CN101613327A - A kind of device and production technique thereof of protecting morpholine catalyst - Google Patents

A kind of device and production technique thereof of protecting morpholine catalyst Download PDF

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Publication number
CN101613327A
CN101613327A CN200910144251A CN200910144251A CN101613327A CN 101613327 A CN101613327 A CN 101613327A CN 200910144251 A CN200910144251 A CN 200910144251A CN 200910144251 A CN200910144251 A CN 200910144251A CN 101613327 A CN101613327 A CN 101613327A
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Prior art keywords
valve
carbon
tank body
filler
cleaner
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CN101613327B (en
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饶金铎
刘博�
张超
王继学
潘家成
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Anhui Haoyuan Chemical Industry (Group) Co Ltd
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Anhui Haoyuan Chemical Industry (Group) Co Ltd
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Abstract

A kind of device and production technique thereof of protecting morpholine catalyst; be in fresh hydrogen; the gas ammonia that circulation gas mixture and heating and gasifying are crossed enters before the reaction bed; one de-carbon cleaner device is set; described de-carbon cleaner device; by tank body; filler, pipeline, valve; tensimeter constitutes; pipeline links to each other with tank body by the de-carbon valve, is provided with in the bottom of tank body and drenches valve, and the top is provided with outlet valve; bottom and top at tank body are respectively equipped with base pressure table and top pressure table; have filtration and adsorbing filler in the setting of the inside of tank body, the use of this equipment resembles a barrier; not only catalyst protection is played a key effect; improve its work-ing life and active persistence greatly, can reduce the generation of a lot of side reactions simultaneously, play a key effect for improving the morpholine yield.

Description

A kind of device and production technique thereof of protecting morpholine catalyst
Technical field:
The invention belongs to the morpholine production technical field, specially refer to and how to avoid toxic substance to cause poisoning of catalyst, deactivated a kind of device and production technique thereof in a kind of device and the production technique thereof of protecting morpholine catalyst, especially the synthesize morpholine process.
Background technology:
Morpholine claims 1,4 morpholine again, molecular formula C 4H 9NO is colourless oil liquid, has water absorbability, and strong basicity has the ammonia flavor, and energy and immiscible organic solvent are insoluble to strong base solution, and be inflammable, is important organic synthesis reagent.Main as rubber accelerator, the raw material of NOBS, OTOS etc. also has extensive use in industries such as medicine, weaving, paint.
In the reaction of glycol ether catalysis synthesize morpholine, the chemical reaction of a series of complexity takes place, wherein:
Main reaction:
Figure G2009101442516D00011
Side reaction:
Glycol ether cracking chain rupture:
Figure G2009101442516D00012
Facing hydrogen replaces:
Figure G2009101442516D00013
Facing hydrogen replaces:
Figure G2009101442516D00021
Glycol ether chain rupture and morpholine face the hydrogen substitution reaction in, carry out following reaction:
-CH 3+-H→CH 4
-C 2H 5+-H→C 2H 6
From above side reaction, be not difficult to find
1, above side reaction easily generates methane, easily causes catalyst contamination, forms carbon distribution, and carbon granules causes catalyst deactivation with the micropore of circulation gas by the bed blocking catalyst.
2, the extraneous hydrogen that is provided is transformation absorption H 2Gas contains certain sorbent particles, and also easy blocking catalyst micropore causes inactivation when gas passes through bed.
3, the raw material glycol ether and the liquefied ammonia of synthesize morpholine are all squeezed into system by volume pump, can bring a part of machine oil and mechanical impurity in the system unavoidably into, As time goes on, also can make catalyst carbon deposit, inactivation.
At present, in producing morpholine technology, employed morpholine catalyst is to be the Cu-Ni series catalysts of carrier with the aluminum oxide, carrier itself has a lot of micropores, and very easily carbon distribution and obstruction is can't solve because of easily generate methane in the side reaction of synthesize morpholine reaction in existing morpholine production technique, cause catalyst contamination, form carbon distribution, carbon granules by the micropore in the reaction bed blocking catalyst, causes technical problems such as catalyst deactivation with circulation gas.
Summary of the invention:
At the problem of above existence, the present invention discloses a kind of de-carbon cleaner device and technology thereof that is used to protect the morpholine synthetic catalyst, and it can overcome the technical problem that exists at present in the synthesize morpholine production technique.
The present invention is achieved through the following technical solutions:
Before the gas ammonia that fresh hydrogen, circulation gas mixture and heating and gasifying are crossed enters reaction bed, a de-carbon cleaner device is set, described de-carbon cleaner device is by tank body
Figure G2009101442516D00022
Filler
Figure G2009101442516D00023
Pipeline
Figure G2009101442516D00024
Valve
Figure G2009101442516D00025
Tensimeter constitutes, pipeline links to each other with tank body by the de-carbon valve, is provided with in the bottom of tank body and drenches valve, and the top is provided with outlet valve, bottom and top at tank body are respectively equipped with base pressure table and top pressure table, are provided with to have in the inside of tank body and filter and adsorbing filler.
Described have filter and adsorbing filler is in the top and the bottom of tank interior one grillflooring to be set respectively, on grillflooring, be covered with Stainless Steel Cloth, adorn one in grillflooring centre up and down and have high-strength absorption and filtering magnet ring.
Its processing method is: (one) fresh hydrogen and gas mixture are after the circulation pressurization, by pipeline through the carbon dioxide cleaner valve, pass through filler, outlet valve dereaction bed through the top, ammonia after the gasification by pipeline through the carbon dioxide cleaner valve, remove fixed-bed reactor by filler through the top exit valve, finish adsorption filtration gas particles and impurity; (2) when being attracted to, a large amount of various particulates and impurity fills out on the magnet ring, the carbon dioxide cleaner inlet outlet pressure differential increases, illustrate that filler is dirty, the resistance that passes through increases, at this moment just isolate the de-carbon cleaner, allow gas change and walk de-carbon cleaner by-pass, incorporate system again into after de-carbon cleaner release water flowing is cleaned, and so forth.
The use of this equipment resembles a barrier, not only catalyst protection is played a key effect, and improves its work-ing life and active persistence greatly, can reduce the generation of a lot of side reactions simultaneously, plays a key effect for improving the morpholine yield.In addition, this equipment uses and can clean very easily under not parking situation, and is respond well, and the advantage that application highlighted of this equipment has profound significance for the development of morpholine industry.
Description of drawings:
Accompanying drawing is a structural representation of the present invention
In the accompanying drawings, the 1st, carbon dioxide cleaner, the 2nd, Stainless Steel Cloth, the 3rd, fresh hydrogen, circulation gas mixture, the 4th, gas ammonia, the 5th, hot water valve, the 6th, gas ammonia advances the carbon dioxide cleaner valve, the 7th, hydrogen, gas mixture advance the carbon dioxide cleaner valve, and the 8th, hydrogen, gas mixture advance carbon dioxide cleaner by-pass valve, the 9th, carbon dioxide cleaner outlet valve, the 10th, drench valve, the 11st, gas ammonia advances carbon dioxide cleaner by-pass valve, and the 12nd, carbon dioxide cleaner base pressure table, the 13rd, carbon dioxide cleaner base pressure table
Embodiment:
The invention will be further described below in conjunction with accompanying drawing.
As shown in the figure: a kind of de-carbon cleaner device that is used to protect the morpholine synthetic catalyst; in fresh hydrogen; the gas ammonia that circulation gas mixture and heating and gasifying are crossed enters before the reaction bed; one de-carbon cleaner device 1 is set; described de-carbon cleaner device; by tank body 1 and filler 2 and annex pipeline; valve; tensimeter constitutes; pipeline is by de-carbon valve 6; 7 link to each other with tank body 1; be provided with in the bottom of tank body and drench valve 10; the top is provided with outlet valve 9; bottom and top at tank body are respectively equipped with base pressure table 12 and top pressure table 13, are provided with to have in the inside of tank body and filter and adsorbing filler 2.
Described have filter and adsorbing filler is in the top and the bottom of tank interior one grillflooring to be set respectively, on grillflooring, be covered with Stainless Steel Cloth, adorn one in grillflooring centre up and down and have high-strength absorption and filtering magnet ring.
Its processing method is: (one) fresh hydrogen and gas mixture are after the circulation pressurization, by pipeline 3 through carbon dioxide cleaner valve 7, by filler 2, outlet valve 9 dereaction beds through the top, ammonia after the gasification passes through pipeline 4 through carbon dioxide cleaner valve 6, remove fixed-bed reactor by filler 2 through top exit valve 9, finish adsorption filtration gas particles and impurity; (2) when being attracted to, a large amount of various particulates and impurity fills out on the magnet ring, the carbon dioxide cleaner inlet outlet pressure differential increases, illustrate that filler is dirty, the resistance that passes through increases, and at this moment just isolates the de-carbon cleaner, closes the carbon dioxide cleaner valve 7 and the gas ammonia carbon dioxide cleaner valve 6 of hydrogen, gas mixture, open hydrogen, gas mixture carbon dioxide cleaner by-pass valve 8 and gas ammonia de-carbon gas device by-pass Figure 11 simultaneously, allow gas change and walk de-carbon cleaner by-pass, incorporate system again into after de-carbon cleaner release water flowing is cleaned, and so forth.
Example: fresh hydrogen and circulation gas mixture are after the circulation pressurization, by pipeline 3 through de-carbon valve 7, by filler 2, through top exit valve 9 dereaction beds, the ammonia after the gasification is by pipeline 4, remove fixed-bed reactor by filler 2 through outlet valve 9 through de-carbon valve 6, finish adsorption filtration, when the pressure reduction of tensimeter 12 and 13 is higher than 0.1MPa, illustrate that filler 2 has polluted gas particles and impurity, resistance increases, open by-pass valve 8 and 11, close carbon dioxide cleaner valve 6 and 7 and de-carbon gas outlet valve 9, open and drench valve 10 releases, after release finishes, open hot-water valve 5 flushings, after clean, valve-off 5, treat valve 10 anhydrous outflows, valve-off 10 is opened valve 6 and 7 and 9, valve-off 8 and 11, the non-stop run of de-carbon cleaner, and so forth.

Claims (3)

1, a kind of device and production technique thereof of protecting morpholine catalyst is before the gas ammonia that fresh hydrogen, circulation gas mixture and heating and gasifying are crossed enters reaction bed, and a de-carbon cleaner device is set, and described de-carbon cleaner device is by jar Filler
Figure A2009101442510002C2
Pipeline
Figure A2009101442510002C3
Valve
Figure A2009101442510002C4
Tensimeter constitutes, it is characterized in that: pipeline links to each other with tank body by the de-carbon valve, is provided with in the bottom of tank body and drenches valve, and the top is provided with outlet valve, bottom and top at tank body are respectively equipped with base pressure table and top pressure table, are provided with to have in the inside of tank body and filter and adsorbing filler.
2, a kind of device and production technique thereof of protecting morpholine catalyst according to claim 1; it is characterized in that: described have filter and adsorbing filler is in the top and the bottom of tank interior one grillflooring to be set respectively; on grillflooring, be covered with Stainless Steel Cloth, in the middle of grillflooring up and down, adorn one and have high-strength absorption and filtering magnet ring.
3, a kind of device and production technique thereof of protecting morpholine catalyst: its production technique is: (one) fresh hydrogen and gas mixture are after the circulation pressurization, by pipeline through the carbon dioxide cleaner valve, pass through filler, outlet valve dereaction bed through the top, ammonia after the gasification by pipeline through the carbon dioxide cleaner valve, remove fixed-bed reactor by filler through the top exit valve, finish adsorption filtration gas particles and impurity; (2) fill out on the magnet ring when a large amount of various particulates and impurity are attracted to, the carbon dioxide cleaner inlet outlet pressure differential increases, and illustrate that filler is dirty, and at this moment the resistance increase of passing through just isolates the de-carbon cleaner, allows gas change and walks de-carbon cleaner by-pass.
CN2009101442516A 2009-07-25 2009-07-25 Device for protecting morpholine catalyst and production process thereof Active CN101613327B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002019A (en) * 2010-10-18 2011-04-06 吉林化工学院 Method for removing ethylene glycol monomethyl ether impurity in coarse product of morpholine device

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102002019A (en) * 2010-10-18 2011-04-06 吉林化工学院 Method for removing ethylene glycol monomethyl ether impurity in coarse product of morpholine device

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