CN117299008A - Forced circulation flow alkynylation reactor and alkynediol synthesis method - Google Patents
Forced circulation flow alkynylation reactor and alkynediol synthesis method Download PDFInfo
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- CN117299008A CN117299008A CN202311191579.XA CN202311191579A CN117299008A CN 117299008 A CN117299008 A CN 117299008A CN 202311191579 A CN202311191579 A CN 202311191579A CN 117299008 A CN117299008 A CN 117299008A
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- 238000005905 alkynylation reaction Methods 0.000 title claims abstract description 16
- 238000001308 synthesis method Methods 0.000 title abstract description 3
- 239000000463 material Substances 0.000 claims abstract description 99
- 238000006243 chemical reaction Methods 0.000 claims abstract description 67
- 239000003054 catalyst Substances 0.000 claims abstract description 34
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims abstract description 25
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 23
- 150000002576 ketones Chemical class 0.000 claims abstract description 21
- 239000000376 reactant Substances 0.000 claims abstract description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 9
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 15
- 238000010924 continuous production Methods 0.000 claims description 5
- 150000002009 diols Chemical class 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000000498 cooling water Substances 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000010923 batch production Methods 0.000 claims description 2
- 239000003638 chemical reducing agent Substances 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 17
- 239000007788 liquid Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 4
- 230000002194 synthesizing effect Effects 0.000 description 4
- 239000002826 coolant Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- -1 alkyne diol Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- 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
- B01F27/80—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis
- B01F27/90—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a substantially vertical axis with paddles or arms
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/085—Feeding reactive fluids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/36—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal
- C07C29/38—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal by reaction with aldehydes or ketones
- C07C29/42—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring increasing the number of carbon atoms by reactions with formation of hydroxy groups, which may occur via intermediates being derivatives of hydroxy, e.g. O-metal by reaction with aldehydes or ketones with compounds containing triple carbon-to-carbon bonds, e.g. with metal-alkynes
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
- B01J2208/00132—Tubes
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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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00168—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
- B01J2208/00176—Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
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- Chemical & Material Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
A forced circulation flow alkynylation reactor and a synthesis method of alkynediol are provided, a jacket and a motor stirrer are arranged on a reaction shell, a dispersion plate with uniformly distributed holes is arranged on the inner wall of the junction of an upper cylinder body and a lower inverted cone of the reaction shell through a plurality of fixed rods, an inner coil is arranged on the dispersion plate, the lower part of the shell is provided with an air inlet for inputting nitrogen replacement or acetylene and a reaction material inlet for dispersing reactant ketone suspended with a catalyst, and the upper part of the reactor shell is provided with a material overflow outlet. The invention has the characteristics of large heat exchange area, forced circulation flow of materials in the reactor, uniform temperature distribution in the materials, high product purity and the like, and can realize continuous synthesis or intermittent synthesis operation of the alkynone method.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to an alkynylation reactor for synthesizing alkynediol by an alkynone method.
Background
The reactors used in the traditional alkyne diol synthesis process mainly comprise three types of trickle fixed bed, slurry bed and stirred tank reactor.
In the traditional trickle bed reactor, a catalyst required by the alkynylation reaction is loaded on a catalyst framework and then filled into a bed, acetylene is taken as a continuous phase and is introduced from the lower part of the bed, and meanwhile, reactant ketone trickles from the upper part of the bed, and the two react on the catalyst bed; the residence time of the acetylene in the reactor is insufficient, so that the conversion rate of the reaction is low, the reactants are unevenly distributed among the parts of the bed layer and cannot fully react, the catalyst is easy to adhere due to byproducts generated by the alkynylation reaction, the danger of pressure increase and even explosion due to the increase of the resistance of the bed layer exists, and meanwhile, the difficulty is caused to the unloading, recycling and the like of the catalyst.
The conventional slurry bed reactor is one of the suspended bed reactors, the catalyst is suspended in the reactant ketone by acetylene bubbling, and in the reaction process, acetylene passes through the suspended bed of the catalyst rapidly in a bubbling mode, so that the safety problem of acetylene aggregation and explosion due to bed resistance in the trickle bed reactor can be solved, but the residence time of the acetylene in the reactor is reduced, the conversion rate of the acetylene is lower, the acetylene tail gas cannot be recovered, the raw material waste is serious, and the catalyst and product slurry are difficult to separate after the reaction is finished due to the structural problem of the reactor, and the subsequent separation operation is complex.
The traditional stirred tank reactor is improved on the basis of a slurry bed reactor, and the distribution state of materials can be improved to a certain extent through stirring, but the problems of uneven distribution, multiple dead angles and the like still exist only by stirring.
In addition, in the process of synthesizing alkynediols by the alkynone method, effective heating and heat removal are required, and the conventional reactor cannot meet the requirements.
Disclosure of Invention
Aiming at the defects of the existing reactor, the invention aims to provide a forced circulation flow alkynylation reactor which can rapidly disperse materials, has uniform temperature distribution and short acetylene residence time.
The purpose of the invention is realized in the following way: the forced circulation flow alkynylation reactor has cylinder in the upper part and inverted cone in the lower part, jacket with heating medium or cooling medium, jacket inlet and jacket outlet in the upper part and the lower part, motor in the arc top, stirring shaft with stirring blades, distributing plate with homogeneously distributed holes, spiral inner coil pipe on the distributing plate, and inner coil pipe inlet and outlet in the upper part and the lower part; the inverted cone at the lower part of the reactor shell is provided with a reaction material inlet which is used for introducing nitrogen to replace or introduce acetylene and dispersing reactant ketone suspended with a catalyst; the upper part of the reactor shell is provided with a material overflow port.
Stirring paddles on the stirring shaft are three layers uniformly distributed.
And a guide cylinder is also arranged on the dispersion plate in the reactor shell, and the guide cylinder is positioned between the inner coil pipe and the stirring blade.
The inner coil extends upwardly from the dispersion plate to a height adjacent the top of the reactor shell, and the draft tube extends upwardly from the dispersion plate to the same height as the inner coil.
The material overflow port is connected with the reaction material inlet through a tee joint and a valve, and during continuous production, the material flowing out of the first 1h overflow port is input through one outlet of the tee joint and returns to the reaction material inlet, and the material flowing out of the second 1h overflow port is collected through the other outlet of the tee joint to be used as a product.
The upper part of the reactor shell is provided with a reserved feed inlet used for being connected with other equipment in series, and the bottom of the inverted cone at the lower part is provided with a discharge outlet.
It is another object of the present invention to provide a process for the synthesis of alkynediols by the alkynone process using the reactor described above.
Another object of the invention is achieved by:
the method for synthesizing the alkynediol by the alkynone method by the reactor comprises the following steps:
the continuous production mode comprises the following steps:
nitrogen enters the reactor from the air inlet for replacement, and is discharged from the air outlet; after the replacement is finished, pumping reactant ketone with dispersed and suspended catalyst into a reactor from a reactant inlet at a certain speed by using a metering pump, after the feeding is finished, turning on stirring, driving a stirring blade by a motor through a stirring shaft to mix the materials, controlling acetylene to enter the bottom of the reactor from an air inlet at a certain flow speed by using a flowmeter, wherein in the reaction process, jacket heating steam enters from a jacket inlet, steam condensate flows out from a jacket outlet, inner coil heating steam enters from an inner coil inlet, and inner coil outlet flows out;
during the reaction, the catalyst is dispersed and suspended in the ketone materials, enters the reactor from a reaction material inlet arranged at the bottom of the reactor, enters a stirring zone after being dispersed through a dispersion plate, and is fully mixed and stirred by a forced circulation flow formed by three layers of stirring blades and a flow guide cylinder, acetylene entering the reactor is absorbed by the ketone in the reactor, the reaction is carried out on the surface of the catalyst dispersed in the ketone materials, the reacted materials flow out through a material overflow port, the reaction materials continuously enter from the bottom in the reaction process, and the product materials continuously flow out from the overflow port, so that the process is continuous; returning the reaction mixture to the reactor from the reaction material inlet through an outlet of the tee joint 1h before the reaction, and starting to discharge the product material after 1 h;
in the reaction, collecting overflowed materials from a material overflow port for 1 h-2 h of the reaction to obtain the product with the material purity of about 95 percent;
batch production mode:
closing the outlet valve of the material overflow port, and changing the original continuous operation of the reactor into intermittent operation; when the temperature of the system rises to a preset value, a certain amount of acetylene is metered in from an air inlet, the jacket steam is closed, cooling water enters from an inner coil inlet, and flows out from an inner coil outlet to remove heat of the system in the reaction process, the reaction time is 4-6 h, materials are discharged from a lower discharge port after the reaction is finished, and the mixed materials are subjected to subsequent treatment to separate and recycle the catalyst.
In contrast to the prior art, the method has the advantages that,
the invention has the following beneficial effects:
(1) The external jacket and the internal coil pipe can be used for heating or cooling mediums, so that the heat exchange area of the reactor can be effectively increased to meet the requirements of a reaction process, and meanwhile, the materials in the reactor can be effectively and uniformly exchanged by matching with the stirring and the guide cylinder, and the influence of the temperature unevenness of the materials in the system on the quality of reaction products is prevented;
(2) The guide cylinder is arranged, so that the mixing efficiency can be improved. The stirring degree of the liquid is improved, and the direct mechanical shearing action of the stirrer on the liquid is enhanced; the circulating path of the liquid is also limited, a fully circulating flow pattern is established, so that all materials in the reactor can pass through a strong mixing area in the guide cylinder, and the chance of short circuit is reduced;
(3) The three-layer stirrer with the variable frequency motor, the dispersing plate and the guide cylinder are matched for use, so that materials can be dispersed more effectively, dead angles are reduced, uneven temperature distribution, catalyst adhesion, stacking and the like are prevented, and the requirements of different processes can be met;
(4) During the reaction, the catalyst is dispersed and suspended in the ketone materials, enters the reactor from a reaction material inlet arranged at the bottom of the reactor, enters a stirring zone after being dispersed through a dispersion plate, and is fully mixed and stirred by a forced circulation flow formed by three layers of stirring blades and a flow guide cylinder, acetylene entering the reactor is absorbed by the ketone in the reactor, the reaction is carried out on the surface of the catalyst dispersed in the ketone materials, the reacted materials flow out through a material overflow port, the reaction materials continuously enter from the bottom in the reaction process, and the product materials continuously flow out from the overflow port, so that the process is continuous;
(5) Compared with an elliptical bottom structure, the structure of the lower cone bottom is more convenient for replacing and recycling the catalyst, and the operation is simpler and more convenient;
(6) The variable frequency motor, the three-layer stirrer, the guide cylinder and the lower cone bottom are matched for use, so that the system material can form a forced circulation flow in the reactor, thereby strengthening heat and mass transfer of the material in the system and effectively preventing the problems of accumulation and agglomeration of the material and the catalyst;
(7) The switching between intermittent operation and continuous operation of the reactor can be realized through the valve switch at the rear end of the overflow outlet.
Drawings
FIG. 1 is a schematic view of the reactor structure of the present invention.
FIG. 2 is a (top) cross-sectional view of the line A-A' of FIG. 1.
FIG. 3 is a flow diagram of a forced circulation flow inside a reactor.
Detailed Description
The present invention will be described in detail with reference to the following examples and drawings, but it should be understood that the examples and drawings are only for illustrative purposes and are not intended to limit the scope of the present invention in any way. All reasonable variations and combinations that are included within the scope of the inventive concept fall within the scope of the present invention.
The relevant expressions in the embodiments of the invention are merely for the purpose of illustrating the invention and are not meant to be the only embodiments.
A forced circulation flow alkynylation reactor comprising:
(1) An outer cylinder: the outer cylinder comprises an arc-shaped sealing head, a straight cylinder section and a conical bottom of an (inverted cone);
(2) An outer jacket: an outer sleeve is arranged at the straight section of the outer cylinder and the bottom part of the cone, and a port is respectively arranged at the position of the jacket close to the end socket and the bottom of the cone and is used as an inlet and an outlet of heating or cooling medium;
(3) Inner coil pipe: the inner coil is a spiral coil and is arranged between the outer cylinder and the guide cylinder, and an upper outlet and a lower outlet are respectively arranged and are fixedly connected with the dispersing plate through a fixing piece;
(4) A guide shell: the stirring device is arranged between the stirring and inner coils and is fixed on the bottom part of the scattering plate;
(5) Dispersion plate: comprises a dispersing plate and a fixing piece thereof, which are fixed on the inner wall of the reactor and used for dispersing the materials entering from the bottom and simultaneously fixing the guide cylinder;
(6) Stirring: comprises a top variable frequency adjustable motor, a stirring shaft and detachable paddles;
(7) Opening: the top end enclosure is provided with a gas phase outlet and an instrument port, the upper part of the straight barrel section of the reactor is provided with a material overflow port, the lower part of the cone bottom is provided with a material inlet, and the lowest part of the cone bottom is provided with a blanking port.
Referring to fig. 1 and 2, a forced circulation flow alkynylation reactor is characterized in that the upper part of a reactor shell 17 is a cylinder, the lower part is an inverted cone, a jacket 6 for heating medium or cooling medium is arranged on the reactor shell, a jacket inlet 16 and a jacket outlet 9 are respectively arranged on the upper part and the lower part of the jacket, a motor 1 is arranged at the arc-shaped top of the reactor shell, the motor 1 is connected with a stirring shaft 19 positioned in the reactor shell through a speed reducer, stirring paddles 14 are arranged on the stirring shaft, holes are uniformly distributed on a dispersing plate 13, the dispersing plate is arranged on the inner wall of the junction of the cylinder at the upper part and the inverted cone at the lower part of the reactor shell through a plurality of fixed rods 12, a spiral inner coil 3 is arranged on the dispersing plate, and an inner coil inlet 4 and an inner coil outlet 7 are respectively positioned at the upper part and the lower part of the inner coil; the inverted cone at the lower part of the reactor shell is provided with a gas inlet 11 for introducing nitrogen for replacement or acetylene and a reaction material inlet 8 for dispersing the reactant ketone with the catalyst suspended therein; the upper part of the reactor shell is provided with a material overflow port 5. (the stirring shaft is positioned on the axis of the shell).
Stirring paddles on the stirring shaft are three layers uniformly distributed.
A guide cylinder 18 is also arranged on the dispersion plate in the reactor shell, and the guide cylinder is positioned between the inner coil pipe and the stirring blade.
The inner coil extends upwardly from the dispersion plate to a height adjacent the top of the reactor shell, and the draft tube extends upwardly from the dispersion plate to the same height as the inner coil.
The material overflow port is connected with the reaction material inlet 8 through a tee joint and a valve, and during continuous production, the material flowing out of the overflow port in the first 1h is input and returned to the reaction material inlet 8 through one outlet of the tee joint, and the material flowing out of the overflow port in the later 1h is collected as a product through the other outlet of the tee joint.
The upper part of the reactor shell is provided with a reserved feed port 16 used for being connected with other equipment in series, and the bottom of the lower inverted cone is provided with a discharge port (10).
Example 1
In this example, as shown in FIG. 1, a reactor in which only the lowermost layer of stirring paddles is provided for the actual synthesis of acetylenic diol was used when the inner coil 3, the dispersion plate 13, and the draft tube 18 were not provided.
The nitrogen enters the reactor from the air inlet 11 for replacement, after the replacement is finished, reactant ketone with dispersed and suspended catalyst is pumped into the reactor from the reactant inlet 8 at a certain speed by a metering pump, after the feeding is finished, stirring is started, the motor 1 drives the stirring blade 14 through the stirring shaft 19 to mix materials, acetylene enters the bottom of the reactor from the air inlet 11 at a certain flow speed by a flowmeter control, heating steam enters from the jacket inlet 16 in the reaction process, steam condensate flows out from the jacket outlet 9, the reacted product flows out from the material overflow port 5, the first 1h returns to the reactor, and the product material starts to be discharged after 1 h.
In this example, after the reaction was completed, it was found that the overflowed materials from the 1 st to 2 nd hour of reaction were collected from the overflow port 5 using the reactor in this example, and the purity of the product material in this stage was about 55%; after stopping the reaction, the materials have large caking in the system, the liquid level of the stirring shaft has caking, and the catalyst also has caking and serious adhesion at the bottom of the reactor.
Example 2
In this example, the process was carried out by optimizing the process of example 1, adding the inner coil 3 and the dispersion plate 13 (fixed to the inner wall of the reactor) to the inside of the outer tube, and synthesizing the acetylenic diol by using the same process flow as in example 1.
After the replacement, reactant ketone with dispersed and suspended catalyst is pumped into the reactor from a reactant inlet 8 at a certain speed by a metering pump, after the material is fed, stirring is started, a motor 1 drives a stirring blade 14 through a guide cylinder 19 to mix materials, acetylene is controlled by a flowmeter to enter the bottom of the reactor from the air inlet 11 at a certain flow speed, in the reaction process, jacket heating steam enters from a jacket inlet 16, steam condensate flows out from a jacket outlet 9, inner coil heating steam enters from a steam inlet 4 and outlet 7; the product after the reaction flows out from the overflow port 5, returns to the reactor for the first 1h, and starts to discharge the product after 1 h.
In this example, after the reaction was completed, it was found that the overflowed materials from the 1 st to 2 nd hour of the reaction were collected from the overflow port 5 using the reactor in this example, and the purity of the product material in this stage was about 62%; after the reaction is stopped, more small-sized caking exists in the system, the caking exists at the liquid surface of the stirring shaft, the caking exists on the inner coil pipe, and the caking adhesion phenomenon still exists at the bottom of the reactor, but less than that in the embodiment 1.
Example 3
In this example, the same procedure as in example 1 was used to synthesize acetylenic diol by optimizing the process based on example 2 and changing the stirring paddle to three layers.
Nitrogen enters the reactor from the air inlet 11 to be replaced, gas phase is discharged from the air outlet 2 after replacement, reactant ketone with dispersed and suspended catalyst is pumped into the reactor from the reactant inlet 8 by a metering pump at a certain speed after replacement, stirring is started after feeding is finished, the motor 1 drives the stirring blade 14 through a stirring shaft to mix materials, acetylene enters the bottom of the reactor from the air inlet 11 at a certain speed under the control of a flow meter, jacket heating steam enters from the jacket inlet 16, steam condensate flows out from the jacket outlet 9, inner coil heating steam enters from the inner coil inlet 4 and inner coil outlet 7; the product after the reaction flows out from the overflow port 5, returns to the reactor for the first 1h, and starts to discharge the product after 1 h.
In this example, after the reaction was completed, it was found that the overflowed materials from the 1 st to 2 nd hour of reaction were collected from the overflow port 5 using the reactor in this example, and the purity of the product material in this stage was about 80%; after stopping the reaction, the materials have a little caking in the system, the inner coil pipe has a little caking, and the catalyst has a little caking adhesion phenomenon at the bottom of the reactor.
Example 4
In this example, the same procedure as in example 1 was used to synthesize acetylenic diol by optimizing the process based on example 3 and adding a guide tube 18.
Nitrogen enters the reactor from the air inlet 11 for replacement, and is discharged from the air outlet 2; after the replacement is finished, pumping reactant ketone with dispersed and suspended catalyst into a reactor from a reactant inlet 8 at a certain speed by using a metering pump, after the feeding is finished, turning on stirring, driving a stirring blade 14 by a motor 1 through a stirring shaft to mix materials, controlling acetylene to enter the bottom of the reactor from an air inlet 11 at a certain speed by using a flowmeter, wherein in the reaction process, jacket heating steam enters from a jacket inlet 16, steam condensate flows out from a jacket outlet 9, inner coil heating steam enters from an inner coil inlet 4, and inner coil outlet 7;
in the reaction, collecting overflowed materials from a material overflow port 5 in the reaction for 1 h-2 h to obtain the product with the material purity of about 95 percent;
after stopping the reaction, the materials are basically and evenly dispersed in the system, the inner coil pipe and the stirring shaft are basically free from caking, the catalyst is basically free from caking and adhesion phenomenon at the bottom of the reactor, and the materials in the reactor can be recycled to the next batch.
Example 5
In this example, the material remaining in the system after the end of the reaction of example 4 was provided with a treatment mode other than recycling, so as to be operated when the end of the reaction and the replacement of the catalyst were required.
Closing the outlet valve of the material overflow port 5, and changing the original continuous operation of the reactor into intermittent operation; at the beginning, jacket heating steam enters from a jacket inlet 16, steam condensate flows out from a jacket outlet 9 for lifting the temperature of a system at the front stage, when the temperature of the system rises to a preset value, a certain amount of acetylene is metered in from an air inlet (11), jacket steam is closed, cooling water enters from an inner coil inlet 4, an inner coil outlet 7 flows out to remove heat of the system in the reaction process, the reaction time is 4-6 hours, after the reaction is finished, materials are discharged from a lower discharge port 10, and the mixed materials are subjected to subsequent treatment to separate and recycle the catalyst.
The above examples only represent several embodiments of the present invention, and are not limited to the scope of the patent of the present invention, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (7)
1. The forced circulation flow alkynylation reactor is characterized in that the upper part of a reactor shell (17) is a cylinder, the lower part of the reactor shell is an inverted cone, a jacket (6) using heating medium is arranged on the reactor shell, a jacket inlet (16) and a jacket outlet (9) are respectively arranged at the upper part and the lower part of the jacket, a motor (1) is arranged at the arc-shaped top of the reactor shell, the motor (1) is connected with a stirring shaft (19) positioned in the reactor shell through a speed reducer, stirring blades (14) are arranged on the stirring shaft, holes are uniformly distributed on a dispersing plate (13), the dispersing plate is arranged on the inner wall of the joint of the cylinder at the upper part of the reactor shell and the inverted cone at the lower part of the reactor shell through a plurality of fixed rods (12), a spiral inner coil (3) is arranged on the dispersing plate, and an inner coil inlet (4) and an inner coil outlet (7) are respectively positioned at the upper part and the lower part of the inner coil; an inverted cone at the lower part of the reactor shell is provided with a gas inlet (11) for introducing nitrogen for replacement or acetylene and a reactant inlet (8) for dispersing reactant ketone suspended with a catalyst; the upper part of the reactor shell is provided with a material overflow port (5).
2. The alkynylation reactor of claim 1, wherein the stirring blades on the stirring shaft are three layers uniformly distributed.
3. A forced circulation flow alkynylation reactor as claimed in claim 2, characterised in that a guide shell (18) is also mounted on the dispersion plate in the reactor housing, the guide shell being located between the inner coil and the stirring blade.
4. A forced circulation flow alkynylation reactor according to claim 3 in which the inner coil extends upwardly from the dispersion plate to a height adjacent the top of the reactor shell and the draft tube extends upwardly from the dispersion plate to the same height as the inner coil.
5. The alkynylation reactor according to claim 4, wherein the material overflow port is connected with the reaction material inlet (8) through a tee joint and a valve, and during continuous production, the material flowing out of the overflow port of the first 1h is input and returned to the reaction material inlet (8) through one outlet of the tee joint, and the material flowing out of the overflow port of the last 1h is collected as a product through the other outlet of the tee joint.
6. A forced circulation flow alkynylation reactor as claimed in claim 5, characterised in that the upper part of the reactor shell is provided with a reserved feed port (16) for use in series with other equipment and the lower inverted cone bottom is provided with a discharge port (10).
7. A process for the synthesis of acetylenic diols by the acetylenic ketonic process using the reactor according to any of the claims 1-6, characterised in, that it comprises the following steps:
the continuous production mode comprises the following steps:
nitrogen enters the reactor from the air inlet (11) for replacement, and is discharged from the air outlet (2); after the replacement is finished, pumping reactant ketone with dispersed and suspended catalyst into a reactor from a reactant inlet (8) at a certain speed by using a metering pump, after the feeding is finished, turning on stirring, driving a stirring blade (14) by a motor (1) through a stirring shaft to mix materials, controlling acetylene to enter the bottom of the reactor from an air inlet (11) at a certain flow rate by using a flowmeter, wherein in the reaction process, jacket heating steam enters from a jacket inlet (16), steam condensate flows out from a jacket outlet (9), inner coil heating steam enters from an inner coil inlet (4), and inner coil outlet (7);
during the reaction, the catalyst is dispersed and suspended in the ketone materials, enters the reactor from a reaction material inlet arranged at the bottom of the reactor, enters a stirring zone after being dispersed through a dispersion plate, and is fully mixed and stirred by a forced circulation flow formed by three layers of stirring blades and a flow guide cylinder, acetylene entering the reactor is absorbed by the ketone in the reactor, the reaction is carried out on the surface of the catalyst dispersed in the ketone materials, the reacted materials flow out through a material overflow port, the reaction materials continuously enter from the bottom in the reaction process, and the product materials continuously flow out from the overflow port, so that the process is continuous; returning the reaction mixture to the reactor from the reaction material inlet through an outlet of the tee joint 1h before the reaction, and starting to discharge the product material after 1 h;
in the reaction, collecting overflowed materials from a material overflow port (5) for 1 h-2 h of the reaction to obtain the product with the material purity of about 95 percent;
batch production mode:
closing an outlet valve of the material overflow port (5), and changing the original continuous operation of the reactor into intermittent operation; at the beginning, jacket heating steam enters from a jacket inlet (16), steam condensate flows out from a jacket outlet (9) and is used for lifting the temperature of a system at the front stage, when the temperature of the system rises to a preset value, a certain amount of acetylene is metered in from an air inlet (11), jacket steam is closed, cooling water enters from an inner coil inlet (4), an inner coil outlet (7) flows out to remove heat of the system in the reaction process, the reaction time is 4-6 hours, after the reaction is finished, materials are discharged from a lower discharge port (10), and the mixed materials are subjected to subsequent treatment to separate and recycle the catalyst.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311191579.XA CN117299008A (en) | 2023-09-15 | 2023-09-15 | Forced circulation flow alkynylation reactor and alkynediol synthesis method |
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| CN202311191579.XA CN117299008A (en) | 2023-09-15 | 2023-09-15 | Forced circulation flow alkynylation reactor and alkynediol synthesis method |
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