CN117695990A - Reactor and preparation method of hexamethylene diisocyanate - Google Patents
Reactor and preparation method of hexamethylene diisocyanate Download PDFInfo
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- CN117695990A CN117695990A CN202311647568.8A CN202311647568A CN117695990A CN 117695990 A CN117695990 A CN 117695990A CN 202311647568 A CN202311647568 A CN 202311647568A CN 117695990 A CN117695990 A CN 117695990A
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- air inlet
- inlet pipe
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- diameter
- reaction gas
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000005057 Hexamethylene diisocyanate Substances 0.000 title claims abstract description 15
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000012495 reaction gas Substances 0.000 claims abstract description 83
- 239000007789 gas Substances 0.000 claims description 85
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 claims description 30
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011261 inert gas Substances 0.000 claims description 11
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- 238000011144 upstream manufacturing Methods 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 2
- 230000003247 decreasing effect Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 description 33
- 239000000047 product Substances 0.000 description 10
- 239000012535 impurity Substances 0.000 description 7
- 239000012948 isocyanate Substances 0.000 description 6
- 150000002513 isocyanates Chemical class 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000012216 screening Methods 0.000 description 5
- 150000004985 diamines Chemical class 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000007086 side reaction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
-
- 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
-
- 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
- B01J19/0053—Details 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
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/006—Baffles
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- 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
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/005—Feed or outlet devices as such, e.g. feeding tubes provided with baffles
-
- 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
-
- 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
- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
-
- 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
- B01J2219/00777—Baffles attached to the reactor wall horizontal
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a reactor and a preparation method of hexamethylene diisocyanate, wherein the reactor comprises the following steps: the first air inlet pipe is used for introducing first reaction gas, the first end of the first air inlet pipe is provided with an end air inlet, the second end of the first air inlet pipe is provided with a first end plate, and the side wall of the first air inlet pipe is provided with an air outlet; the first air inlet pipe is inserted into the second end plate, the end air inlet is positioned outside the second air inlet pipe, and the side air outlet is positioned in the second air inlet pipe and is positioned at the downstream of the side air inlet; and the mixing pipe is arranged at the downstream of the second air inlet pipe and communicated with the air outlet at the end part of the second air inlet pipe. The technical scheme of the application can effectively solve the problem of uneven mixing of the reaction gas in the related technology.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a reactor and a preparation method of hexamethylene diisocyanate.
Background
The gas phase phosgene process is currently the most commonly used process for producing isocyanates. The isocyanate product is obtained through the steps of mixing gasified diamine, phosgene and inert gas, reacting in a reactor, quenching, spraying, rectifying and the like. How to improve the mixing uniformity of the raw materials and select a proper reaction control point is the key to obtain a high isocyanate content product.
Patent CN1263732C discloses a process for the preparation of isocyanate in the gas phase. The method adopts a tubular reactor as a main reaction part. The main body of the tubular reactor is filled with diamine or phosgene through a central nozzle, and phosgene or diamine is introduced into the upper middle part of the tubular reactor through a lateral air inlet. The lateral air inlet is uniformly introduced into the tubular reactor main body after being distributed by the flow homogenizer and the flow balancer in sequence. The reactor can well solve the problem of uneven distribution of one of phosgene or diamine in the reactor, but has poor mixing effect of two gases. And the phenomenon of back mixing of a small part of gas can exist, so that the uniformity of gas mixing is further influenced, and the blocking phenomenon is easy to occur after long-time operation.
It was found that the uniformity of mixing of 1, 6-hexamethylenediamine with the phosgene starting material has a great influence on the formation of reaction impurities. Promoting the raw materials to be fully mixed and realizing efficient reaction is the key for obtaining the high-content isocyanate product.
Disclosure of Invention
The invention mainly aims to provide a reactor and a preparation method of hexamethylene diisocyanate, so as to solve the problem of uneven mixing of reaction gases in the related art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a reactor comprising: the first air inlet pipe is used for introducing first reaction gas, the first end of the first air inlet pipe is provided with an end air inlet, the second end of the first air inlet pipe is provided with a first end plate, the side part of the side wall of the first air inlet pipe is provided with an air outlet, and the side part of the air outlet is close to the second end of the first air inlet pipe; the first air inlet pipe is inserted into the second end plate, the end air inlet is positioned outside the second air inlet pipe, and the side air outlet is positioned in the second air inlet pipe and is positioned at the downstream of the side air inlet; and the mixing pipe is arranged at the downstream of the second air inlet pipe and communicated with the air outlet at the end part of the second air inlet pipe.
Further, the diameter of the second air inlet pipe is larger than the diameter of the mixing pipe.
Further, the reactor further comprises a necking connection pipe arranged between the second air inlet pipe and the mixing pipe, the necking connection pipe comprises a first pipe section and a second pipe section, wherein the first end of the first pipe section is connected with the second air inlet pipe, the second end of the first pipe section is connected with the first end of the second pipe section, the second end of the second pipe section is connected with the mixing pipe, and the diameter of the first pipe section is gradually reduced and the diameter of the second pipe section is gradually increased in the direction from the first pipe section to the second pipe section.
Further, the ratio between the diameter of the first air inlet pipe and the diameter of the second air inlet pipe is between 1/5 and 1/3; and/or the ratio between the length of the first air inlet pipe and the length of the second air inlet pipe in the second air inlet pipe is between 2/3 and 5/6.
Further, a plurality of side air outlets are arranged on the first air inlet pipe, the side air outlets are of round hole structures, and the ratio of the aperture of the side air outlets to the diameter of the first air inlet pipe is 1/50-1/25; and/or the ratio between the sum of the areas of the plurality of side air outlets and the total area of the first air inlet pipe positioned in the second air inlet pipe is between 1/5 and 2/5.
Further, the ratio between the smallest diameter of the first pipe section and the largest diameter of the first pipe section is between 1/2 and 7/10; and/or the ratio between the maximum diameter of the second pipe section and the maximum diameter of the first pipe section is between 7/10 and 4/5.
Further, the reactor also comprises a distributor which is arranged in the second air inlet pipe and sleeved on the periphery of the first air inlet pipe, and the distributor is positioned at the downstream of the side air inlet and the upstream of the side air outlet.
Further, the distributor comprises a sieve plate, and a plurality of sieve holes are formed in the sieve plate, wherein the ratio of the diameter of the sieve holes to the diameter of the second air inlet pipe is 1/60 to 1/30; and/or the ratio between the sum of the areas of the plurality of sieve holes and the area of the sieve plate is between 3/20 and 2/5.
Further, the mixing tube is an SV type static mixer; and/or the ratio between the length of the mixing tube and the diameter of the mixing tube is between 4 and 10.
According to another aspect of the present invention, there is provided a method for preparing hexamethylene diisocyanate, wherein the method for preparing hexamethylene diisocyanate is prepared by using the reactor described above, and the method for preparing hexamethylene diisocyanate comprises: introducing a first reaction gas into the first air inlet pipe through an end air inlet, wherein the first reaction gas comprises inert gas and 1, 6-hexamethylenediamine gas; introducing a second reaction gas into the second air inlet pipe through the side air inlet, wherein the second reaction gas is phosgene; the first and second reaction gases are mixed in a mixing tube at a preset ratio and a preset temperature.
Further, before the first reaction gas is introduced into the first air inlet pipe, the preparation method further comprises the steps of heating and pressurizing the first reaction gas to pressurize the first reaction gas to 0.2-0.5 MPa, and heating the first reaction gas to 200-350 ℃; and/or, before introducing the phosgene into the second air inlet pipe, the preparation method further comprises heating and pressurizing the phosgene to pressurize the phosgene to 0.2-0.5 MPa and heating the phosgene to 200-350 ℃.
Further, the preset ratio is: the molar ratio of 1, 6-hexamethylenediamine gas to phosgene is 1: (2-5); and/or the preset temperature is 350-500 ℃.
Further, the inert gas comprises at least one of nitrogen, chlorobenzene and o-dichlorobenzene; and/or the molar ratio of the inert gas and the 1, 6-hexamethylenediamine gas in the first reaction gas is 1: (2-5).
By applying the technical scheme of the invention, the reactor comprises a first air inlet pipe for introducing first reaction gas and a second air inlet pipe for introducing second reaction gas, wherein the first reaction gas enters the first air inlet pipe from an end air inlet at the first end of the first air inlet pipe along the axial direction and enters the second air inlet pipe from a side air outlet close to the second end of the first air inlet pipe along the radial direction; the second reaction gas enters an annular space formed between the first air inlet pipe and the second air inlet pipe from a side air inlet at the first end of the second air inlet pipe along the radial direction, then moves along the axial direction of the annular space and contacts the first reaction gas moving along the radial direction to realize preliminary mixing, the flowing directions of the first reaction gas and the second reaction gas are different when the first reaction gas and the second reaction gas contact, and the two gases can be fully contacted when the two gases meet to realize uniform mixing; the first reaction gas and the second reaction gas which are subjected to preliminary mixing enter the mixing pipe through the gas outlet at the end part, so that the mixing degree is increased, and the generation of impurities is reduced. The technical scheme of the application can realize the thorough mixing and efficient reaction of two raw materials, so that the problem of uneven mixing of reaction gas in the related technology can be effectively solved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
fig. 1 shows a schematic structural view of an embodiment of a reactor according to the present invention;
FIG. 2 shows a schematic structural diagram of a distributor of the reactor of FIG. 1;
fig. 3 shows a schematic structural view of the neck joint pipe of fig. 1.
Wherein the above figures include the following reference numerals:
10. a first air inlet pipe; 11. an end air inlet; 12. a side air outlet;
20. a second air inlet pipe; 21. a side air inlet; 22. an end air outlet;
30. a mixing tube;
40. necking the connecting pipe; 41. a first pipe section; 42. a second pipe section;
50. a distributor; 51. a sieve plate; 52. and (5) screening holes.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments in accordance with the present application. As used herein, the singular is also intended to include the plural unless the context clearly indicates otherwise, and furthermore, it is to be understood that the terms "comprises" and/or "comprising" when used in this specification are taken to specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof.
The relative arrangement of the components and steps, numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless it is specifically stated otherwise. Meanwhile, it should be understood that the sizes of the respective parts shown in the drawings are not drawn in actual scale for convenience of description. Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values. It should be noted that: like reference numerals and letters denote like items in the following figures, and thus once an item is defined in one figure, no further discussion thereof is necessary in subsequent figures.
As shown in fig. 1, the present application provides a reactor, an embodiment of which includes: a first intake pipe 10, a second intake pipe 20, and a mixing pipe 30. The first air inlet pipe 10 is used for introducing first reaction gas, the first end of the first air inlet pipe 10 is provided with an end air inlet 11, the second end of the first air inlet pipe 10 is provided with a first end plate, the side part of the side wall of the first air inlet pipe 10 is provided with an air outlet 12, and the side part of the air outlet 12 is close to the second end of the first air inlet pipe 10; the second air inlet pipe 20 is used for introducing second reaction gas, a second end plate is arranged at the first end of the second air inlet pipe 20, a side air inlet 21 close to the second end plate is arranged on the side wall of the second air inlet pipe 20, an end air outlet 22 is arranged at the second end of the second air inlet pipe 20, the first air inlet pipe 10 is inserted into the second end plate, the end air inlet 11 is positioned outside the second air inlet pipe 20, and the side air outlet 12 is positioned in the second air inlet pipe 20 and positioned at the downstream of the side air inlet 21; the mixing pipe 30 is disposed downstream of the second intake pipe 20 and communicates with the end air outlet 22 of the second intake pipe 20.
Applying the technical solution of the present embodiment, the reactor comprises a first gas inlet pipe 10 for introducing a first reactive gas and a second gas inlet pipe 20 for introducing a second reactive gas, wherein the first reactive gas enters the first gas inlet pipe 10 from an end gas inlet 11 at a first end of the first gas inlet pipe 10 in an axial direction and enters the second gas inlet pipe 20 from a side gas outlet 12 near a second end of the first gas inlet pipe 10 in a radial direction; the second reaction gas enters an annular space formed between the first gas inlet pipe 10 and the second gas inlet pipe 20 from a side gas inlet 21 at the first end of the second gas inlet pipe along the radial direction, then moves along the axial direction of the annular space and contacts the first reaction gas moving along the radial direction to realize preliminary mixing, the flowing directions of the first reaction gas and the second reaction gas are different when the first reaction gas and the second reaction gas contact, and the two gases can be fully contacted when meeting to realize uniform mixing; the primarily mixed first and second reactant gases are then introduced into the mixing tube 30 through the end gas outlet 22, thereby increasing the mixing degree and reducing the generation of impurities. The technical scheme of the embodiment can realize the full mixing and efficient reaction of the two raw materials, so that the problem of uneven mixing of the reaction gas in the related technology can be effectively solved.
Specifically, the reactor in this embodiment is used for preparing hexamethylene diisocyanate, wherein the first reaction gas is a mixed gas formed by inert gas and 1, 6-hexamethylenediamine gas, and the second reaction gas is phosgene. Of course, the locations of the two types of reaction gases may be interchanged. The reactor for preparing hexamethylene diisocyanate has the advantages of good material mixing uniformity, high content of generated isocyanate and no blockage during long-time operation.
It should be noted that the above-mentioned "the side air outlet 12 is disposed near the second end of the first air intake pipe 10" means that the distance between the center of the side air outlet 12 in the vertical direction in fig. 1 and the end plate of the first end of the first air intake pipe 10 is greater than the distance between the center of the side air outlet 12 in the vertical direction in fig. 1 and the end plate of the second end of the first air intake pipe 10.
In this embodiment, the flow directions of the first reactive gas and the second reactive gas are perpendicular when they are in contact, so that sufficient mixing is achieved. Of course, in other possible embodiments, as long as the flow directions of the two reaction gases have a certain angle.
As shown in fig. 1, the diameter of the second air inlet pipe 20 is larger than the diameter of the mixing pipe 30. The first reaction gas and the second reaction gas after preliminary mixing enter the mixing pipe 30 with smaller pipe diameter, so that the flow speed of the mixed gas can be improved, the two reaction gases can be further mixed, and the final mixing uniformity is ensured.
In this embodiment, the second air inlet pipe 20 has a cylindrical pipe structure with an aspect ratio of 10-20:1.
As shown in fig. 1 and 3, in the present embodiment, the reactor further includes a necked-in connection pipe 40 provided between the second intake pipe 20 and the mixing pipe 30, the necked-in connection pipe 40 including a first pipe section 41 and a second pipe section 42, wherein a first end of the first pipe section 41 is connected to the second intake pipe 20, a second end of the first pipe section 41 is connected to a first end of the second pipe section 42, a second end of the second pipe section 42 is connected to the mixing pipe 30, and a diameter of the first pipe section 41 gradually decreases and a diameter of the second pipe section 42 gradually increases in a direction from the first pipe section 41 to the second pipe section 42. The necking connection pipe 40 is arranged between the second air inlet pipe 20 and the mixing pipe 30, so that the gas flow rate of gas passing through the necking connection pipe 40 can be effectively increased, the occurrence of backmixing phenomenon can be effectively avoided, the contact of reaction raw materials and reaction products is avoided, caking and deposition are further caused, more impurities in the final product are caused, and the yield can be effectively improved.
Specifically, in the present embodiment, the diameter of the end gas outlet 22 is larger than the diameter of the mixing pipe 30, so that the gas pressure at the end gas outlet 22 is larger than the pressure at the gas inlet of the mixing pipe 30, back mixing is suppressed, more impurities are prevented from being generated, and further caking is not easy to occur on the pipe wall of the reactor, and blocking is avoided.
In the present embodiment, the ratio between the diameter of the first intake pipe 10 and the diameter of the second intake pipe 20 is between 1/5 and 1/3. The ratio between the diameter of the first gas inlet pipe 10 and the diameter of the second gas inlet pipe within the above-described range can correspond to the amounts of the two reaction gases required in the reaction process, thereby enabling the two reaction gases to be sufficiently mixed and reacted. Preferably, the ratio between the diameter of the first air inlet pipe 10 and the diameter of the second air inlet pipe 20 may be 1/5, 1/4 or 1/3.
In the present embodiment, the ratio between the length of the first intake pipe 10 and the length of the second intake pipe 20, which are located inside the second intake pipe 20, is between 2/3 and 5/6. The ratio between the length of the first air inlet pipe 10 and the length of the second air inlet pipe 20 in the second air inlet pipe 20 is in the above range, and can correspond to the amounts of the two reaction gases required in the reaction process, so that the two reaction gases can be sufficiently mixed and reacted. Preferably, the ratio between the length of the first air intake pipe 10 located in the second air intake pipe 20 and the length of the second air intake pipe 20 may be 2/3, 9/12 or 5/6.
As shown in fig. 1, the first air inlet pipe 10 is provided with a plurality of side air outlets 12, the side air outlets 12 are in a round hole structure, and the ratio of the aperture of the side air outlets 12 to the diameter of the first air inlet pipe 10 is between 1/50 and 1/25; the ratio between the sum of the areas of the plurality of side air outlets 12 and the total area of the first air inlet pipe 10 located in the second air inlet pipe 20 is between 1/5 and 2/5. Specifically, the side air outlets 12 are provided in plural, and the plurality of side air outlets 12 are uniformly distributed on the side wall of the first air intake pipe 10, and the first reaction gas can uniformly enter the circumferential space of the annular space when entering from the first air intake pipe 10 to the second air intake pipe 20 through the side air outlets 12, thereby enabling the first reaction gas to be uniformly mixed with the second reaction gas.
Wherein the ratio between the aperture of the side gas outlet 12 and the diameter of the first gas inlet pipe 10 and the ratio between the sum of the areas of the plurality of side gas outlets 12 and the total area of the first gas inlet pipe 10 located in the second gas inlet pipe 20 are within the above-mentioned ranges, on the one hand, the uniformity of the first reaction gas entering into the annular space can be ensured, and on the other hand, the first reaction gas can have a suitable flow rate to be more uniformly mixed with the second reaction gas. Preferably, the ratio between the aperture of the side air outlet 12 and the diameter of the first air inlet duct 10 may be 1/50, 3/100 or 1/25; the ratio between the sum of the areas of the plurality of side air outlets 12 and the total area of the first air inlet pipe 10 located in the second air inlet pipe 20 may be 1/5, 3/10 or 2/5.
Specifically, in the present embodiment, the ratio between the minimum diameter of the first pipe section 41 and the maximum diameter of the first pipe section 41 is between 1/2 and 7/10; the ratio between the maximum diameter of the second tube section 42 and the maximum diameter of the first tube section 41 is between 7/10 and 4/5. The first pipe section 41 and the second pipe section 42 are connected, so that the minimum diameters of the two pipe sections are the same, and the reasonable minimum diameter can be obtained by reasonably setting the ratio between the minimum diameter and the maximum diameter of the two pipe sections so as to improve the flow rate of the mixed gas and avoid back mixing; on the other hand, the ratio of the diameter of the second inlet pipe 20 to the diameter of the mixing pipe 30 can be made within a suitable range to ensure the subsequent mixing effect in the mixing pipe 30. Preferably, the ratio between the smallest diameter of the first tube section 41 and the largest diameter of the first tube section 41 may be 1/2, 3/5 or 7/10; the ratio between the maximum diameter of the second tube section 42 and the maximum diameter of the first tube section 41 may be 7/10, 15/20 or 4/5.
In this embodiment, the axial height of the first tube section 41 and the second tube section 42 is 1.2 to 2 times the maximum diameter of each. The arrangement is such that the first pipe section 41 and the second pipe section 42 can be gently changed, and further, the rate of change of the gas flow rate of the mixed gas flowing through the first pipe section 41 and the second pipe section 42 can be controlled within a suitable range.
As shown in fig. 1, the reactor further includes a distributor 50 disposed in the second air inlet pipe 20 and sleeved on the outer periphery of the first air inlet pipe 10, the distributor 50 being located downstream of the side air inlet 21 and upstream of the side air outlet 12. After the second reaction gas enters the second gas inlet pipe 20 and before contacting with the first reaction gas, the second reaction gas can be uniformly distributed in the annular space through the distributor 50, so that the mixing uniformity of the second reaction gas and the first reaction gas is ensured when the second reaction gas and the first reaction gas are contacted later.
Specifically, as shown in fig. 2, in the present embodiment, the distributor 50 includes a screen plate 51, and a plurality of screen holes 52 are provided on the screen plate 51, wherein a ratio between diameters of the screen holes 52 and diameters of the second air intake pipe 20 is between 1/60 and 1/30; the ratio between the sum of the areas of the plurality of screening holes 52 and the area of the screening deck 51 is between 3/20 and 2/5. The ratio between the diameter of the mesh holes 52 and the diameter of the second inlet pipe 20 and the ratio between the sum of the areas of the plurality of mesh holes 52 and the area of the screen plate 51 are within the above-mentioned ranges, on the one hand, the uniformity of the second reaction gas entering the annular space can be ensured, and on the other hand, the second reaction gas can have a suitable flow rate to be mixed with the first reaction gas more uniformly. Preferably, the ratio between the diameter of the mesh openings 52 and the diameter of the second air inlet duct 20 may be 1/60, 1/40 or 1/30; the ratio between the sum of the areas of the plurality of screening holes 52 and the area of the screening deck 51 may be 3/20, 11/40 or 2/5.
In this embodiment, the mixing tube 30 is an SV type static mixer; the ratio between the length of the mixing tube 30 and the diameter of the mixing tube 30 is between 4 and 10. The use of an SV-type static mixer as the mixing tube 30 and the ratio between the length of the mixing tube 30 and the diameter of the mixing tube 30 in the above-described range enable efficient mixing of the first reaction gas and the second reaction gas. Preferably, the ratio between the length of the mixing tube 30 and the diameter of the mixing tube 30 may be 4, 7 or 10.
The application also provides a preparation method of hexamethylene diisocyanate, wherein the embodiment of the preparation method of the application adopts the reactor to prepare, and the preparation method comprises the following steps:
step S1: introducing a first reaction gas into the first gas inlet pipe 10 through the end gas inlet 11, wherein the first reaction gas comprises inert gas and 1, 6-hexamethylenediamine gas;
step S2: introducing a second reaction gas into the second air inlet pipe 20 through the side air inlet 21, wherein the second reaction gas is phosgene;
step S3: the first and second reaction gases are mixed in a preset ratio at a preset temperature in the mixing tube 30.
The hexamethylene diisocyanate prepared by the reactor has the advantages of uniform mixing, less side reaction, high yield and high purity. In addition, after the reactor is operated for a long time, the sediment on the inner wall of the reactor is less, the reactor is not easy to be blocked, and the preparation of hexamethylene diisocyanate can be carried out for a long time with high efficiency.
Before the first reaction gas is introduced into the first air inlet pipe 10, the preparation method further comprises the steps of heating and pressurizing the first reaction gas to pressurize the first reaction gas to 0.2-0.5 MPa, and heating the first reaction gas to 200-350 ℃; the preparation method further comprises heating and pressurizing the phosgene to pressurize the phosgene to 0.2-0.5 MPa and heating the phosgene to 200-350 ℃ before introducing the phosgene into the second air inlet pipe 20.
Before the first reaction gas and the second reaction gas are respectively introduced into the first air inlet pipe 10 and the second air inlet pipe 20, the first reaction gas and the second reaction gas are respectively pressurized and heated, and the first reaction gas and the second reaction gas are pressurized and heated to a considerable degree, so that the subsequent mixing and full reaction of the two reaction gases are facilitated.
Preferably, the preset ratio is: the molar ratio of 1, 6-hexamethylenediamine gas to phosgene is 1: (2-5); the preset temperature is 350-500 ℃. The absolute pressure of the two reaction gases in the mixing tube 30 is 0.2 to 0.5MPa. By controlling the amount of the raw materials and the reaction temperature within the above ranges, mixing and reaction can be more sufficiently performed to improve the yield and the purity of the product.
After the first reactive gas and the second reactive gas are respectively introduced into the first air inlet pipe 10 and the second air inlet pipe 20, the first reactive gas and the second reactive gas are primarily mixed in the second air inlet pipe 20 for 1-5 s.
Specifically, in the present embodiment, the inert gas includes at least one of nitrogen, chlorobenzene, o-dichlorobenzene; the molar ratio of the inert gas and the 1, 6-hexamethylenediamine gas in the first reaction gas is 1: (2-5).
In order to enable those skilled in the art to better understand the present invention, a detailed description of the technical solution of the present application will be provided below with reference to specific examples. These examples should not be construed as limiting the scope of the application.
Example 1
The reactor parameters were as follows: the reactor consists of three parts, namely a tubular mixing device, a necked-in connection 40 and a mixing tube 30. Wherein the tubular mixing device comprises a first air inlet pipe 10, a second air inlet pipe 20 and a distributor 50.
The second air inlet pipe 20 is of a cylindrical structure, and the length-diameter ratio is 10:1. The tail end (i.e., the second end) of the first air intake pipe 10 penetrates through the second end plate of the second air intake pipe 20 into the second air intake pipe 20, and the front end (i.e., the first end) of the first air intake pipe 10 is outside the second air intake pipe 20. The part of the first air inlet pipe 10 in the second air inlet pipe 20 is provided with a plurality of small holes (namely side air outlets 12) on the pipe wall along the axial direction of the first air inlet pipe 10, and the tail end of the first air inlet pipe 10 is in a closed state. The ratio of the diameter of the first air intake pipe 10 to the diameter of the second air intake pipe 20 is 1:3. the ratio of the diameter of the small hole to the diameter of the first air inlet pipe 10 is 1:35; the total area of the small holes occupies 28% of the area of the first air intake pipe 10 in the second air intake pipe 20. The ratio of the length of the first air inlet pipe 10 to the length of the second air inlet pipe 20 in the second air inlet pipe 20 is 1:1.2.
The distributor 50 is a circular sieve plate structure, the center of the sieve plate 51 is penetrated and occupied by the first air inlet pipe 10, a plurality of circular holes (i.e. sieve holes 52) are distributed in the rest part, and the sieve plate 51 is connected with the outer wall of the first air inlet pipe 10 and the inner wall of the second air inlet pipe 20. The diameter of the screen plate 51 is the same as the diameter of the second inlet duct 20. The ratio of the diameter of the circular hole to the diameter of the second air inlet pipe 20 is 1:45. the circular holes are uniformly distributed along the radial direction of the distributor 50, and the aperture ratio of the screen plate 51 is 25%.
The first pipe section 41 and the second pipe section 42 are both in a truncated cone-shaped structure, and one end of the first pipe section 41 with a large cross section area is axially connected with the air outlet 22 at the end part of the second air inlet pipe 20, and the diameters of the first pipe section 41 and the second pipe section are equal. The end of the second pipe section 42 having a larger cross-sectional area is axially connected to the inlet end of the mixing pipe 30, both of which have equal diameters. The diameter of the end of the second tube section 42 having the larger cross-sectional area is 0.75 times the diameter of the end of the first tube section 41 having the larger cross-sectional area. The ends of the first tube section 41 and the second tube section 42 having the smaller cross-sectional areas are connected to each other in the axial direction, and the diameters thereof are equal to each other, and are 0.5 times the diameter of the end of the first tube section 41 having the larger cross-sectional area. The axial height of the first tube section 41 and the second tube section 42 is 1.5 times the diameter of the end of the respective larger cross-sectional area.
The mixing tube 30 is in a cylindrical structure and is an SV type static mixer, and the length-diameter ratio of the static mixer is 5:1.
the reactor is adopted as a reaction device. Introducing a mixed gas of 1, 6-hexamethylenediamine and nitrogen into a first air inlet pipe 10, wherein the molar ratio of the 1, 6-hexamethylenediamine to the nitrogen is 1:3, and controlling the absolute pressure of the mixed gas to be 0.4MPa and the temperature to be 300 ℃; phosgene was introduced into the second inlet pipe 20, wherein the absolute pressure of phosgene was 0.4MPa; the temperature of phosgene was 300 ℃. The two are mixed in a second air inlet pipe 20, the mol ratio of 1, 6-hexamethylenediamine to phosgene is 1:4, and the reaction residence time of the mixed gas in the second air inlet pipe 20 is 2s.
The mixed gas was reacted in the mixing tube 30 through the first tube section 41 and the second tube section 42 at a temperature of 350℃and an absolute pressure of 0.38MPa. After the reaction, the mixed gas leaves the reactor.
And quenching, spraying, rectifying and other steps to obtain hexamethylene diisocyanate product. The purity of the product was calculated to be 99.7% and the yield 96.7%.
Example 2
The reaction apparatus of example 2 was identical to example 1, with the following differences in the preparation method:
introducing mixed gas of 1, 6-hexamethylenediamine and nitrogen into the first air inlet pipe 10, wherein the absolute pressure is 0.5MPa, and the temperature is 350 ℃; the absolute pressure of the phosgene introduced into the second inlet pipe 20 was 0.5MPa; the temperature of phosgene was 350 ℃.
The subsequent treatment process was the same as in example 1. The purity of the product was calculated to be 99.5% and the yield was 96.47%.
Example 3
The preparation of example 3 was identical to that of example 1, with the following differences in the reactor:
the ratio of the diameter of the first air intake pipe 10 to the diameter of the second air intake pipe 20 is 1/5, and the ratio of the length of the first air intake pipe 10 to the length of the second air intake pipe 20 in the second air intake pipe 20 is 2/3.
The purity of the product was calculated to be 99.48% and the yield 96.44%.
Comparative example 1
Comparative example 1 was prepared in the same manner as in example 1, with the following differences in the reactor:
the air outlet on the first air inlet pipe 10 is provided on the first end plate of the first air inlet pipe 10.
The purity of the product is 98.45% and the yield is 80.25% by calculation.
Through analysis, when the first reaction gas and the second reaction gas are contacted, the flowing directions of the two reaction gases are the same, the mixing is insufficient, a certain amount of byproducts are generated in the reaction process, and after long-time operation, part of solids are deposited on the pipe wall, so that the impurities of the side reaction polymer remain.
Comparative example 2
Comparative example 2 was prepared in the same manner as in example 1, with the following differences in the reactor:
in comparative example 2, no mixing tube was provided.
The purity of the product was calculated to be 98.2% and the yield was 83.25%.
According to analysis, the residence time of the two reaction gases in the reactor is short, the two reaction gases cannot be fully mixed, a certain amount of byproducts are generated in the reaction process, and after long-time operation, part of solids are deposited on the pipe wall, so that the polymer impurities remain in side reaction.
In the description of the present invention, it should be understood that the azimuth or positional relationships indicated by the azimuth terms such as "front, rear, upper, lower, left, right", "lateral, vertical, horizontal", and "top, bottom", etc., are generally based on the azimuth or positional relationships shown in the drawings, merely to facilitate description of the present invention and simplify the description, and these azimuth terms do not indicate and imply that the apparatus or elements referred to must have a specific azimuth or be constructed and operated in a specific azimuth, and thus should not be construed as limiting the scope of protection of the present invention; the orientation word "inner and outer" refers to inner and outer relative to the contour of the respective component itself.
Spatially relative terms, such as "above … …," "above … …," "upper surface at … …," "above," and the like, may be used herein for ease of description to describe one device or feature's spatial location relative to another device or feature as illustrated in the figures. It will be understood that the spatially relative terms are intended to encompass different orientations in use or operation in addition to the orientation depicted in the figures. For example, if the device in the figures is turned over, elements described as "above" or "over" other devices or structures would then be oriented "below" or "beneath" the other devices or structures. Thus, the exemplary term "above … …" may include both orientations of "above … …" and "below … …". The device may also be positioned in other different ways (rotated 90 degrees or at other orientations) and the spatially relative descriptors used herein interpreted accordingly.
In addition, the terms "first", "second", etc. are used to define the components, and are only for convenience of distinguishing the corresponding components, and the terms have no special meaning unless otherwise stated, and therefore should not be construed as limiting the scope of the present invention.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. A reactor, comprising:
the device comprises a first air inlet pipe (10) for introducing first reaction gas, wherein the first end of the first air inlet pipe (10) is provided with an end air inlet (11), the second end of the first air inlet pipe (10) is provided with a first end plate, the side part of the side wall of the first air inlet pipe (10) is provided with an air outlet (12), and the side part of the air outlet (12) is close to the second end of the first air inlet pipe (10);
the second air inlet pipe (20) is used for introducing second reaction gas, a second end plate is arranged at the first end of the second air inlet pipe (20), a side air inlet (21) close to the second end plate is arranged on the side wall of the second air inlet pipe (20), an end air outlet (22) is arranged at the second end of the second air inlet pipe (20), the first air inlet pipe (10) is inserted into the second end plate, the end air inlet (11) is positioned outside the second air inlet pipe (20), and the side air outlet (12) is positioned in the second air inlet pipe (20) and is positioned at the downstream of the side air inlet (21);
and a mixing pipe (30) which is arranged downstream of the second air inlet pipe (20) and is communicated with an end air outlet (22) of the second air inlet pipe (20).
2. Reactor according to claim 1, characterized in that the diameter of the second inlet pipe (20) is larger than the diameter of the mixing pipe (30).
3. The reactor according to claim 2, further comprising a necked-in connection pipe (40) arranged between the second inlet pipe (20) and the mixing pipe (30), the necked-in connection pipe (40) comprising a first pipe section (41) and a second pipe section (42), wherein a first end of the first pipe section (41) is connected to the second inlet pipe (20), a second end of the first pipe section (41) is connected to a first end of the second pipe section (42), a second end of the second pipe section (42) is connected to the mixing pipe (30), the diameter of the first pipe section (41) gradually decreasing and the diameter of the second pipe section (42) gradually increasing in a direction from the first pipe section (41) to the second pipe section (42).
4. A reactor according to any one of claim 1 to 3,
the ratio between the diameter of the first inlet pipe (10) and the diameter of the second inlet pipe (20) is between 1/5 and 1/3; and/or the number of the groups of groups,
the ratio between the length of the first air inlet pipe (10) and the length of the second air inlet pipe (20) in the second air inlet pipe (20) is between 2/3 and 5/6.
5. A reactor according to any one of claims 1 to 3, wherein the first inlet pipe (10) is provided with a plurality of side air outlets (12), the side air outlets (12) being of circular hole configuration, wherein,
the ratio between the aperture of the side air outlet (12) and the diameter of the first air inlet pipe (10) is between 1/50 and 1/25; and/or the number of the groups of groups,
the ratio between the sum of the areas of the plurality of side air outlets (12) and the total area of the first air inlet pipe (10) located in the second air inlet pipe (20) is between 1/5 and 2/5.
6. A reactor according to claim 3,
-the ratio between the smallest diameter of the first tube section (41) and the largest diameter of the first tube section (41) is between 1/2 and 7/10; and/or the number of the groups of groups,
the ratio between the maximum diameter of the second tube section (42) and the maximum diameter of the first tube section (41) is between 7/10 and 4/5.
7. A reactor according to any one of claims 1 to 3, further comprising a distributor (50) arranged in the second inlet pipe (20) and around the periphery of the first inlet pipe (10), the distributor (50) being located downstream of the side inlet port (21) and upstream of the side outlet port (12).
8. The reactor according to claim 7, wherein the distributor (50) comprises a screen (51), the screen (51) being provided with a plurality of screen holes (52), wherein,
the ratio between the diameter of the sieve mesh (52) and the diameter of the second air inlet pipe (20) is between 1/60 and 1/30; and/or the number of the groups of groups,
the ratio between the sum of the areas of the plurality of sieve holes (52) and the area of the sieve plate (51) is between 3/20 and 2/5.
9. A reactor according to any one of claim 1 to 3,
the mixing pipe (30) is an SV type static mixer; and/or the number of the groups of groups,
the ratio between the length of the mixing tube (30) and the diameter of the mixing tube (30) is between 4 and 10.
10. A process for preparing hexamethylene diisocyanate, characterized in that it is prepared using the reactor according to any one of claims 1 to 9, comprising:
introducing the first reaction gas into the first air inlet pipe (10) through the end air inlet (11), wherein the first reaction gas comprises inert gas and 1, 6-hexamethylenediamine gas;
introducing a second reaction gas into the second air inlet pipe (20) through the side air inlet (21), wherein the second reaction gas is phosgene;
the first and second reactant gases are mixed in a predetermined ratio within the mixing tube (30) at a predetermined temperature.
11. The method according to claim 10, wherein,
before the first reaction gas is introduced into the first air inlet pipe (10), the preparation method further comprises the steps of heating and pressurizing the first reaction gas to pressurize the first reaction gas to 0.2-0.5 MPa, and heating the first reaction gas to 200-350 ℃; and/or the number of the groups of groups,
the preparation method further comprises the step of heating and pressurizing the phosgene to 0.2-0.5 MPa and heating the phosgene to 200-350 ℃ before the phosgene is introduced into the second air inlet pipe (20).
12. The method according to claim 10, wherein,
the preset proportion is as follows: the molar ratio of the 1, 6-hexamethylenediamine gas to the phosgene is 1: (2-5); and/or the number of the groups of groups,
the preset temperature is 350-500 ℃.
13. The method according to claim 10, wherein,
the inert gas comprises at least one of nitrogen, chlorobenzene and o-dichlorobenzene; and/or the number of the groups of groups,
the molar ratio of the inert gas and the 1, 6-hexamethylenediamine gas in the first reaction gas is 1:
(2～5)。
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| CN202311647568.8A CN117695990A (en) | 2023-12-04 | 2023-12-04 | Reactor and preparation method of hexamethylene diisocyanate |
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| CN202311647568.8A CN117695990A (en) | 2023-12-04 | 2023-12-04 | Reactor and preparation method of hexamethylene diisocyanate |
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