CN105295021A - Process of continuously producing amine-terminated polyether and reactor design of process - Google Patents
Process of continuously producing amine-terminated polyether and reactor design of process Download PDFInfo
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Abstract
The invention relates to a process of continuously producing amine-terminated polyether and a reactor design of the process, and mainly aims to solve the problems that the production is not continuous, the reaction control is difficult, the operation is complex, the fluctuation of product quality is large, equipment investment is large and the like in the prior art. The invention reaches the aims by adopting the following technical scheme: after being boosted by a pump, polyether and liquid ammonia enter into a reactor from the bottom by passing through an inlet liquid distributor; after being boosted, fresh hydrogen is mixed with recycle hydrogen, and then enter into the reactor from the bottom by passing through an inlet gas distributor; a loaded nickel-based catalyst is loaded on a support grid, and a catalyst lifting internal component is designed on the top of the reactor; a reaction product is discharged from the side surface of the top of the reactor, and enters a high-pressure flash drum; the gas phase of the high-pressure flash drum is the recycle hydrogen, and the liquid phase enters a low-pressure flash drum; the gas phase of the low-pressure flash drum is unreacted ammonia gas which is recycled after compression liquidation, and the liquid phase of the low-pressure flash drum is a polyether amine crude product which enters a separation refined unit, and separation is performed to obtain a polyether amine product. The process and the reactor design thereof, provided by the invention can be applied to the industrial field of producing amine-terminated polyether.
Description
Technical field
The present invention relates to a kind of technique and reactor design thereof of continuous seepage Amino Terminated polyether(ATPE).
Background technology
Amino Terminated polyether(ATPE), has another name called polyetheramine.The amino of Amino Terminated polyether(ATPE) contained by it is positioned at polyethers macromole key end and gains the name.Amino End Group is primary amino especially, containing reactive hydrogen, speed of response is fast, there is the characteristic of some uniquenesses, extensively be used as the main raw material of the cure-crosslinking agent of epoxy resin, reaction injection moulding polyureas and Spray Polyurea Elastomer, simultaneously also by a large scale for fields such as tensio-active agent, ornaments glue, polyester resin, wind electricity blade materials.
The elastomerics synthesized by Amino Terminated polyether(ATPE), as various urethane, polyureas etc., its elastomeric physicals and resistance toheat are much better than other like products, there is excellent stability, weather resistance and ageing resistance, can construct under high-moisture, high humidity environment and use, be widely used in multiple industrial circle, as fields such as anticorrosion, antiseepages.
Owing to lacking the Amino Terminated polyether(ATPE) production technology of high technology content, domestic device adopts interval or semicontinuous production technique substantially, not only product yield is low, production cost is high, and produces instability, quality product fluctuation greatly, cannot compare favourably with external product.
The many Amino Terminated polyether(ATPE) synthetic method of current research mainly contains three kinds: the direct aminatin of (1) polyethers; Polyethers, ammonia, hydrogen directly synthesize Amino Terminated polyether(ATPE) under the effect of catalyzer; (2) polyethers and cyano-containing compound react, and introduce cyano group, then under catalyst action, carry out hydrogenation to cyano group, obtain Amino Terminated polyether(ATPE); (3) leavings group method; Polyethers first reacts with the compound containing leavings group, and generate the polyethers containing leavings group, and then replace leavings group with ammonia, obtain Amino Terminated polyether(ATPE), leaving group compound mainly contains phosgene, methylsulfonyl chloride, phosphorus trihalide etc.Above-mentioned three kinds of methods respectively have relative merits.
The industrial leavings group method that substantially do not adopt produces polyetheramine.Patent CN201210052388.0 discloses a kind of preparation method of polyetheramine, and adopt the amido of tertbutyloxycarbonyl protection alcamine compound, hydroxyl retains; Then highly basic or double metal cyanide-catalyzed under, cause the mixture reaction of oxyethane, propylene oxide, tetrahydrofuran (THF) or three, carry out ring-opening polymerization; In acid condition, remove tertbutyloxycarbonyl, obtain polyetheramine finally.This method synthesis step is many, and intermediate raw material is not easily purchased and easy contaminate environment, and need in building-up process to use a large amount of bronsted lowry acids and bases bronsted lowries to carry out neutralization reaction, product separation is very difficult, and production cannot be carried out at all continuously.
The synthesis technique of the second polyetheramine, reaction conditions is gentleer, if control the transformation efficiency of reaction raw materials, the selectivity etc. of major product well, then product separation difficulty is little.Patent CN201010295482.X discloses a kind of synthetic method of polyetheramine, adopt oxyethane and/or propylene oxide, first synthesizing polyether, and then obtain polyethers nitrile with acrylonitrile reactor, polyethers nitrile is hydrogenation acquisition product polyetheramine under the effect of two luxuriant titanium class Primary Catalystss again.The all processes of this patent are all carried out in reactor, cannot realize continuous seepage, and two metallocene-titanium catalyst costs are high.Document " synthesis of polyetheramine " (Changchun Polytechnic Univ.'s journal, August the 23rd in 2002 volume) to report with potassium hydroxide be catalyzer, the first step vinyl cyanide and glycol ether Reactive Synthesis polyethers nitrile, determine best reaction process condition, and then be catalyzer with Raney's nickel, produce polyetheramine by polyethers hydrogenation of nitriles, and inquire into the optimum process condition of hydrogenation reaction.The first step that this document is determined and second step reaction process condition, all only for rhythmic reaction technique, are not suitable for continuous seepage, and the Raney's nickel catalyst fuel very easily in atmosphere that hydrogenation is used, not only poor stability, and also difficult with product separation, production cost is high.
Industrial first method application is more, but this method often adopts the Discontinuous manufacture mode of batch tank reactor, and under high pressure, reactant reacts several hours or several days in tank reactor, then reactor stopped reaction, pressure release, discharge, last separated product again, obtains product; This kind of mode of production significantly reduces production efficiency, poor stability, production instability, quality product fluctuation greatly.Patent CN201010525067.9 discloses a kind of method adopting amorphous alloy catalyst to prepare polyetheramine, patent CN201010623376.X discloses a kind of preparation method of matrix material polyetheramine, and patent CN200310112615.5 discloses a kind of production method of aliphatics Amino Terminated polyether(ATPE).These patents are all the production technique of interval, pressure autoclave type polyethers direct aminatin.Exploitation had the continuous Amination Technique of polyethers successively afterwards, as patent CN201210056365.5 discloses a kind of continuous production method of amino-terminated polyethers, have employed filling large hole nickel-based catalyst in tubular reactor and reactor.Although this method achieves continuous seepage, the inefficiency of tubular reactor usually, for improving industrial scale, require that reactor is very long, floor space is large, and reaction controlling is difficult, temperature of reaction gradient is large.Patent application CN201410396520.9 discloses the technique that continuous processing produces small-molecular-weight polyetheramine, adopt multiple fixed bed or shell and tube reactor series connection, the catalyzer that inside reactor filling nickel content is above high, the catalyzer that inside reactor filling nickel content is below low.This technique adopts multiple reactors in series, and not only reaction controlling is difficult, and the feed composition of each reactor and state are completely different, and reactor design is difficult to accomplish optimum.In addition, this reaction is under high pressure carried out, and reactor is more, and equipment, pipeline and instrument are more, and operation easier is higher, and equipment safety is poorer, and plant investment is higher.Patent application CN201410396107.2 discloses a kind of production equipment of continuous processing polyetheramine, adopt multiple fixed bed or shell and tube reactor series connection, arrange dewatering unit between two reactors, dewatering unit comprises multiple equipment such as condenser, knockout drum, vaporizer.The equipment of this patent application is more, and plant investment and operation easier are larger, and continuous condensation, evaporation drastically increase the energy consumption of device.These continuous processings produce the technique of polyetheramine, all have that plant efficiency is low, reaction controlling is difficult, complicated operation and a shortcoming such as investment is large, cannot large-scale commercial promote.
Summary of the invention
The present invention relates to a kind of technique and reactor design thereof of continuous seepage Amino Terminated polyether(ATPE), be mainly used in manufacturing side amino-polyether continuously.
The object of the invention is the technique developing a kind of amino-polyether of the manufacturing side serially, technical problem to be solved produces discontinuous, that reaction controlling is difficult, the fluctuation of complicated operation, quality product is large and plant investment is large etc. problem in conventional art, provides a kind of new continuous print Amino Terminated polyether(ATPE) production technique and reactor design thereof.This technique adopts bubbling bed reactor, and polyethers, liquefied ammonia are under the effect of catalyzer and hydrogen, and amination generates polyetheramine, excess ammonia and hydrogen recycle use, whole process implementation continuous prodution; Regulate the loadings of catalyzer or the feed rate of polyethers, reaction process can be controlled simply, constant product quality; Separate unit bubbling bed reactor can realize different production-scale requirement, and equipment, pipeline and instrument are simple, and plant investment is low; Whole technical process is simple, and can realize whole process Automated condtrol easily, operation easier is little.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: enter from reactor bottom through Inlet fluid sparger after polyethers, liquefied ammonia are boosted by pump, and liquefied ammonia (containing circulation liquefied ammonia) is 10-40 with the charge proportion (mol ratio) of polyethers; Fresh hydrogen, after boosting, mixes with recycle hydrogen and enters from reactor bottom through inlet gas sparger, and hydrogen (containing recycle hydrogen) is 0.5-2.5 with the charge proportion (mol ratio) of polyethers; Loading type nickel-based catalyst fills on supportive grid, and reactor head is designed with catalyzer lifting inner member; Reactor is followed successively by Inlet fluid sparger, inlet gas sparger, supportive grid, beds, catalyzer lifting inner member from bottom to top; Reaction product, from the discharging of reactor head side, enters hp flash drum; Hp flash drum gas phase is recycle hydrogen, and liquid phase enters low pressure flash chamber; Low pressure flash chamber gas phase is unreacted ammonia, compresses and liquefies Posterior circle and uses; Low pressure flash chamber liquid phase is the thick product of polyetheramine, enters separation and purification unit, is separated and obtains polyetheramine product.
In technique scheme, raw material polyethers is the aliphatic polyether that two ends have primary hydroxyl functional group, and its molecular weight is 106-4000.
The loadings of loading type nickel-based catalyst and the ratio of polyethers inlet amount are 1.0-10.0 (weight); In loading type nickel-based catalyst, nickel content is 45-75% (weight), and copper content is 5-25% (weight), and Fe content is 1-5% (weight), and all the other are aluminum oxide or silicon oxide.
Top and the side of Inlet fluid sparger have rectangle hole, and total port area is not less than 60% of Inlet fluid sparger surface-area and is not more than the feed-pipe sectional area be connected with Inlet fluid sparger.
Inlet gas sparger is two concentric pipes be communicated with, and the radius of inner pipe is the 1/4-1/2 of reactor radius, and the radius of external circular tube is the 1/2-3/4 of reactor radius; All evenly have two row's apertures bottom two pipes, hole diameter is 10-16 millimeter; Two row's apertures, centered by pipe central shaft, become 60 ° of angles; The aperture total area is the 10-25% of pipe outer surface area.
Catalyzer lifting inner member is the conical funnel shape structure of back-off, conical side surface perforate, and aperture is 10-16 millimeter, and opening area is 1/4-3/4 cone height, and hole area is the 30%-80% of opening area; Inert ceramic balls is all loaded in circular cone inside; Conical top is hollow circular-tube, and pipe volume is more than or equal to circular cone volume; Inverted cone top diameter equals the 1/5-1/3 of reactor diameter, and base diameter equals reactor diameter.
The working pressure of hp flash drum is greater than the liquefied ammonia vapour pressure under hp flash drum service temperature, and the working pressure of low pressure flash chamber is less than the liquefied ammonia vapour pressure under low pressure flash chamber service temperature.
The reaction pressure that reactor adopts is 10-18MPa, and temperature of reaction is 160-260 DEG C.
The present invention adopts bubbling bed reactor, and amination reaction carries out in gas-liquid-solid three-phase, and polyethers, liquefied ammonia are liquid phase, and load-type nickel series catalysts is solid phase, and hydrogen is gas phase.Compared to fixed-bed reactor, shell and tube reactor or tank reactor, reactor of the present invention has obvious advantage: (1) is broken by the bubbling in hydrogen uphill process and bubble, greatly can increase the gas, liquid, solid disturbance of inside reactor, improve heat transfer and the mass transfer of inside reactor, thus improve amination efficiency.(2) reactor head arranges catalyzer lifting inner member, inner filling inert ceramic balls, top reserves porcelain ball lifting space, because catalyzer expands with heat and contract with cold the operation life that the catalyzer extruding that causes is damaged, improve catalyzer during decreasing device shutting down.When reactor initial charge or reactor heat up, beds under the impact of charging or thermal expansion time, entirety upwards loosens, and now inert ceramic balls can enter lifting space, avoids catalyzer and is extruded; Otherwise when reactor stops charging or reactor cooling, beds falls, and now inert ceramic balls drops to original position from lifting space.(3) by regulating the feed rate of raw material polyethers, changing the loadings of catalyzer, the residence time of polyethers in reactor, reaction times and transformation efficiency etc. can be controlled easily.
Catalyst loading of the present invention is on supportive grid, and without the need to carrying out the filtering separation of catalyzer and liquid product, reaction product directly flows out from reactor head side, reduces catalyst consumption, production cost.
The pressure that hp flash drum adopts enables hydrogen flash off, but liquefied ammonia can not gasify, and only reaches the effect of separating hydrogen gas; The pressure that low pressure flash chamber adopts then can make liquefied ammonia all gasify, and reaches the effect being separated unreacted ammonia.Adopt this kind of design, decrease the equipment of separating hydrogen gas, excess ammonia, simplify technical process, reduce production cost.
In sum, present invention achieves the continuous seepage of Amino Terminated polyether(ATPE), and there is simpler technical process and device operation, more efficient reactor design, the more advantage such as stable product quality and lower plant investment, achieve good technique effect.
Accompanying drawing explanation
Figure 1A-Fig. 1 E is process flow diagram of the present invention.
Figure 1A-Fig. 1 E numbers explanation:
1, raw material polyethers; 2, liquefied ammonia; 3, hydrogen; 4, circulating hydrogen; 5, reactor; 6, reaction product; 7, hp flash drum; 8, hp flash drum liquid phase; 9, low pressure flash chamber; 10, hp flash drum gas phase; 11, low pressure flash chamber gas phase; 12, thick polyetheramine; 13, circulation liquefied ammonia; 14, circulating hydrogen compressor; 15, ammonia compressor; 16, refining spearation unit; 17, water and light constituent; 18, polyetheramine product; 19, heavy constituent; 20, Inlet fluid sparger perforate.
A, Inlet fluid sparger; B, inlet gas sparger; C, supportive grid; D, catalyzer; E, catalyzer lifting inner member; H, inverted cone height; D1, rounding vertex of a cone diameter; D2, rounding cone bottom diameter.
After the mixing of raw material polyethers 1, liquefied ammonia 2 and circulation liquefied ammonia 13, enter reactor 5 by Inlet fluid sparger A, hydrogen 3 and circulating hydrogen 4 enter reactor 5 by inlet gas sparger B.Catalyzer D fills on supportive grid C, reaction product 6 is flowed out by the top-side of reactor, enters hp flash drum 7 and carries out gas-liquid separation, and the gas phase 10 of this hp flash drum is hydrogen, after being boosted by circulating hydrogen compressor 14, use as circulating hydrogen 4.Hp flash drum liquid phase 8 enters low pressure flash chamber 9 and carries out gas-liquid separation, and this low pressure flash chamber gas phase 11 is ammonia, to be boosted post liquefaction, use as circulation liquefied ammonia 13 by ammonia compressor 15.Low pressure flash chamber liquid phase 12 is thick polyetheramine product, enters refining spearation unit 16 and carries out refining spearation, obtains polyetheramine product 18, isolates water byproduct and a small amount of light constituent 17, a small amount of heavy constituent 19 simultaneously.
Below by embodiment, the invention will be further elaborated.
Embodiment
[embodiment 1]
Shown in Fig. 1, the molecular weight of raw material polyethers is 230, and liquefied ammonia (containing circulation liquefied ammonia) is 20 with the charge proportion (mol ratio) of polyethers, and hydrogen (containing recycle hydrogen) is 2.0 with the charge proportion (mol ratio) of polyethers; Loaded catalyst is 3.0 with the ratio (weight) of polyethers inlet amount, and Nickel Content In Catalyst is 75% (weight), and ketone content is 5% (weight), and Fe content is 1.5% (weight), and all the other are aluminum oxide; The total port area of Inlet fluid sparger is 68% of its surface-area, the inside pipe radius of inlet gas sparger is 1/2 of reactor radius, external circular tube radius is 3/4 of reactor radius, and pipe hole diameter is 12 millimeters, and the aperture total area is 15% of pipe outer surface area; The conical side surface small aperture of catalyzer lifting inner member is 12 millimeters, and hole area is 80% of opening area, and inverted cone top diameter equals 1/4 of reactor diameter; The reaction pressure that reactor adopts is 11.5MPa, and temperature of reaction is 180 DEG C.
Experimental result is in table 1.
[embodiment 2]
Adopt the scheme of embodiment 1, only feed change polyethers.
Experimental result is in table 1.
[embodiment 3]
Adopt the scheme of embodiment 1, only change the charge proportion of liquefied ammonia, hydrogen and polyethers.
Experimental result is in table 1.
[embodiment 4]
Adopt the scheme of embodiment 1, only change the composition of loaded catalyst and catalyzer.
Experimental result is in table 1.
[embodiment 5]
Adopt the scheme of embodiment 1, only change the perforated area of Inlet fluid sparger and the perforated area of inlet gas sparger.
[embodiment 6]
Adopt the scheme of embodiment 1, only change the conical side surface perforated area of catalyzer lifting inner member.
[embodiment 7]
Adopt the scheme of embodiment 1, only the reaction pressure of altering reactor and temperature of reaction.
Experimental result is in table 1.
Table 1 the results show, adopt the inventive method can realize the continuous seepage of polyetheramine, and the yield of polyetheramine is more than 90%, is better than existing domestic production technology.
Table 1 experimental result
Claims (8)
1. the technique of a continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof, be mainly used in continuous seepage Amino Terminated polyether(ATPE), by achieving the goal by the following technical solutions: enter from reactor bottom through Inlet fluid sparger after polyethers, liquefied ammonia are boosted by pump, liquefied ammonia (containing circulation liquefied ammonia) is 10-40 with the charge proportion (mol ratio) of polyethers; Fresh hydrogen, after boosting, mixes with recycle hydrogen and enters from reactor bottom through inlet gas sparger, and hydrogen (containing recycle hydrogen) is 0.5-2.5 with the charge proportion (mol ratio) of polyethers; Loading type nickel-based catalyst fills on supportive grid, and reactor head is designed with catalyzer lifting inner member; Reactor is followed successively by Inlet fluid sparger, inlet gas sparger, supportive grid, beds, catalyzer lifting inner member from bottom to top; Reaction product, from the discharging of reactor head side, enters hp flash drum; Hp flash drum gas phase is recycle hydrogen, and liquid phase enters low pressure flash chamber; Low pressure flash chamber gas phase is unreacted ammonia, and compress and liquefy Posterior circle and use, low pressure flash chamber liquid phase is the thick product of polyetheramine, enters separation and purification unit, is separated and obtains polyetheramine product.
2. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that raw material polyethers is the aliphatic polyether that two ends have primary hydroxyl functional group, its molecular weight is 106-4000.
3. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, is characterized in that the loadings of loading type nickel-based catalyst and the ratio of polyethers inlet amount are 1.0-10.0 (weight); The nickel content of loading type nickel-based catalyst is 45-75% (weight), and copper content is 5-25% (weight), and Fe content is 1-5% (weight), and all the other are aluminum oxide or silicon oxide.
4. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that top and the side of Inlet fluid sparger have rectangle hole, total port area is not less than 60% of Inlet fluid sparger surface-area and is not more than the feed-pipe sectional area be connected with Inlet fluid sparger.
5. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that inlet gas sparger is two concentric pipes be communicated with, the radius of inner pipe is the 1/4-1/2 of reactor radius, and the radius of external circular tube is the 1/2-3/4 of reactor radius; All evenly have two row's apertures bottom two pipes, hole diameter is 10-16 millimeter; Two row's apertures, centered by pipe central shaft, become 60 ° of angles; The aperture total area is the 10-25% of pipe outer surface area.
6. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that catalyzer lifting inner member is the conical funnel shape structure of back-off, conical side surface perforate, aperture is 10-16 millimeter, opening area is 1/4-3/4 cone height, and hole area is the 30%-80% of opening area; Inert ceramic balls is all loaded in circular cone inside; Conical top is hollow circular-tube, and pipe volume is more than or equal to circular cone volume; Inverted cone top diameter equals the 1/5-1/3 of reactor diameter, and base diameter equals reactor diameter.
7. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that the working pressure of hp flash drum be greater than hp flash drum service temperature under liquefied ammonia vapour pressure, the working pressure of low pressure flash chamber is less than the liquefied ammonia vapour pressure under low pressure flash chamber service temperature.
8. the technique of continuous seepage Amino Terminated polyether(ATPE) and reactor design thereof according to claim 1, it is characterized in that the reaction pressure that reactor adopts is 10-18MPa, temperature of reaction is 160-260 DEG C.
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Application publication date: 20160203 |