyst |
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| CN103769245A true CN103769245A (en) | 2014-05-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622039A (en) * | 2016-12-12 | 2017-05-10 | 中北大学 | Reaction and separation integrated process and device for synthesizing poly-alpha-olefin (PAO) |
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| WO2004101442A1 (en) * | 2003-05-19 | 2004-11-25 | Ntu Ventures Private Limited | Method and system for the degradation of halogenated compounds |
| CN1690035A (en) * | 2004-04-29 | 2005-11-02 | 中国石油化工股份有限公司 | Process for hydrogenation of alkyl anthraquinone by using magnetically stabilized bed |
| US20090065437A1 (en) * | 2007-09-10 | 2009-03-12 | Rentech, Inc. | Magnetic separation combined with dynamic settling for fischer-tropsch processes |
| CN102375045A (en) * | 2010-08-17 | 2012-03-14 | 中国石油化工股份有限公司 | Evaluation method of polypropylene synthesis catalyst |
| CN102516013A (en) * | 2011-11-09 | 2012-06-27 | 中国石油大学(华东) | Method for preparing cyclohexene by selectively hydrogenising benzene in magnetic stabilization bed |
-
2012
- 2012-10-23 CN CN201210405120.0A patent/CN103769245A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004101442A1 (en) * | 2003-05-19 | 2004-11-25 | Ntu Ventures Private Limited | Method and system for the degradation of halogenated compounds |
| CN1690035A (en) * | 2004-04-29 | 2005-11-02 | 中国石油化工股份有限公司 | Process for hydrogenation of alkyl anthraquinone by using magnetically stabilized bed |
| US20090065437A1 (en) * | 2007-09-10 | 2009-03-12 | Rentech, Inc. | Magnetic separation combined with dynamic settling for fischer-tropsch processes |
| CN102375045A (en) * | 2010-08-17 | 2012-03-14 | 中国石油化工股份有限公司 | Evaluation method of polypropylene synthesis catalyst |
| CN102516013A (en) * | 2011-11-09 | 2012-06-27 | 中国石油大学(华东) | Method for preparing cyclohexene by selectively hydrogenising benzene in magnetic stabilization bed |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622039A (en) * | 2016-12-12 | 2017-05-10 | 中北大学 | Reaction and separation integrated process and device for synthesizing poly-alpha-olefin (PAO) |
| CN106622039B (en) * | 2016-12-12 | 2019-08-30 | 中北大学 | The integrated reaction and separation technique and device of synthesizing poly alpha-olefin (PAO) |
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Application publication date: 20140507 |