CN205556526U - Device of serialization preparation polyetheramine - Google Patents
Device of serialization preparation polyetheramine Download PDFInfo
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- CN205556526U CN205556526U CN201620337316.4U CN201620337316U CN205556526U CN 205556526 U CN205556526 U CN 205556526U CN 201620337316 U CN201620337316 U CN 201620337316U CN 205556526 U CN205556526 U CN 205556526U
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
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Abstract
The utility model provides a device of serialization preparation polyetheramine, relates to polyether glycol's hydrogenation ammonia (amine) and changes technical field. Fluidized bed reactor inside sets up the atomizer, the catalyst bears device, ammonia, the mixed air distributor of hydrogen and liquid distributor, fluidized bed reactor manage to say and to meet vapour and liquid separator, and ammonia, hydrogen mixed export that the vapour and liquid separator upper end set up manage and say and connect the recycle compressor, otherly on the pipeline connects fresh hydrogen to mend the entry to mend with fresh ammonia and enter the mouth, and the exit linkage of recycle compressor is at ammonia, the mixed air distributor's of hydrogen entrance point, vapour and liquid separator's lower extreme passes through the water recovery mouth to be connected with the water collection tank, and the circulating pump passes through the pipeline to be connected with the liquid distributor exit end, circulating pump export through tee bend and ooff valve go into respectively the catalyst bear the device above and the product collection tank. The utility model discloses increased the contact of catalyst with the material, the side reaction is few, and equipment is simple, and the reaction rate is fast, have higher ammoniation rate, high primary amine selectivity, zero pollutes.
Description
Technical field
The utility model relates to the hydrogenation ammonia (amine) of PPG and changes technical field.
Background technology
Polyetheramine (PEA): be a class main chain be polyether structure, end active functional group is the polymer of amido.Polyetheramine is to be reaction raw materials by PPG, and ammonification obtains at high temperature under high pressure.By a series of performances such as the polyoxyalkyl structure that selection is different, the reactivity of adjustable polyetheramine, toughness, viscosity and hydrophilies, and amido is supplied to the possibility that polyetheramine reacts with multiple compounds.
PPG containing terminal hydroxy group is carried out faces hydrogen ammonia (amine) and changes reaction, can prepare a series of aminated compounds, this compounds can be widely used for the fields such as epoxy curing agent, wind power blade curing agent, polyurethane polyureas urea elastomers, gasoline cleaning agent, water base coating, textile finish and epoxy toughening.
Patent CN104693434A discloses the production method of a kind of fixed bed continuity method synthesizing polyether amine, uses fixed bed reactors to realize continuous prodution polyetheramine；Patent CN104117333A discloses the process units of a kind of continuity method polyetheramine, uses the mode of multiple reactor series connection to realize continuous prodution polyetheramine；Patent CN103524725A discloses the devices and methods therefor of a kind of fixed bed continuous synthesis amine terminated polyether, its technique using successive reaction, react under conditions of 1～3 fixed bed, 150 DEG C～300 DEG C, 1～20MPa, ammonia-alcohol ratio 1～15, recycle excess of ammonia and hydrogen.Patent CN104119239A discloses a kind of continuity method and produces the technique of small-molecular-weight polyetheramine, uses the form of continuity method fixed bed, uses the form of 2～6 reactor series connection, and improves the conversion ratio of reaction in each reactor equipped with different catalyst.Patent CN101522607 discloses the preparation method of a kind of polyetheramine, containing under the metallic framework Raney nickel effects such as cobalt, aluminium, copper, carries out continuous reaction in fixed-bed tube reactor.
Patent CN 102408559A discloses the preparation technology of a kind of amine terminated polyether, the method is with PPG that number-average molecular weight is more than 100 as raw material, in the presence of hydrogen, aminating agent and skeletal nickel catalyst, in autoclave, prepare polyetheramine by catalysis reduction amination；Patent CN102336903A discloses production method and the preparation of special-purpose catalyst thereof of a kind of aliphatic poly ether amines, its catalyst is frame special Raney nickel, and the method uses in autoclave is faced hydrogen ammonification synthesizing polyether amine by PPG under frame special Raney nickel.
Method made above uses the batch process of reaction under high pressure autoclave and produces or serialization fixed-bed approach.And batch tank method product all exists quality instability, side reaction is many, is difficult to realize the shortcomings such as Automated condtrol；Serialization fixed-bed approach by contrast relatively batch tank method constant product quality, side reaction, it easily is automated control, but above-mentioned continuity method uses fixed bed type reactor, have that equipment is complicated, catalyst change is difficult, produce the shortcoming that kind is single.
Utility model content
Utility model purpose is to provide a kind of energy amination rate height, primary amine selectivity is good, technique is simple, catalyst is easily changed, the device of the continuously preparing poly ether amines of same set of device changeable production multi items.
Technical solutions of the utility model are: arrange atomizer in fluidized-bed reactor inner upper, set catalyst carrier arrangement at the middle part of fluidized-bed reactor, in the fluidized-bed reactor below catalyst carrier arrangement, be respectively provided with ammonia, hydrogen mixed gas distributor and liquid distribution trough；Gas-liquid separator is connected by the first pipeline on the upper top of fluidized-bed reactor, the upper end of gas-liquid separator arranges ammonia, hydrogen mixed export, this ammonia, hydrogen mixed export are connected to the entrance of a recycle compressor again by second pipe, on second pipe, the also other fresh hydrogen that connects fills into mouth and fresh ammonia fills into mouth, and the outlet of recycle compressor is connected to ammonia, the entrance point of hydrogen mixed gas distributor；The lower end of gas-liquid separator arranges Water Sproading mouth, and is connected with water collecting tank by the 3rd pipeline；Circulating pump is set outside fluidized-bed reactor, the import of circulating pump is connected to the port of export of liquid distribution trough by the 4th pipeline, circulation delivery side of pump connects one end of two switch valves respectively by threeway, the other end of one switch valve by the catalyst carrier arrangement in the 5th pipeline incoming stream fluidized bed reactor above, the other end of another switch valve is practiced midwifery product collecting tank by the 6th pipeline.
PPG through preheating is sprayed on skeletal nickel catalyst continuously through atomizer and carries out facing hydrogen aminating reaction.Fluidized-bed reactor upper end outlet passes through gas-liquid separator separates water outlet, and isolated ammonia, hydrogen mixed gas are entered fluidized-bed reactor by ammonia, hydrogen mixed gas distributor after compressor and fresh ammonia, hydrogen adjust mixing ratio；Liquid distribution trough collects the reactant mixture of fluidized-bed reactor, and through the upper end of circulating pump reflux again to skeletal nickel catalyst, the polyetheramine of acquirement is in circulating pump is collected in product collecting tank.
Compared with prior art, use the utility model that the catalyst in fluidized-bed reactor can be made to be in dynamically, add contacting of catalyst and material；Reaction temperature is steady；Pressure and temperature that reaction needs are low, and side reaction is few, and equipment is simple, and reaction speed is fast；There is higher ammonification rate, high primary amine selectivity, reaction conversion ratio >=99.0%, primary amine selectivity >=99.0%；Catalyst is more easy to change, diversification of varieties；Gaseous ammonia and the hydrogen of the excess in course of reaction recycle, and environment realizes no pollution to external world.
It addition, the utility model also can concatenate Water Sproading valve on the 3rd pipeline between gas-liquid separator and water collecting tank.After being separated to a number of moisture in gas-liquid separator, by the unlatching of Water Sproading valve, can make moisture collection in water collecting tank.When closing Water Sproading valve, the operating efficiency of gas-liquid separator can be improved.
Accompanying drawing explanation
Fig. 1 is a kind of structural representation of the present utility model.
Detailed description of the invention
One, preparation is set:
As it is shown in figure 1, arrange atomizer 1-1 in fluidized-bed reactor 1 inner upper, for providing uniform temperature and the PPG of pressure in fluidized-bed reactor 1.Catalyst carrier arrangement 1-1 is set, for providing the skeletal nickel catalyst needed for reaction at the middle part of fluidized-bed reactor 1.Ammonia, hydrogen mixed gas distributor 9 and liquid distribution trough 8 it is respectively provided with in fluidized-bed reactor 1 below catalyst carrier arrangement 1-1.
Gas-liquid separator 2 is connected by the first pipeline 10 on the upper top of fluidized-bed reactor 1, the upper end of gas-liquid separator 2 arranges ammonia, hydrogen mixed export, this ammonia, hydrogen mixed export are connected to the entrance of a recycle compressor 3 again by second pipe 11, on second pipe 11, the also other fresh hydrogen that connects fills into mouth 12 and fresh ammonia fills into mouth 13, and the outlet of recycle compressor 3 is connected to ammonia, the entrance point of hydrogen mixed gas distributor 9.The lower end of gas-liquid separator 2 arranges Water Sproading mouth, and is connected with water collecting tank 5 by the Water Sproading valve 15 of the 3rd pipeline 14 and series connection.
Circulating pump 4 is set outside fluidized-bed reactor 1, the import of circulating pump 4 is connected to the port of export of liquid distribution trough 8 by the 4th pipeline 16, the outlet of circulating pump 4 connects one end of two switch valves 17,18 respectively by threeway, the other end of switch valve 17 by the catalyst carrier arrangement 1-1 in the 5th pipeline 19 incoming stream fluidized bed reactor 1 above, the other end of switch valve 18 is practiced midwifery product collecting tank 6 by the 6th pipeline 20.
Two, example is produced:
Polypropylene glycol ether atomizer 7 through fluidized-bed reactor 1 top after preheater is warming up to 130 DEG C in advance is continuously entered in fluidized-bed reactor 1, hydrogen and ammonia from bottom ammonia, being passed through fluidized-bed reactor 1 of hydrogen mixed gas distributor 9, face hydrogen aminating reaction by recycle compressor 3 under the conditions of temperature is 130 DEG C and pressure is 6MPa.
Fluidized-bed reactor 1 top reactant separates water outlet and ammonia, hydrogen through gas-liquid separator 2, and the ammonia of separation, hydrogen mixed gas, through compressor 3 and fresh hydrogen, the regulation mixing of ammonia gaseous mixture, are again introduced in fluidized-bed reactor 1.Bottom unreacted fluidized-bed reactor 1 completely, reactant is recycled to fluidized-bed reactor 1 continuation reaction by circulating pump 4, reacts product completely and, then by opening switch valve 18 continuous discharge, obtains polyetheramine product in product collecting tank 6.
Claims (2)
1. the device of a continuously preparing poly ether amines, it is characterized in that including fluidized-bed reactor, in fluidized-bed reactor inner upper, atomizer is set, set catalyst carrier arrangement at the middle part of fluidized-bed reactor, in the fluidized-bed reactor below catalyst carrier arrangement, be respectively provided with ammonia, hydrogen mixed gas distributor and liquid distribution trough；Gas-liquid separator is connected by the first pipeline on the upper top of fluidized-bed reactor, the upper end of gas-liquid separator arranges ammonia, hydrogen mixed export, this ammonia, hydrogen mixed export are connected to the entrance of a recycle compressor again by second pipe, on second pipe, the also other fresh hydrogen that connects fills into mouth and fresh ammonia fills into mouth, and the outlet of recycle compressor is connected to ammonia, the entrance point of hydrogen mixed gas distributor；The lower end of gas-liquid separator arranges Water Sproading mouth, and is connected with water collecting tank by the 3rd pipeline；Circulating pump is set outside fluidized-bed reactor, the import of circulating pump is connected to the port of export of liquid distribution trough by the 4th pipeline, circulation delivery side of pump connects one end of two switch valves respectively by threeway, the other end of one switch valve by the catalyst carrier arrangement in the 5th pipeline incoming stream fluidized bed reactor above, the other end of another switch valve is practiced midwifery product collecting tank by the 6th pipeline.
The device of continuously preparing poly ether amines the most according to claim 1, it is characterised in that concatenate Water Sproading valve on the 3rd pipeline between gas-liquid separator and water collecting tank.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620337316.4U CN205556526U (en) | 2016-04-21 | 2016-04-21 | Device of serialization preparation polyetheramine |
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| CN201620337316.4U CN205556526U (en) | 2016-04-21 | 2016-04-21 | Device of serialization preparation polyetheramine |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727580A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of vulcanization bed reaction technique preparing amine terminated polyether |
| CN113603880A (en) * | 2021-09-10 | 2021-11-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
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2016
- 2016-04-21 CN CN201620337316.4U patent/CN205556526U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727580A (en) * | 2017-04-21 | 2018-11-02 | 中国石油化工股份有限公司 | A kind of vulcanization bed reaction technique preparing amine terminated polyether |
| CN108727580B (en) * | 2017-04-21 | 2021-04-06 | 中国石油化工股份有限公司 | Fluidized bed reaction process for preparing amino-terminated polyether |
| CN113603880A (en) * | 2021-09-10 | 2021-11-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
| CN113603880B (en) * | 2021-09-10 | 2022-08-05 | 扬州晨化新材料股份有限公司 | System and method for continuously producing low molecular weight polyether amine |
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