WO2012088671A1 - 一种快速混合反应器及其应用 - Google Patents
一种快速混合反应器及其应用 Download PDFInfo
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- WO2012088671A1 WO2012088671A1 PCT/CN2010/080434 CN2010080434W WO2012088671A1 WO 2012088671 A1 WO2012088671 A1 WO 2012088671A1 CN 2010080434 W CN2010080434 W CN 2010080434W WO 2012088671 A1 WO2012088671 A1 WO 2012088671A1
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- reactor
- feed
- distributor
- disposed
- hollow impeller
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/27—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices
- B01F27/272—Mixers with stator-rotor systems, e.g. with intermeshing teeth or cylinders or having orifices with means for moving the materials to be mixed axially between the surfaces of the rotor and the stator, e.g. the stator rotor system formed by conical or cylindrical surfaces
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/62—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis comprising liquid feeding, e.g. spraying means
- B01F27/621—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis comprising liquid feeding, e.g. spraying means the liquid being fed through the shaft of the stirrer
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/625—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis the receptacle being divided into compartments, e.g. with porous divisions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/78—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton from carbonyl compounds, e.g. from formaldehyde, and amines having amino groups bound to carbon atoms of six-membered aromatic rings, with formation of methylene-diarylamines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
- C07C263/10—Preparation of derivatives of isocyanic acid by reaction of amines with carbonyl halides, e.g. with phosgene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/06—Amines
- C08G12/08—Amines aromatic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00189—Controlling or regulating processes controlling the stirring velocity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00245—Avoiding undesirable reactions or side-effects
- B01J2219/00247—Fouling of the reactor or the process equipment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00761—Details of the reactor
- B01J2219/00763—Baffles
- B01J2219/00765—Baffles attached to the reactor wall
Definitions
- the present invention relates to a rapid mixing reactor, and more particularly to a dynamic reactor for achieving rapid mixing and rapid reaction between fluids under a large-scale production capacity. Meanwhile, the present invention also provides a process for producing an isocyanate by phosgenation using the reactor, and a process for producing a polymethylene polyphenylpolyamine by using the reactor through aniline and formaldehyde. Background technique
- reaction products or intermediates may be directly related to a component of the raw materials. Therefore, the initial mixing effect between the materials will greatly affect the final product distribution, the yield and quality of the target product, and at the same time affect the design and energy consumption of the entire production process.
- the reaction process mainly includes a phosgene gasification stage and a thermo-optic gasification stage.
- the liquid polyamine and the liquid phosgene are separately dissolved in an inert solvent such as chlorobenzene, dichlorobenzene, toluene, chlorinated naphthalene, 1,2,4-trichlorobenzene, etc. They are reacted at a low temperature of 0 to 9 (TC).
- TC 0 to 9
- This process is a complex multi-step tandem competitive response.
- the main reaction is an instantaneous reaction, and the time scale of the reaction is on the order of milliseconds or less; the resulting product further reacts rapidly with the raw material to form a by-product which is insoluble in the system. Therefore, the initial mixing effect of the two raw materials will directly affect the yield and selectivity of the main product.
- Successfully designing a fast liquid mixing reactor to increase the initial mixing effect of the two feed streams is of great significance for increasing the yield and selectivity of the main product and reducing the formation of by-product viscous materials.
- the reaction process mainly includes a salt formation reaction stage, a precondensation reaction stage, and an index reaction stage.
- the precondensation reaction stage the mixture of aniline hydrochloride and circulating liquid is rapidly mixed with formaldehyde at a pre-condensation reaction at 20-90 ° C.
- Cross-flow mixing is an important method to achieve rapid mixing between fluids.
- One way is that one fluid is injected into another fluid through several small holes, which is divided into many small pieces due to the passage of fluid through the small holes.
- the stream is injected into the main stream, and each fluid is rapidly surrounded by the main stream after injection, thereby achieving rapid mixing between the two streams.
- a pore jet injection reactor (Fig. 1) is disclosed in U.S. Patent No. 5,117,048, which is a cross-flow type of a small hole in which a fluid (polyamine) is distributed through a reduced diameter. Jet into the main fluid (phosgene) to achieve rapid mixing of the two fluids.
- the reactor is mainly designed to reduce the degree of turbulence of the two materials by reducing the diameter of the material, thereby enhancing the initial mixing effect between the materials.
- the jet reactor reduces the amount of solvent used to dilute the reactants.
- the object of the present invention is to provide a novel rapid mixing reactor for achieving rapid mixing between two materials under a large production capacity, strengthening the main reaction, suppressing side reactions, and improving the yield and quality of the target product.
- the reactor provided by the present invention is based on the following design concept: the first fluid is introduced through the flow passage, and the second fluid is uniformly injected into the first fluid through the rotating impeller inlet. Since the second fluid is added to the first fluid through the rotating impeller, the two materials are uniformly hooked at the first time and no further mixing space is required.
- the rotating feed port also acts as a stirrer, thus achieving the purpose of quickly mixing the two materials without mixing space.
- the material inlet can be arranged relative to the other stream, so it is not limited by the flow space, without any amplification effect, and can be realized under large-scale production capacity. Rapid mixing between fluids, rapid response.
- the basic structure of the rapid mixing reactor provided by the present invention is as follows:
- a rapid mixing reactor comprising the following components: a first feed channel housing, a reactor housing, a second feed channel, a hollow impeller material distributor, a rotating shaft, a first feed distributor;
- the first feed channel housing and the reactor housing are coaxially disposed, and are disposed in the first a first feed distributor at the end of the feed passage housing is in communication with a reaction space in the reactor housing;
- the second feed passage, the hollow impeller material distributor and the rotating shaft are disposed along a central axis of the reactor,
- the hollow impeller material distributor is located in the reactor housing and is rotatable within the reactor housing by the rotating shaft, and the second feed passage is in communication with the material passage in the hollow impeller material distributor;
- At least one first feed port is disposed on a feed passage housing;
- at least one reaction liquid outlet is disposed at an end of the reactor housing; and
- a first feed distributor and a hollow impeller material distributor are respectively disposed The first feed injection port and the second feed injection port.
- the second feed passage, the hollow impeller material distributor and the rotating shaft are sequentially fixedly coupled along the central axis of the rapid mixing reactor.
- a dynamic seal ring and a static seal ring capable of being attached to each other are disposed at a joint of the hollow impeller material distributor and the second feed passage, and the dynamic seal ring is disposed on the hollow impeller material distributor, and the The static sealing ring is disposed at the end of the second feeding passage, one side of the static sealing ring is attached to the dynamic sealing ring on the hollow impeller material distributor, and the other side is passed through the expansion joint and the magazine from the inside to the outside.
- Fixed on the first feed distributor With this design, the dynamic seal ring and the static seal ring can be closely fitted when the hollow impeller material distributor rotates.
- the second feeding passage is disposed inside the rotating shaft and is fixedly connected and communicated with the hollow impeller material distributor, so that the hollow impeller material distributor is The rotating shaft is rotated in the reactor housing.
- the second feed injection port is disposed on the side of the hollow impeller material distributor, or disposed on the outermost edge of the hollow impeller material distributor, or disposed on the A channel drawn from the hollow impeller material distributor perpendicular to the impeller disk.
- the present invention has no special requirements on the shape, size and number of the second feed injection port on the hollow impeller material distributor, as long as the process requirements can be met, for example, the shape of the injection port (referring to the injection port)
- the shape of the cross section of the internal passage may be selected from any one or more of a circle, a triangle, a diamond, a trapezoid, a polygon, an ellipse, a square, a rectangle, etc., preferably a circle or a rectangle.
- the specific size and number of the injection ports can be calculated by a person skilled in the art by a conventional process in accordance with specific process requirements.
- the first feed distributor is provided with a first feed injection port, and preferably, the first feed injection port may be an annular gap or a uniform hook distribution. Multiple openings.
- the annular gap-shaped first feed injection port is the same and/or different from a plurality of inner diameters disposed at the same center of the first feed distributor An arc-shaped slit; wherein a plurality of arc-shaped slits having the same inner diameter are spaced apart from each other, and the circle in which they are located is the same as the center of the first feed distributor.
- circles of different inner diameters formed by arcuate slits having different inner diameters are also preferably disposed at the same center as the first feed distributor.
- the shape of the opening may be selected from the group consisting of a circle, a triangle, a diamond, a trapezoid, a polygon, an ellipse, a square, and a rectangle. Any one or more of them are preferably circular.
- the present invention has no special requirements for the specific size and quantity of the first feed injection port, and can be determined by a person skilled in the art according to specific process requirements by conventional process calculation.
- an annular inwardly projecting reaction channel adjusting block is disposed on the inner wall of the reactor casing downstream of the hollow impeller material distributor for To a lesser extent, the flow path of the reactants is reduced.
- the flow rate of the reaction liquid can be between 10 m/s and 500 m/s, preferably 30 m/s to 300 m/s.
- the reaction channel adjusting block can be separately formed and fixed on the inner wall of the reactor casing, or can be integrally formed with the reactor casing.
- At least one primary stirring blade is vertically disposed on the rotating shaft, and the stirring blade includes at least two stirring blades to enhance the downstream of the hollow impeller material distributor.
- Instantaneous rapid mixing of the reactant stream further preferably, one to three stages of agitating blades are vertically disposed on the rotating shaft, and each stage of the agitating blades comprises 2 to 20 pieces of agitating blades; and further preferably, the rotating shaft is vertically disposed one level
- the paddle is agitated, and the agitating paddle and the reaction channel adjusting block are disposed on the same section perpendicular to the central axis of the reactor.
- the reactor of the present invention further comprises a rotating motor coupling disposed at the end of the reactor to facilitate the relative fixation of the reactor to the rotating motor.
- the rapid mixing reactor provided by the present invention, there is no special requirement for the material of the reactor, and any material commonly used in the art can be used, including but not limited to steel, glass, ceramics, alloys, silicon carbide or enamelled steel.
- the present invention also provides an amine having the general formula (I) using the above-described rapid mixing reactor Process for the preparation of an aliphatic, alicyclic or aromatic isocyanate of the formula (II), R(NH 2 ) n (I)
- the phosgene solution is a phosgene solution having a concentration of 30-100% by weight formed by dissolving pure phosgene or phosgene in an inert organic solvent;
- the organic solution of the amine is The amine represented by the formula (I) is dissolved in an inert organic solvent to form an amine solution having a concentration of 10 to 60% by weight, preferably 20 to 50% by weight.
- the amine represented by the formula (I) may be selected from any one of the following compounds: toluenediamine, 4, 4'-diaminodiphenylmethane, multi-Asia Methyl polyphenyl polyamine, isophorone diamine, hexamethylene diamine, cyclohexane diamine, naphthalene diamine, p-phenylenediamine, benzene dimethylene diamine, cyclohexane dimethylene diamine And trimethyl-1,6-hexamethylenediamine, tetramethylm-xylylenediamine, dimethylbiphenyldiamine and methylcyclohexyldiamine, preferably toluenediamine.
- the inert organic solvent for dissolving phosgene and the amine may be the same or different, and the inert organic solvent is respectively selected from the group consisting of: benzene, toluene, chlorobenzene, o-dichlorobenzene, and Dichlorobenzene, monochlorobiphenyl, dialkyl terephthalate or o-benzene One or more of diethyl formate.
- the present invention provides a method for preparing a polymethylene polyphenyl polyamine (referred to as a polyamine) from aniline using the above-described rapid mixing reactor, the method comprising the steps of:
- a raw material is evenly distributed into the other stream through a rotating distribution channel to achieve rapid mixing of the two streams;
- the reactor can theoretically be infinitely enlarged, which can realize rapid instantaneous mixing between two fluids under large-scale production capacity, and overcome the mixing distance caused by the increase of the flow channel space in the conventional reactor during the amplification process. And the disadvantage of correspondingly increasing the mixing time;
- the mixing is fast and uniform, and the side reaction is minimized, and the amount of solvent and the excess of phosgene in the reactant feed are reduced in the process of phosgenation to prepare isocyanate.
- This increases the capacity of the unit, improves product quality and reduces energy consumption.
- the reactor provided by the present invention is used for preparing polymethylene polyphenylpolyamine from aniline and formaldehyde, the precondensation reaction temperature can be improved, the product quality can be improved, and the apparatus can be stably operated for a long period of time.
- Figure 1 is a schematic view showing the structure of a pore jet type jet reactor disclosed in US 5, 117, 048;
- Figure 1 is a schematic view showing the structure of a reactor disclosed in US 5, 931, 579;
- Figure 3 is a schematic view showing the structure of a preferred embodiment of the reactor provided by the present invention
- Figure 4 is a schematic view showing the structure of another preferred embodiment of the reactor provided by the present invention
- Figures 5a - 5c are described in the present invention. Schematic diagram of the arrangement of the feed injection port on the hollow impeller material distributor;
- 6a-6c are schematic views showing the arrangement of the feed injection ports on the first feed distributor of the present invention. detailed description
- the rapid mixing reactor mainly comprises the following components: a first feed channel housing 1, a reactor housing 4, a second feed passage 17, a hollow impeller material distributor 6, and a rotation.
- Axis 1 0, first feed distributor 3.
- the first feed channel housing and the reactor housing are disposed coaxially and in communication with a reaction space within the reactor housing through a first feed distributor disposed at an end of the first feed channel housing.
- the second feed channel, the hollow impeller material distributor and the rotating shaft are sequentially fixedly connected along a central axis of the rapid mixing reactor.
- the hollow impeller material distributor is disposed in the reactor housing and is axially rotatable within the reactor housing by the rotating shaft.
- the second feed passage is in communication with the material passage 12 in the hollow impeller material distributor.
- the first feed channel housing is provided with at least one first feed port 2, and the space enclosed by the first feed channel housing 1 and the first feed distributor 3 is a first feed channel 18. At least one reaction liquid outlet 8 is provided at the end of the reactor housing.
- a plurality of first feed injection ports 13 are uniformly disposed on the first feed distributor 3, and the hollow impeller material distributor 6 is provided with a plurality of passages perpendicular to the impeller discs, and the passages are perpendicular to the impeller discs.
- Figure 5c is a partial enlarged view of the passage perpendicular to the impeller disk, the opening of which is slightly different from that shown in Figure 3.
- the hollow impeller described in the present invention The material distributor may also provide a second feed injection port in accordance with Figures 5a, 5b or other possible means.
- a dynamic seal ring 14 and a static seal ring 19 which are capable of abutting each other are provided at the junction of the hollow impeller material distributor 6 and the second feed passage 17.
- the dynamic seal ring 14 is disposed on the hollow impeller material distributor, and the static seal ring 19 is disposed at the end of the second feed passage, one side of the static seal ring 19 and the hollow impeller material distributor
- the movable seal ring 14 is fitted, and the other side thereof is fixed to the first feed distributor 3 by the expansion joint 16 and the spring 15 from the inside to the outside.
- an annular inwardly projecting reaction channel adjusting block 7 is disposed on the inner wall of the reactor casing downstream of the hollow impeller material distributor for narrowing the reactants to some extent.
- An agitating paddle 11 is vertically disposed on the rotating shaft 10, and the agitating paddle 1 and the reaction channel adjusting block 7 are disposed on the same section perpendicular to the central axis of the reactor.
- the reactor of the present invention further comprises a rotating motor coupling 9 disposed at the end of the reactor housing to facilitate relative fixation of the reactor to the rotating electrical machine.
- the first feed injection port provided on the first feed distributor may be an annular gap or a plurality of openings uniformly distributed, as long as the first feed can be uniformly ensured. It is sufficient to enter the downstream reaction zone through the injection port.
- the phosgene solution first enters through the first feed port 1 and fills the first feed channel 18, and then uniformly sets a plurality of first through the first feed distributor 3.
- a feed injection port 13 enters the reactor housing.
- the organic solution of the amine of formula (I) is introduced by the second feed channel , through the material channel 12 in the rotating hollow impeller material distributor 16 and through a plurality of second feed ports. 5
- the polyamine solution is uniformly sprayed into the phosgene solution stream to achieve rapid mixing and rapid reaction.
- the mixed material continues to move downstream under the action of the feed pressure, and is agitated by the stirring blade 1 1 perpendicular to the rotating shaft, and then passed through the reaction liquid outlet 8 to the next-stage reactor, and the final isocyanate is obtained by raising the temperature.
- FIG. 4 is a schematic view showing the structure of another preferred embodiment of the reactor provided by the present invention, As can be seen from the figure, the reactor mainly comprises the following components: a first feed channel housing 21, a reactor housing 24, a second feed channel 34, a hollow impeller material distributor 26, a rotating shaft 30, a A feed distributor 23.
- the first feed channel housing 21 and the reactor housing 24 are coaxially disposed, and are in communication with a reaction space in the reactor housing through a first feed distributor 23 disposed at an end of the first feed passage housing .
- the second feeding passage 34 is disposed inside the rotating shaft 30, and the second feeding passage 34, the rotating shaft 30 and the hollow impeller material distributor 26 are coaxially disposed with the quick mixing reactor, and the hollow impeller material
- the distributor 26 is fixedly coupled to one end of the rotating shaft 30 such that the hollow impeller material distributor 26 is axially rotated within the reactor housing by the rotating shaft 30.
- the second feed passage is in communication with the material passage 32 in the hollow impeller material distributor.
- the first feed channel housing is provided with at least one first feed port 22, and the space enclosed by the first feed channel housing 21 and the first feed distributor 23 is a first feed channel 35.
- At least one reaction liquid outlet 28 is provided at the end of the reactor housing.
- the first feed distributor 23 is provided with a plurality of first feed injection ports 33, and the hollow impeller material distributor 26 is provided with a plurality of passages perpendicular to the impeller disc, and the passages are perpendicular to the impeller discs. There are a plurality of second feed injection ports 25. Furthermore, the hollow impeller material distributor of the present invention may also be provided with a second feed injection port in accordance with Figures 5a, 5b, 5c or other possible means.
- an annular inwardly projecting reaction channel adjusting block 27 is disposed on the inner wall of the reactor casing downstream of the hollow impeller material distributor 26 to reduce the reactants to some extent.
- the first rotating blade 31 is vertically disposed on the rotating shaft 30, and the stirring blade 31 and the reaction passage adjusting block 27 are disposed on the same section perpendicular to the central axis of the reactor.
- the reactor of the present invention further includes a rotating motor coupling 29 disposed at the end of the reactor housing to facilitate relative fixation of the reactor to the rotating electrical machine.
- the phosgene solution first enters through the first feed port 22 and fills the first feed channel 35, and then is uniformly disposed through the first feed distributor 23.
- the first feed injection port 33 enters the reactor housing.
- an organic solution having an amine of the general formula (I) is introduced via a second feed channel 34 disposed inside the rotating shaft, flowing through the material passage 32 in the rotating hollow impeller material distributor 26, and through a plurality of The second feed injection port 25 sprays the polyamine solution into the phosgene solution stream to achieve rapid
- the reaction liquid outlet 28 is passed through the reaction liquid outlet 28 to the next stage reactor, and the final isocyanate is obtained by raising the temperature.
- the first feed distributor as shown in FIG. 6c, distributes a plurality of circular channels having a diameter of 20 ⁇ on the first feed distributor, and the exit velocity of the phosgene solution through the circular orifice of the first feed distributor 6m/s;
- the opening manner of the second feed injection port on the hollow impeller material distributor is as shown in Fig. 5c, the opening diameter is 10mm, and the outlet speed of the amine solution through the second feed injection port is 16m/ s ;
- the rotational speed of the rotating shaft is 1200 rpm.
- the reactor was tested on an MDI apparatus with a test load of 220,000 tons of MDI/year, an amine solution feed of 24 t/h, and chlorobenzene as the reaction solvent.
- the amine chlorobenzene solution had a mass concentration of 33%.
- the amine chlorobenzene solution is injected into the interior of the reactor through a rotating hollow impeller material distributor, and reacts rapidly with the phosgene solution entering the reactor housing through the first material distributor, wherein the concentration of the phosgene solution 80%, the mass ratio of phosgene to amine is 1.7, and then the reaction mixture obtained at the outlet of the reactor is sequentially sent to four reactors connected in series for phosgenation high temperature reaction until the solution becomes clear.
- Example 1 The temperature of the four reactors connected in series was 90, 105, 115 and 120 ° C, and the volume of each reactor was 40 m 3 . After the reaction, the product was subjected to a distillation to obtain a polymerized MD I product having a viscosity of 20 Ocp.
- Example 1 The temperature of the four reactors connected in series was 90, 105, 115 and 120 ° C, and the volume of each reactor was 40 m 3 . After the reaction, the product was subjected to a distillation to obtain a polymerized MD I product having a viscosity of 20 Ocp.
- Example 1 The temperature of the four reactors connected in series was 90, 105, 115 and 120 ° C, and the volume of each reactor was 40 m 3 . After the reaction, the product was subjected to a distillation to obtain a polymerized MD I product having a viscosity of 20 Ocp.
- the production of MDI was tested using the rapid mixing reactor shown in FIG.
- the first feed distributor is as shown in FIG. 6b, and an arc-shaped slit having a different inner diameter is distributed on the first feed distributor, and the radial width of the slit is 2 ⁇ ; the phosgene solution passes through the circle
- the exit velocity of the arcuate slit is 10 m/s.
- the opening of the second feed injection port on the hollow impeller material distributor is as shown in Fig. 5b, and the injection port is a rectangle of 3 mm x 8 mm; the amine solution passes through the second feed injection port.
- the exit speed is 22m/s.
- the rotational speed of the rotating shaft was 1400 rpm.
- the reactor was tested on an MDI apparatus with a test load of 300,000 tons of MDI/year, an amine solution feed of 33 t/h, and chlorobenzene as a reaction solvent.
- the mass concentration of the amine chlorobenzene solution was 33%.
- the amine chlorobenzene solution is injected into the interior of the reactor housing through the second feed distribution, and reacts rapidly with the phosgene solution entering the reactor housing through the first material distributor, wherein the concentration of the phosgene solution is 75%.
- the mass ratio of phosgene to amine is 1.8, and then the reaction mixture obtained at the outlet of the reactor is sequentially sent to four reactors connected in series for phosgenation and high temperature reaction until the solution becomes clear.
- the temperature of the four reactors connected in series was 90, 105, 115 and 12 (TC, the volume of each reactor was 40 m 3 .
- TC the volume of each reactor was 40 m 3 .
- a polymerized MDI product was obtained with a viscosity of 200 cp, and the NC0 mass was analyzed. The content is 31.56%.
- the mass concentration of the amine reaches 33%, and the mass ratio of phosgene to the amine is reduced to 1.7.
- Currently widely used reactors (amine concentration 15%-22%, phosgene to amine mass ratio 4-2. 4), by reducing the amount of solvent and phosgene excess ratio, not only can improve reactor utilization, improve Capacity, while reducing the energy consumed by condensation and solvent removal of excess phosgene, reducing energy consumption per unit of mass by 40%.
- the production test of polymethylene polyphenylpolyamine was carried out using the rapid mixing reactor shown in FIG.
- the first feed distributor is as shown in FIG. 6b, and the arc-shaped slits having different inner diameters are evenly distributed on the first feed distributor, and the radial width of the slit is 6 ⁇ ; aniline hydrochloride and circulating liquid
- the outlet velocity of the mixed liquid through the arcuate slit was 5 m/s.
- the opening of the second feed injection port on the hollow impeller material distributor is as shown in Fig. 5b, and the injection port has a rectangular shape of 3 mm x 8 mm; the exit velocity of the formaldehyde solution through the second feed injection port is 20 m/s.
- the rotational speed of the rotating shaft was 2400 rpm.
- the reactor was tested on a polymethylene polyphenyl polyamine apparatus with a test load of 300,000 tons of polyamine/year, and a formaldehyde solution (mass fraction of 37%) with a feed amount of 16 t/h, formaldehyde solution.
- the reaction mixture obtained at the outlet of the reactor is sent to a stirred tank for further precondensation reaction, the precondensation reaction temperature is 65 ° C, and after the steps of temperature increase, molecular rearrangement reaction, neutralization, water washing, and polyamine purification, A refined polymethylene polyphenyl polyamine product is obtained, wherein the content of the nitrogen methyl compound is 0.12%, which satisfies the product quality index.
- the reaction temperature of the precondensation is raised from 40 ° C to 65 ° C when the pore jet reactor is used, the energy consumption is reduced by 35%, and the equipment blockage is cleaned from 1 month.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
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Description
Claims
Priority Applications (8)
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HUE10852321A HUE026867T2 (en) | 2010-12-29 | 2010-12-29 | Fast mixing reactor and application |
PCT/CN2010/080434 WO2012088671A1 (zh) | 2010-12-29 | 2010-12-29 | 一种快速混合反应器及其应用 |
US13/499,703 US9138717B2 (en) | 2010-12-29 | 2010-12-29 | High-speed mixing reactor and application thereof |
BR112012029403-2A BR112012029403B1 (pt) | 2010-12-29 | 2010-12-29 | reator de rápida mistura de alta velocidade e sua aplicação |
JP2013546549A JP5850345B2 (ja) | 2010-12-29 | 2010-12-29 | 高速混合反応器およびその使用 |
EP10852321.8A EP2486975B1 (en) | 2010-12-29 | 2010-12-29 | Fast mixing reactor and use thereof |
KR1020137018951A KR101499758B1 (ko) | 2010-12-29 | 2010-12-29 | 고속 혼합 반응기 및 그의 사용방법 |
SA111330016A SA111330016B1 (ar) | 2010-12-29 | 2011-11-30 | مفاعل - خلط سريع وتطبيقاته |
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US (1) | US9138717B2 (zh) |
EP (1) | EP2486975B1 (zh) |
JP (1) | JP5850345B2 (zh) |
KR (1) | KR101499758B1 (zh) |
BR (1) | BR112012029403B1 (zh) |
HU (1) | HUE026867T2 (zh) |
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- 2010-12-29 EP EP10852321.8A patent/EP2486975B1/en active Active
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Cited By (12)
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KR101577760B1 (ko) * | 2013-08-23 | 2015-12-15 | 금호석유화학 주식회사 | 고속 분사를 이용한 이종 유체의 혼합반응기 |
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Also Published As
Publication number | Publication date |
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EP2486975B1 (en) | 2015-09-23 |
KR101499758B1 (ko) | 2015-03-06 |
BR112012029403A2 (pt) | 2016-12-06 |
HUE026867T2 (en) | 2016-08-29 |
US9138717B2 (en) | 2015-09-22 |
SA111330016B1 (ar) | 2015-01-27 |
JP5850345B2 (ja) | 2016-02-03 |
EP2486975A4 (en) | 2012-09-12 |
BR112012029403B1 (pt) | 2018-11-27 |
EP2486975A1 (en) | 2012-08-15 |
JP2014509247A (ja) | 2014-04-17 |
US20130178596A1 (en) | 2013-07-11 |
KR20130099200A (ko) | 2013-09-05 |
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