CN113634198A - Multi-site fluid distribution device and continuous flow nitration reaction device - Google Patents

Multi-site fluid distribution device and continuous flow nitration reaction device Download PDF

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Publication number
CN113634198A
CN113634198A CN202111213090.9A CN202111213090A CN113634198A CN 113634198 A CN113634198 A CN 113634198A CN 202111213090 A CN202111213090 A CN 202111213090A CN 113634198 A CN113634198 A CN 113634198A
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branch
reactor
fluid distribution
inner diameter
pipeline
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陶建
洪浩
洪亮
郑淞元
王苗
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Asymchem Laboratories Tianjin Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/001Feed or outlet devices as such, e.g. feeding tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/002Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/008Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/02Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2204/00Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
    • B01J2204/002Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00027Process aspects
    • B01J2219/00033Continuous processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects

Abstract

The invention provides a multi-point fluid distribution device and a continuous flow nitration device. The multi-site fluid distribution apparatus comprises: the tubular pressure-stabilizing chamber and the at least two branch pipelines are communicated, the inner diameter of each branch pipeline is communicated with the inlet end of the target reactor, the ratio of the inner diameter of each branch pipeline to the inner diameter of the target reactor is less than or equal to 1:4, and the target reactor comprises a coil reactor or a columnar reactor. The application provides a multiposition fluid distribution device includes steady voltage cavity and a plurality of branch pipelines that communicate with steady voltage cavity, can make it regulate and control the flow in each branch pipe through the hydraulics flow resistance through injecing the internal diameter ratio of target reactor and branch pipeline in above-mentioned scope to the realization improves the effect of fluid distribution homogeneity in each branch pipeline.

Description

Multi-site fluid distribution device and continuous flow nitration reaction device
Technical Field
The invention relates to the field of synthesis of medical intermediates, in particular to a multi-site fluid distribution device and a continuous flow nitration device.
Background
The mixed acid nitration reaction plays an important role in the synthesis of medical intermediates, the reaction is a typical rapid strong exothermic reaction, and the reaction process is characterized by comprising the following steps: (1) the reaction speed is high, and the reaction is almost instantly finished; (2) the heat release is large, and there is a risk of heat accumulation. Therefore, the feeding speed and the temperature are strictly controlled in the mixed acid nitration process, the higher the temperature is, the faster the nitration reaction speed is, the more heat is emitted, and the temperature is easy to lose control and explode. Therefore, the process often needs to add the nitric acid in different strands to achieve the effects of dispersing the reaction heat and adjusting the feeding ratio.
The existing multi-site feeding mode generally adopts a plurality of pumps to carry out dispersed feeding. However, the method has large equipment investment, and related technologies are not developed to feed materials in a mode of 'one to more'.
The prior literature also reports multi-channel parallel amplification techniques for nitration reactions. However, the technology can only realize the uniform distribution of the fluid under the working condition that the pressure at the tail end of each parallel branch is consistent, and no relevant report is reported on the uniform distribution of the parallel connection of multiple pipes under the condition that the pressure at the tail end sites of the parallel branches is inconsistent.
Another prior document also reports a multipoint dripping device for a reaction kettle, which comprises a reaction kettle with an opening at the upper part and a dripping pipe extending into the reaction kettle through the hole, wherein the lower part of the dripping pipe is integrally connected with a dripping ring, and the dripping ring is provided with a plurality of dripping holes. The method also has the problem that when the dripping rings are not positioned on the same horizontal plane, the fluid distribution at each position is not uniform.
In view of the above problems, it is desirable to provide a fluid distribution device capable of solving the uneven distribution of fluid at multiple points at different levels.
Disclosure of Invention
The invention mainly aims to provide a multi-point fluid distribution device and a continuous flow nitration device, which aim to solve the problem of uneven fluid distribution caused by uneven fluid distribution of all points with different horizontal heights or hydraulic pressure drop existing in the same horizontal height of the existing multi-point fluid distribution device.
To achieve the above object, an aspect of the present invention provides a multi-site fluid distribution apparatus comprising: the device comprises a tubular pressure-stabilizing chamber and at least two branch pipelines, wherein each branch pipeline is distributed along the length direction of the tubular pressure-stabilizing chamber and is communicated with the tubular pressure-stabilizing chamber, the inner diameter of each branch pipeline is communicated with the inlet end of a target reactor, the ratio of the inner diameter of each branch pipeline to the inner diameter of the target reactor is less than or equal to 1:4, and the target reactor comprises a coil reactor or a columnar reactor.
Furthermore, the tubular pressure stabilizing chamber is provided with a feed inlet and an exhaust outlet, and the exhaust outlet and the feed inlet are respectively positioned at two ends of the tubular pressure stabilizing chamber.
Further, when the number of the branch pipelines is recorded as N and the length of the tubular pressure stabilizing chamber is recorded as L, the shortest distance between the branch pipelines and the feed inlet is L/(N + 1), and the branch pipelines are uniformly distributed on the tubular pressure stabilizing chamber.
Furthermore, the ratio of the inner diameter of the branch pipeline to the inner diameter of the tubular pressure stabilizing chamber is 1 (10-100).
Further, the number of branch pipelines is N, N is more than or equal to 2, and when the main pipeline communicated with each branch pipeline is a coil reactor, each branch pipeline meets the following formula:
Figure 953039DEST_PATH_IMAGE001
whereinl n Represents the distance from the nth-1 site to the nth site, and has the unit of m;u nthe mixing flow rate at the n-1 th site is shown,u 1the inlet flow velocity of the main pipeline of the coil reactor is expressed in m/s;
Figure 909494DEST_PATH_IMAGE002
representing the branch length of the nth branch line of the multi-point fluid distribution apparatus,
Figure 728545DEST_PATH_IMAGE003
representing the branch flow rate of the nth branch line of the multi-point fluid distribution device in m/s;
Figure 22124DEST_PATH_IMAGE004
which represents the viscosity of the mixed fluid in the main line of the coil reactor,the unit is Pa.s;dthe inner diameter of the main pipeline of the coil reactor is expressed in m;
Figure 607301DEST_PATH_IMAGE005
the viscosity of the mixed fluid in each branch line of the multi-point fluid distribution device is expressed by Pa & s;
Figure 328133DEST_PATH_IMAGE006
the inner diameter of each branch pipeline of the multi-point fluid distribution device is expressed in m;
when the main pipeline communicated with each branch pipeline is a columnar reactor, each branch pipeline meets the following formula:
Figure 634480DEST_PATH_IMAGE007
Z nis the height of a point in the n branch pipeline, and takes z =0 as a reference point, and the position where z =0 is the horizontal height of a feed inlet at the lower end of the columnar reactor,Z n-1is the height of the position point in the branch pipeline No. n-1 in the unit of m; g is the acceleration of gravity, and the value is 9.8 m/s2P n-1Representing the pressure at the (n-1) th feed location,P nrepresents the pressure at the nth feed position in Pa; rho is the density of the main fluid in the main pipeline, and the unit is kg/m;u n-1the mixed fluid flow rate of the main pipeline in the (n-1) th feeding point,
Figure 731749DEST_PATH_IMAGE004
the viscosity of the mixed fluid of the main pipeline is expressed as Pa.s; ln-1The length of the main pipeline from the n-1 st feeding point to the n-th feeding point,dis the inner diameter of the main pipe of the columnar reactor in m.
Further, when the main pipeline communicated with each branch pipeline is a coil reactor and the inner diameter of the coil reactor is 2mm, the inner diameter of the tubular pressure stabilizing chamber is 14 mm; the number of the branch pipelines is 4, and when the inner diameter is 0.5mm, the length of each branch pipeline is 4.2m, 1m and 1 m; when the main pipeline communicated with each branch pipeline is a columnar reactor and the inner diameter of the columnar reactor is 35mm, the inner diameter of the tubular pressure stabilizing chamber is 14mm, the number of the branch pipelines is 3, and the inner diameter of each branch pipeline is 0.5mm, the length of each branch pipeline is 0.5m, 0.5m and 0.5 m.
Furthermore, the multi-point fluid distribution device is provided with throttle valves, and the throttle valves are arranged on the branch pipelines in a one-to-one correspondence manner.
In another aspect, the present application provides a continuous flow nitration apparatus, comprising a feeding device and a reaction device in communication with the feeding device, wherein the feeding device is a multi-point fluid distribution device as provided herein.
Further, the continuous flow nitration reaction device is a coil reactor or a column reactor.
By applying the technical scheme of the invention, the multi-point fluid distribution device comprises the pressure stabilizing chamber and the branch pipelines communicated with the pressure stabilizing chamber, and the flow in each branch pipeline can be regulated and controlled through the hydraulic flow resistance by limiting the inner diameter ratio of the pressure stabilizing chamber to the branch pipelines within the range, so that the effect of improving the fluid distribution uniformity in each branch pipeline is realized.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a preferred four-in-one multi-point fluid distribution apparatus;
FIG. 2 is a continuous flow nitration apparatus adapted for use in a coil reactor as used in example 1;
FIG. 3 shows a continuous flow nitration apparatus adapted for use in a column reactor as used in example 2.
Wherein the figures include the following reference numerals:
10. a pressure-stabilizing chamber; 20. a branch pipeline; 11. a feed inlet; 12. an exhaust port; 30. a coil reactor; 40. a columnar reactor.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background, the existing multi-site fluid distribution device has the problems of uneven fluid distribution at sites with different levels or uneven fluid distribution caused by hydraulic pressure drop at the same level. In order to solve the above technical problem, the present application provides a multi-point fluid distribution apparatus, comprising: the device comprises a pressure stabilizing chamber and at least two branch pipelines, wherein each branch pipeline is distributed along the length direction of the pressure stabilizing chamber and is communicated with the pressure stabilizing chamber, the inner diameter of each branch pipeline is communicated with the inlet end of a target reactor, the ratio of the inner diameter of each branch pipeline to the inner diameter of the target reactor is less than or equal to 1:4, and the target reactor comprises a coil reactor or a columnar reactor.
The application provides a multiposition fluid distribution device includes steady voltage cavity and a plurality of branch pipelines that communicate with steady voltage cavity, can make it regulate and control the flow in each branch pipe through the hydraulics flow resistance through injecing the internal diameter ratio of target reactor and branch pipeline in above-mentioned scope to the realization improves the effect of fluid distribution homogeneity in each branch pipeline.
In a preferred multi-site fluid distribution device, as shown in FIG. 1. Comprises a pressure stabilizing chamber 10, a branch pipeline 20, a feed inlet 11 and an exhaust port 12.
In a preferred embodiment, the pressure stabilizing chamber is provided with a feeding port and an exhaust port, and the exhaust port and the feeding port are respectively positioned at two ends of the pressure stabilizing chamber. The feeding hole and the exhaust port are arranged at the two ends of the pressure stabilizing cavity, so that the influence of the feeding and exhausting processes on the flowing of fluid in the pressure stabilizing cavity can be reduced, and the risk of uneven distribution of fluid in each branch pipeline can be reduced.
In a preferred embodiment, when the number of the branch pipes is N and the length of the pressure stabilizing chamber is L, the shortest distance between the branch pipes and the feed port is L/(N + 1), and the branch pipes are uniformly distributed on the pressure stabilizing chamber.
The uniformity of the feeding pressure at the tail end of the branch pipeline can be regulated and controlled by regulating the proportion between the pressure stabilizing chamber and the branch pipeline, and the smaller the inner diameter ratio of the branch outlet pipeline to the pressure stabilizing chamber, the more obvious the effect of the regulating action of the hydraulic flow resistance is. Preferably, the ratio of the inner diameter of the branch pipeline to the inner diameter of the tubular pressure stabilizing chamber is 1 (10-100).
Aiming at the common coil reactor and the columnar reactor, in order to further reduce the flow difference in each branch pipeline and improve the feeding uniformity, in a preferred embodiment, the number of the branch pipelines is N, N is more than or equal to 2, and when the main pipeline communicated with each branch pipeline is the coil reactor, each branch pipeline meets the following formula:
Figure 439942DEST_PATH_IMAGE001
whereinl n Represents the distance from the nth-1 site to the nth site, and has the unit of m;u nthe mixing flow rate at the n-1 th site is shown,u 1the inlet flow velocity of the main pipeline of the coil reactor is expressed in m/s;
Figure 3779DEST_PATH_IMAGE002
representing the branch length of the nth branch line of the multi-point fluid distribution apparatus,
Figure 125318DEST_PATH_IMAGE003
representing the branch flow rate of the nth branch line of the multi-point fluid distribution device in m/s;
Figure 698382DEST_PATH_IMAGE004
the viscosity of the mixed fluid in the main pipeline of the coil reactor is expressed in Pa & s;dthe inner diameter of the main pipeline of the coil reactor is expressed in m;
Figure 120136DEST_PATH_IMAGE005
the viscosity of the mixed fluid in each branch line of the multi-point fluid distribution device is expressed by Pa & s;
Figure 323716DEST_PATH_IMAGE006
in each branch line representing a multi-point fluid distribution apparatusDiameter, in m;
when the main pipeline communicated with each branch pipeline is a columnar reactor, each branch pipeline meets the following formula:
Figure 463710DEST_PATH_IMAGE008
Z nis the height of a point in the n branch pipeline, and takes z =0 as a reference point, and the position where z =0 is the horizontal height of a feed inlet at the lower end of the columnar reactor,Zn-1is the height of the position point in the branch pipeline No. n-1 in the unit of m; g is the acceleration of gravity, and the value is 9.8 m/s2P n-1Representing the pressure at the (n-1) th feed location,P nrepresents the pressure at the nth feed position in Pa; rho is the density of the main fluid in the main pipeline, and the unit is kg/m;u n-1the mixed fluid flow rate of the main pipeline in the (n-1) th feeding point,
Figure 43727DEST_PATH_IMAGE004
the viscosity of the mixed fluid of the main pipeline is expressed as Pa.s; ln-1The length of the main pipeline from the n-1 st feeding point to the n-th feeding point,dis the inner diameter of the main pipe of the columnar reactor in m.
More preferably, when the main pipeline communicated with each branch pipeline is a coil reactor, and the inner diameter of the coil reactor is 2mm, the inner diameter of the tubular pressure stabilizing chamber is 14 mm; the number of the branch pipelines is 4, and when the inner diameter is 0.5mm, the length of each branch pipeline is 4.2m, 1m and 1 m; when the main pipeline communicated with each branch pipeline is a columnar reactor, the inner diameter of the tubular pressure stabilizing chamber is 14mm, and the inner diameter of the columnar reactor is 35 mm; the number of branch pipes is 3, and when the inner diameter of each branch pipe is 0.5mm, the length of each branch pipe is 0.5m, 0.5 m. Limiting the inner diameter of the reactor, the inner diameter of the pressure stabilizing chamber, the number and inner diameter of the branch pipes and the height difference of the feeding sites within the above ranges can further reduce the risk of inconsistent pressure at each site caused by on-way flow resistance caused by fluid flow in the pressure stabilizing chamber, or reduce the risk of inconsistent pressure at each site caused by mechanical energy loss caused by the height difference, thereby further improving the feeding uniformity at each site.
In a preferred embodiment, the multi-point fluid distribution device is provided with throttle valves, which are arranged in a one-to-one correspondence on the branch lines. The throttle valves are respectively arranged on the branch pipelines to adjust the flow in the branch pipelines, and the feeding uniformity of each site is further improved by combining with the hydraulic flow resistance.
The higher the temperature of the mixed acid nitration process is, the faster the nitration reaction speed is, the more heat is released, the explosion caused by temperature runaway is easy to be caused, and therefore, the feeding speed and the temperature need to be strictly controlled. In another aspect, the present application provides a continuous flow nitration apparatus, comprising a feeding device, a reaction device in communication with the feeding device, the feeding device being a multi-point fluid distribution device as provided herein.
Because the multi-point fluid distribution device provided by the application can enable the pressure stabilizing chamber and the branch pipelines to regulate and control the flow in each branch pipeline through the hydraulic flow resistance by limiting the inner diameter ratio of the pressure stabilizing chamber and the branch pipelines in the range, the effect of improving the distribution uniformity of the fluid in each branch pipeline is realized. Therefore, the device is used as a feeding device of a continuous flow nitration reaction device, and the nitration reaction in the reaction device is more smoothly carried out. Meanwhile, by adopting the multi-point feeding, the heat generated by the reaction can be distributed to different parts, the temperature fluctuation is slowed down, and the temperature runaway phenomenon is inhibited. The catalyst is used in the reaction with violent reaction and large heat release, and the safety of the reaction is greatly improved.
The multi-point fluid distribution device can achieve the effect of adjusting the volume ratio of the raw materials. For the reaction with larger volume ratio, large streams can be fed in a dispersed mode, and the feeding ratio of the mixing section can be adjusted. For the reaction with more side reactions, starvation reaction can be carried out, and the occurrence of side reactions is reduced. The above-mentioned reaction apparatus may be a reactor commonly used in the art, for example, in the case where the reaction apparatus is a coil reactor or a column reactor.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
Example 1 a continuous flow nitration reactor apparatus suitable for use in a coil reactor is shown in figure 2.
The homogeneous nitration reaction is carried out in the device, and the specific process comprises the following steps:
main ingredient (C)12H18Cl2O2) The mixture with concentrated sulfuric acid is pumped into a coil reactor 30 at a feeding speed of 11.98mL/min, nitric acid enters a pressure stabilizing chamber 10 of a multi-point fluid distribution device at a total flow rate of 1.1mL/min and is divided into four strands through a branch pipeline 20 for dripping from different points, the height difference of each dripping point is 0mm, the adding mode of the nitric acid strands adopts a multi-point dripping device, in the multi-point dripping device, the ratio of the inner diameter of the pressure stabilizing chamber 10 to the inner diameter of the branch pipeline 20 is 28:1(14mm, 0.5mm), the inner diameter of the coil reactor is 2mm, and the lengths of the branch pipelines are 4.2m, 1m and 1m respectively.
Example 2
Example 2 a continuous flow nitration reaction apparatus suitable for use in a column reactor is shown in figure 3.
The homogeneous nitration reaction comprises the following steps:
a mixture of a main material (isooctanol) and concentrated sulfuric acid is pumped into a columnar reactor 40 at a feeding speed of 2.3mL/min, nitric acid enters a pressure stabilizing chamber 10 of a multi-point fluid distribution device at a total flow rate of 0.17mL/min and is divided into three strands through a branch pipeline 20 to be dripped from different points, the height difference of each dripping point is 35mm, the inner diameter of the columnar reactor is 35mm, a multi-point dripping device is applied to the adding mode of the nitric acid strands, the ratio of the inner diameter in the pressure stabilizing chamber to the inner diameter of the branch pipeline is 28:1(14mm, 0.5mm), and the lengths of the branch pipelines are 0.5m, 0.5m and 0.5m respectively.
Comparative example 1
The raw materials used in example 1 were identical in type and amount, except that nitric acid was added in one portion.
And (3) comparing reaction results: respectively carrying out 'one strand of feeding' and 'multi-point dropping' reaction tests under the same operation condition, and tracking the purity of the raw material residue, the product and impurities by using HPLC; the results show that:
in comparative example 1, the effect of the "one feed" reaction: 1.22 percent of the raw material, 76.66 percent of product purity, 4.06 percent of peroxidation impurity and 18.06 percent of other impurity;
in example 1, the reaction effect of "multipoint dropping" was adopted: 0% of the raw material, 82.65% of product purity, 6.03% of peroxidation impurity and 11.32% of other impurity; in example 2, the reaction effect of "multipoint dropping" was adopted: 0% of the raw material, 81.44% of product purity, 9.99% of peroxidation impurity and 8.57% of other impurity.
From the reaction result, the reaction effect is improved to a certain extent by 'multi-point dropwise adding', all raw materials are completely reacted, the product purity is correspondingly improved, and the subsequent verification that the increase of the peroxidation impurities is caused by overhigh quenching temperature is carried out.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the application provides a multiposition fluid distribution device includes steady voltage cavity and a plurality of branch pipelines that communicate with steady voltage cavity, and the internal diameter ratio through with steady voltage cavity and branch pipeline is injectd and can be made it to regulate and control the flow in each branch pipe through the hydraulics flow resistance in above-mentioned scope to the realization improves the effect of fluid distribution homogeneity in each branch pipeline, and then is favorable to improving the yield and the purity of target product.
It is noted that the terms first, second and the like in the description and in the claims of the present application are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described or illustrated herein.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (9)

1. A multi-site fluid distribution apparatus, comprising: the device comprises a tubular pressure stabilizing chamber and at least two branch pipelines, wherein each branch pipeline is distributed along the length direction of the tubular pressure stabilizing chamber and is communicated with the tubular pressure stabilizing chamber, the inner diameter of each branch pipeline is communicated with the inlet end of a target reactor, the ratio of the inner diameter of each branch pipeline to the inner diameter of the target reactor is less than or equal to 1:4, and the target reactor comprises a coil reactor or a columnar reactor.
2. The multi-site fluid distribution apparatus of claim 1, wherein the tubular plenum chamber is provided with a feed port and an exhaust port, the exhaust port and the feed port being located at respective ends of the tubular plenum chamber.
3. The multi-site fluid distribution apparatus of claim 2, wherein when the number of the branch pipes is denoted as N and the length of the tubular plenum chamber is denoted as L, the shortest distance between the branch pipes and the feed inlet is L/(N + 1), and each branch pipe is uniformly distributed on the tubular plenum chamber.
4. The multi-site fluid distribution apparatus of any of claims 1-3, wherein the ratio of the internal diameter of the branch pipe to the internal diameter of the tubular plenum chamber is 1 (10-100).
5. The multi-point fluid distribution apparatus of claim 4, wherein the number of said branch pipes is N, N is greater than or equal to 2, and when the main pipe communicating with each of said branch pipes is a coil pipe reactor, each of said branch pipes satisfies the following formula:
Figure 621334DEST_PATH_IMAGE001
whereinl n Represents the distance from the nth-1 site to the nth site, and has the unit of m;u nthe mixing flow rate at the n-1 th site is shown,u 1indicating the inlet flow rate of the main pipe of a coil reactorThe unit is m/s;
Figure 767144DEST_PATH_IMAGE002
representing the branch length of the nth branch line of the multi-point fluid distribution apparatus,
Figure 877183DEST_PATH_IMAGE003
representing the branch flow rate of the nth branch line of the multi-point fluid distribution device in m/s;
Figure 907587DEST_PATH_IMAGE004
the viscosity of the mixed fluid in the main pipeline of the coil reactor is expressed in Pa & s;dthe inner diameter of the main pipeline of the coil reactor is expressed in m;
Figure 911315DEST_PATH_IMAGE005
the viscosity of the mixed fluid in each branch line of the multi-point fluid distribution device is expressed by Pa & s;
Figure 431289DEST_PATH_IMAGE006
the inner diameter of each branch pipeline of the multi-point fluid distribution device is expressed in m;
when the main pipeline communicated with each branch pipeline is a columnar reactor, each branch pipeline meets the following formula:
Figure 622099DEST_PATH_IMAGE007
Z nis the height of a point in the n branch pipeline, and takes z =0 as a reference point, and the position where z =0 is the horizontal height of a feed inlet at the lower end of the columnar reactor,Z n-1is the height of the position point in the branch pipeline No. n-1 in the unit of m; g is the acceleration of gravity, and the value is 9.8 m/s2P n-1Representing the pressure at the (n-1) th feed location,P nrepresents the pressure at the nth feed position in Pa; ρ is the density of the main fluid in the main pipeline, and the unit is kg ^ erm³;u n-1The mixed fluid flow rate of the main pipeline in the (n-1) th feeding point,
Figure 252932DEST_PATH_IMAGE004
the viscosity of the mixed fluid of the main pipeline is expressed as Pa.s; ln-1The length of the main pipeline from the n-1 st feeding point to the n-th feeding point,dis the inner diameter of the main pipe of the columnar reactor in m.
6. The multi-point fluid distribution apparatus of claim 5, wherein when the main pipe communicating with each of the branch pipes is a coil reactor having an inner diameter of 2mm, the inner diameter of the tubular plenum chamber is 14 mm; the number of the branch pipelines is 4, and when the inner diameter is 0.5mm, the length of each branch pipeline is 4.2m, 1m and 1 m;
when the main pipeline communicated with each branch pipeline is a columnar reactor and the inner diameter of the columnar reactor is 35mm, the inner diameter of the tubular pressure stabilizing chamber is 14mm, the number of the branch pipelines is 3, and the inner diameter of each branch pipeline is 0.5mm, the length of each branch pipeline is 0.5m, 0.5m and 0.5 m.
7. The multi-site fluid distribution apparatus of claim 5, wherein the multi-site fluid distribution apparatus is provided with throttling valves, the throttling valves being provided on the branch lines in a one-to-one correspondence.
8. A continuous flow nitration reaction apparatus comprising a feed means and a reaction means in communication with the feed means, wherein the feed means is a multi-point fluid distribution apparatus according to any one of claims 1 to 7.
9. The continuous-flow nitration apparatus of claim 8, wherein said continuous-flow nitration apparatus is a coil reactor or a column reactor.
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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101184983A (en) * 2005-03-16 2008-05-21 雅拓晶科生物系统(私人)有限公司 Methods and device for transmitting, enclosing and analysing fluid samples
CN101370577A (en) * 2006-02-23 2009-02-18 托塔尔石油化学产品研究弗吕公司 Transfer pipe between loop reactors
CN103933898A (en) * 2014-05-08 2014-07-23 中国石油大学(华东) Device and method for preparing ethylene from ethane oxidative dehydrogenation
WO2014114646A1 (en) * 2013-01-22 2014-07-31 Total Research & Technology Feluy Olefin polymerization process with continuous transfer
CN104817654A (en) * 2015-04-16 2015-08-05 浙江大学 Method and device for producing low density polyethylene
CN205868196U (en) * 2015-09-06 2017-01-11 中国石油化工股份有限公司 Feed distribution ware
CN206354257U (en) * 2016-12-05 2017-07-28 山东农业大学 A kind of multidigit point droping irrigating pipe
CN109772236A (en) * 2017-11-14 2019-05-21 中国石油化工股份有限公司 A kind of fluid distributor, reaction unit and its application
CN111647012A (en) * 2020-04-24 2020-09-11 浙江大学 Method for preparing alkylaluminoxane by using microreactor
CN112156734A (en) * 2020-10-15 2021-01-01 濮阳市欧亚化工科技有限公司 Micro-channel reactor integrating hybrid reaction and cooling and application method

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101184983A (en) * 2005-03-16 2008-05-21 雅拓晶科生物系统(私人)有限公司 Methods and device for transmitting, enclosing and analysing fluid samples
CN101370577A (en) * 2006-02-23 2009-02-18 托塔尔石油化学产品研究弗吕公司 Transfer pipe between loop reactors
WO2014114646A1 (en) * 2013-01-22 2014-07-31 Total Research & Technology Feluy Olefin polymerization process with continuous transfer
CN103933898A (en) * 2014-05-08 2014-07-23 中国石油大学(华东) Device and method for preparing ethylene from ethane oxidative dehydrogenation
CN104817654A (en) * 2015-04-16 2015-08-05 浙江大学 Method and device for producing low density polyethylene
CN205868196U (en) * 2015-09-06 2017-01-11 中国石油化工股份有限公司 Feed distribution ware
CN206354257U (en) * 2016-12-05 2017-07-28 山东农业大学 A kind of multidigit point droping irrigating pipe
CN109772236A (en) * 2017-11-14 2019-05-21 中国石油化工股份有限公司 A kind of fluid distributor, reaction unit and its application
CN111647012A (en) * 2020-04-24 2020-09-11 浙江大学 Method for preparing alkylaluminoxane by using microreactor
CN112156734A (en) * 2020-10-15 2021-01-01 濮阳市欧亚化工科技有限公司 Micro-channel reactor integrating hybrid reaction and cooling and application method

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