CN114471386B - Ammonolysis reactor and amide preparation method - Google Patents

Ammonolysis reactor and amide preparation method Download PDF

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CN114471386B
CN114471386B CN202210337875.5A CN202210337875A CN114471386B CN 114471386 B CN114471386 B CN 114471386B CN 202210337875 A CN202210337875 A CN 202210337875A CN 114471386 B CN114471386 B CN 114471386B
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liquid
reaction
cavity
distributor
vaporization
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CN114471386A (en
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马磊
蹇守华
杨松
邓龙伟
周强
赵丽红
游林
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Southwest Research and Desigin Institute of Chemical Industry
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Southwest Research and Desigin Institute of Chemical Industry
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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
    • B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
    • 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
    • B01J19/0073—Sealings
    • 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
    • B01J19/2425—Tubular reactors in parallel
    • 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
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C231/00—Preparation of carboxylic acid amides
    • C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00051—Controlling the temperature
    • B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049—Controlling or regulating processes
    • B01J2219/00245—Avoiding undesirable reactions or side-effects
    • B01J2219/00256—Leakage
    • 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
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/0095—Control aspects
    • B01J2219/00952—Sensing operations
    • B01J2219/00954—Measured properties
    • B01J2219/00963—Pressure
    • 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
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0869—Feeding or evacuating 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
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
    • B01J2219/0873—Materials to be treated
    • B01J2219/0881—Two or more materials
    • B01J2219/0884—Gas-liquid
    • 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
    • B01J2219/32—Details relating to packing elements in the form of grids or built-up elements for forming a unit of module inside the apparatus for mass or heat transfer
    • B01J2219/332—Details relating to the flow of the phases
    • B01J2219/3325—Counter-current flow
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses an ammonolysis reactor and an amide preparation method, which relate to the technical field of amide preparation and have the technical scheme that: the ammonolysis reactor comprises a shell, a liquid inlet cavity, a reaction cavity and a liquid outlet cavity, wherein the inner cavity of the shell is vertically arranged and is sequentially divided into the liquid inlet cavity, the reaction cavity and the liquid outlet cavity from top to bottom, and the liquid inlet cavity is provided with a liquid-phase ester feeding nozzle and an exhaust nozzle; the reaction cavity is adapted with a cooling working medium circulating system, and a plurality of reaction tubes are arranged in the reaction cavity and are communicated with the liquid inlet cavity and the liquid outlet cavity; the liquid outlet cavity is internally provided with a vaporization distributor, each air outlet end of the vaporization distributor is connected with the lower end of the corresponding reaction tube, and the lower end of the reaction tube is provided with an overflow path; the lower end of the liquid outlet cavity is adapted with a product discharging nozzle and an ammonia liquid feeding nozzle, the ammonia liquid feeding nozzle is connected with the feeding end of the vaporization distributor, and ammonia gas is countercurrent to liquid phase ester in the reaction tube during use, so that efficient ammonolysis reaction is realized, a plurality of reaction kettles are not required to be connected in series, and the investment and the occupied area of equipment can be reduced. The amide preparation method is based on the ammonolysis reactor, and can reduce the production cost.

Description

Ammonolysis reactor and amide preparation method
Technical Field
The invention relates to the technical field of amide preparation, in particular to an ammonolysis reactor and an amide preparation method.
Background
Amides are an important class of organic compounds containing an amide bond, and can be structurally considered as compounds produced by substitution of a hydroxyl group on a carboxyl group with an amino group or an alkylamino group. Amides generally have a higher boiling point, low molecular weight amides have a lower melting point and are liquid at ordinary temperatures and are often used as high boiling solvents in chemical reactions, such as N, N-dimethylformamide. In addition, N-dimethylformamide has excellent solubility and can dissolve various organic matters, so that the solvent is called as a universal solvent.
The synthesis method of the amide mainly comprises the following two types:
1) Ammonolysis, including acid halide ammonolysis, acid anhydride ammonolysis, ester ammonolysis, and the like. The ammonolysis method is the most classical amide preparation method, and has the characteristics of mild reaction conditions, low raw material cost and the like, and the ester ammonolysis method has the lowest reaction activity and needs longer time to obtain better yield.
2) Nitrile compounds, which are a class of organic compounds containing cyano groups, are generally more toxic by the nitrile hydrolysis process. The nitrile hydrolysis method is to hydrolyze under strong acid or strong alkaline condition to generate amide. However, since amides are easily hydrolyzed into carboxylic acids and amines under strong acid or basic conditions, and the reaction is strongly exothermic, the reaction is not easy to control and the toxicity is extremely high.
In the comprehensive view, the raw materials of the nitrile hydrolysis method have larger safety risk, severe reaction and more side reactions, and the reaction is difficult to control, so that the ammonolysis method is obviously superior to the nitrile hydrolysis method. However, the ester ammonolysis method has low reactivity and needs longer residence time, so that the existing ester ammonolysis method adopts a preparation system (shown in figure 1) with a plurality of kettle reactors with stirrers connected in series, and has large equipment investment and large occupied area.
Disclosure of Invention
Aiming at the problems of large equipment investment and technical problems of the existing ammonolysis method for producing the amide; the invention provides an ammonolysis reactor and an amide preparation method, which do not need to be connected with a plurality of reaction kettles in series, and the reactor shell is vertically arranged, so that the investment of equipment can be reduced, the occupied area of the equipment can be reduced, the production cost of the amide can be reduced, and the land resources can be saved.
The invention is realized by the following technical scheme:
in a first aspect, the invention provides an ammonolysis reactor, which comprises a shell arranged vertically, wherein the inner cavity of the shell is divided into a liquid inlet cavity, a reaction cavity and a liquid outlet cavity from top to bottom in sequence; the liquid inlet cavity is adapted with a liquid phase ester feeding nozzle, and the top of the liquid inlet cavity is provided with an exhaust nozzle; the reaction cavity is adapted with a cooling working medium circulating system, a plurality of reaction pipes are arranged in the reaction cavity, and the reaction pipes are communicated with the liquid inlet cavity and the liquid outlet cavity; the liquid outlet cavity is internally provided with a vaporization distributor, each air outlet end of the vaporization distributor is connected with the lower end of the corresponding reaction tube, and the lower end of the reaction tube is provided with an overflow channel; the lower end of the liquid outlet cavity is adapted with a product discharging nozzle and an ammonia liquid feeding nozzle, and the ammonia liquid feeding nozzle is connected with the feeding end of the vaporization distributor.
When the ammonolysis reactor provided by the invention is used, liquid phase ester enters the liquid inlet cavity through the liquid phase ester feeding nozzle to form a liquid level in the liquid inlet cavity, and enters the reaction tube partially under the action of gravity, meanwhile, the cooling working medium is circularly fed into the reaction cavity through the cooling working medium circulating system matched with the reaction cavity to cool the reaction cavity, and liquid ammonia is gasified through the gasification distributor in the liquid outlet cavity and then enters the reaction tube, so that ammonia gas flows back in the reaction tube, thereby the ammonolysis reaction is efficient, a plurality of reaction kettles are not required to be connected in series, the reactor shell is vertically arranged, the investment of equipment can be reduced, the occupied area of the equipment is reduced, the production cost of amide is reduced, and the land resources are saved.
The liquid ammonia is vaporized and uniformly distributed by the vaporization distributor and then enters the reaction tube for countercurrent, the resistance of liquid phase ester in the reaction tube can be overcome by the pressure of the vaporized liquid ammonia, the concentration of the ammonia at each point in the axial direction of the reaction tube is kept approximate, the conversion rate of ammonolysis reaction in the reaction tube can be ensured, and meanwhile, the local overheating of the reaction tube is avoided; liquid phase ester feeding forms the liquid level in the feed liquor intracavity to be full of the reaction tube, with through liquid phase ester liquid seal ammonia, prevent ammonia escape when guaranteeing that the reaction is gone on with high efficiency, can reduce ammonia escape rate by a wide margin, not only practice thrift manufacturing cost, can protect the environment moreover.
In an alternative embodiment, a first liquid phase distributor is arranged at the upper part of the liquid inlet cavity, and the liquid inlet end of the first liquid phase distributor is connected with the liquid outlet end of the liquid phase ester feeding nozzle so as to disperse the liquid phase ester entering the liquid inlet cavity, thereby absorbing the ammonia penetrating through the liquid level.
In an alternative embodiment, the upper part of the liquid inlet cavity is further provided with a second liquid phase distributor, and the second liquid phase distributor is located below the first liquid phase distributor to disperse into the liquid phase ester dispersed by the first liquid phase distributor to form droplets with smaller particle size, so that the contact area of the liquid phase ester and ammonia is increased, the reaction efficiency and the capture rate of the ammonia penetrating through the liquid level are improved, and the escape rate of the ammonia is further reduced.
In an alternative embodiment, the upper part of the liquid inlet cavity is provided with a foam remover in an adapting way so as to break bubbles through the foam remover and avoid that the gas discharged from the gas outlet nozzle brings liquid phase ester out of the reactor.
In an alternative embodiment, the reaction chamber is adapted with a cooling medium inlet and a cooling medium outlet; the cooling working medium inlet is positioned at the lower end of the reaction cavity, and the cooling working medium outlet is positioned at the upper end of the reaction cavity, so that the cooling working medium sufficiently cools the reaction tube.
In an alternative embodiment, the vaporization distributor is of a butterfly-shaped box-type structure to ensure that the liquid ammonia is vaporized in the distributor and uniformly distributed to each outlet.
In an alternative embodiment, the vaporization distributor is vertically provided with a plurality of liquid-lowering channels, so as to ensure that liquid amide generated by the reaction smoothly enters the bottom of the liquid outlet cavity through the vaporization distributor.
In an alternative embodiment, the liquid outlet end of the vaporizing distributor is connected with a plurality of pulse distribution pipes, and the gas outlet end of the pulse distribution pipes is connected with the lower end of the reaction pipe so as to connect the vaporizing distributor and the reaction pipe through pulse distribution.
In an alternative embodiment, the outlet of the pulse distribution pipe is a necking port so as to increase the initial speed of the ammonia gas entering the reaction pipe, improve the distribution rate of the ammonia gas in the reaction pipe, and effectively prevent the liquid phase ester from flowing backwards from the inlet of the pulse distribution pipe into the vaporization distributor.
In a second aspect, the present invention provides a process for the preparation of an amide comprising the steps of:
s1, feeding liquid phase amide into a liquid inlet cavity at the upper end of a reactor shell, wherein the shell is vertically arranged, the inner cavity of the shell is sequentially divided into a liquid inlet cavity, a reaction cavity and a liquid outlet cavity from top to bottom, and the liquid inlet cavity is communicated with the liquid outlet cavity through a reaction tube inserted into the reaction cavity;
s2, connecting a cooling system with the reaction cavity, and cooling the reaction tube through a cooling working medium;
s3, sending the liquid-phase ammonia into a vaporization distributor in a liquid outlet cavity, and sending the liquid-phase ammonia into the reaction tube through the vaporization distributor for ammonolysis reaction to generate amide.
The amide preparation method provided by the invention is based on the ammonolysis reactor, so that the investment of equipment can be reduced, the occupied area of the equipment is reduced, the production cost of the amide is reduced, the land resources are saved, the resistance of liquid phase ester in the reaction tube can be overcome by the pressure of liquid ammonia after vaporization, the concentration of ammonia in the reaction tube is kept to be approximate to each point in the axial direction of the reaction tube, the conversion rate of ammonolysis reaction in the reaction tube can be ensured, meanwhile, the local overheating of the reaction tube is avoided, the ammonia escape rate can be greatly reduced, the production cost is saved, and the environment is protected.
The invention has the beneficial effects that:
1. the ammonolysis reactor provided by the invention has the advantages that the inner cavity of the shell which is vertically arranged is sequentially divided into a liquid inlet cavity, a reaction cavity and a liquid outlet cavity from top to bottom, and the liquid inlet cavity is provided with a liquid phase ester feeding nozzle and an exhaust nozzle; the reaction cavity is adapted with a cooling working medium circulating system, and a plurality of reaction tubes are arranged in the reaction cavity and are communicated with the liquid inlet cavity and the liquid outlet cavity; the liquid outlet cavity is internally provided with a vaporization distributor, each air outlet end of the vaporization distributor is connected with the lower end of the corresponding reaction tube, and the lower end of the reaction tube is provided with an overflow path; the liquid outlet cavity lower end adaptation has product discharge to chew and ammonia liquid feed to chew, ammonia liquid feed is chewed and is linked to each other with the feed end of vaporization distributor, so that liquid phase ester forms the liquid seal and gets into in the reaction tube in the feed liquor cavity, liquid ammonia gets into the reaction tube countercurrent after vaporization distributor vaporization equipartition, thereby efficient ammonolysis, and cool off by the cooling medium that cooling system provided, need not a plurality of reation kettle of establishing ties, and the vertical setting of reactor shell, can reduce the investment of equipment, reduce the area of equipment, with the manufacturing cost of reduction amide and saving land resources.
2. When the ammonolysis reactor provided by the invention is used, liquid phase ester forms a liquid seal in the liquid inlet cavity and enters the reaction tube, liquid ammonia enters the reaction tube for countercurrent after being vaporized and uniformly distributed in the vaporization distributor, the resistance of the liquid phase ester in the reaction tube can be overcome by the pressure of the vaporized liquid ammonia, the concentration of the reaction ammonia at each point in the axial direction in the reaction tube is kept approximate, the conversion rate of ammonolysis reaction in the reaction tube can be ensured, and meanwhile, the local overheating of the reaction tube is avoided.
3. When the ammonolysis reactor provided by the invention is used, liquid phase ester forms liquid level in the liquid inlet cavity and enters the reaction tube, and liquid ammonia enters the reaction tube for countercurrent after being vaporized and uniformly distributed by the vaporization distributor, so that ammonia gas is sealed by the liquid phase ester liquid, the ammonia gas is prevented from escaping while the efficient reaction is ensured, the ammonia escape rate can be greatly reduced, the production cost is saved, and the environment is protected.
4. The amide preparation method provided by the invention is based on the ammonolysis reactor, can reduce equipment investment and equipment occupied area, so as to reduce the production cost of the amide and save land resources, can overcome the resistance of liquid phase ester in the reaction tube by the pressure of liquid ammonia after vaporization, keep the concentration of ammonia in the reaction tube at each point in the axial direction approximately, can ensure the conversion rate of ammonolysis reaction in the reaction tube, can avoid local overheating of the reaction tube, can greatly reduce the ammonia escape rate, saves the production cost and protects the environment.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present application and therefore should not be considered limiting the scope, and that other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of a conventional preparation system for preparing amide based on serial ammonolysis of a plurality of stirring reaction kettles;
FIG. 2 is a schematic diagram of an ammonolysis reactor according to an embodiment of the invention;
FIG. 3 is an enlarged schematic view of portion A of FIG. 2;
FIG. 4 is a schematic diagram of a vaporization distributor according to an embodiment of the present invention;
fig. 5 is a schematic structural diagram of a pulse distribution tube according to an embodiment of the present invention.
Reference numerals:
10-a reaction kettle, 11-a stirrer and 12-an aging tank;
20-a shell, 21-a liquid inlet cavity, 211-a liquid level detection interface, 22-a liquid phase ester feeding nozzle, 23-an exhaust nozzle, 24-a reaction cavity, 25-a liquid outlet cavity, 26-a product discharging nozzle, 27-a liquid ammonia feeding nozzle, 28-a cooling working medium inlet and 29-a cooling working medium outlet;
30-reaction tube, 31-overflow;
40-vaporization distributor, 41-liquid-lowering channel, 42-pulse distributing pipe;
50-a first liquid phase distributor;
60-a second liquid phase distributor;
70-demister.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. The indicated azimuth or position relationship is based on the azimuth or position relationship shown in the drawings, or is the azimuth or position relationship which is placed conventionally when the application product is used, or is the azimuth or position relationship which is understood conventionally by a person skilled in the art. The terms "disposed," "configured," "mounted," "connected," "coupled," and "connected" are to be construed broadly.
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 definition or explanation thereof is necessary in the following figures. And the embodiments and features of the embodiments in this application may be combined with each other without conflict.
In the prior amide products, certain amides containing double bonds, such as acrylamide, can be used for preparing polyacrylamide, and the polyacrylamide is a water-soluble high polymer and can be used as a drag reducer for reducing friction force in liquid in the process of transporting petroleum pipes.
In addition, amide herbicides such as dimethenamid, flufenacet, thiabendazole, clethodim and the like are available as herbicides in agricultural fields, and in recent years, the use amount and the use area of amide herbicides have been increased to be inferior to those of organophosphorus herbicides. Long-chain amide can be used as surfactant added into detergents such as shampoo, bath lotion, shaving products, etc. to be used as thickener and foam stabilizer; the other active groups such as amino, carboxyl and the like can be further reacted to enhance the surface activity.
Therefore, the cost of amide formation and preparation is reduced, and the method has great technical and economic values. The common urethane ammonolysis method has the advantages of easily available raw materials and low cost; the reaction is mild and the operation is easy; the heat release amount is small, and the heat sensitive amide product is friendly, so that the heat sensitive amide product becomes the most main amide synthesis process flow. However, in the prior art, the ester ammonolysis method adopts a preparation system (as shown in fig. 1) in which a plurality of kettle reactors with stirrers are connected in series, so that the equipment investment and the occupied area are large. In view of this, the present invention provides an ammonolysis reactor and a method for producing amide, see in particular the following examples:
example 1
Referring to fig. 2, this embodiment provides an ammonolysis reactor, which includes a vertically arranged housing 20, wherein the inner cavity of the housing 20 is divided into a liquid inlet cavity 21, a reaction cavity 24 and a liquid outlet cavity 25 from top to bottom in sequence; the liquid inlet cavity 21 is adapted with a liquid phase ester feeding nozzle 22, and the top of the liquid inlet cavity 21 is provided with an exhaust nozzle 23; the reaction chamber 24 is adapted with a cooling working medium circulation system, a plurality of reaction tubes 30 are arranged in the reaction chamber 24, and the reaction tubes 30 are communicated with the liquid inlet chamber 21 and the liquid outlet chamber 25; a vaporization distributor 40 is arranged in the liquid outlet cavity 25, each air outlet end of the vaporization distributor 40 is connected with the lower end of the corresponding reaction tube 30, and the lower end of the reaction tube 30 is provided with an overflow channel 31; the lower end of the liquid outlet cavity 25 is provided with a product discharging nozzle 26 and an ammonia liquid feeding nozzle, and the ammonia liquid feeding nozzle is connected with the feeding end of the vaporization distributor 40.
Specifically, the liquid-phase ester feed nozzle 22 is connected to the liquid-phase ester supply means such that the liquid-phase ester enters the liquid-intake chamber 21 through the liquid-phase ester feed nozzle 22 to form a liquid level in the liquid-intake chamber 21. Because the reaction tube 30 communicates with the liquid inlet chamber 21 and the liquid outlet chamber 25, a part of the liquid phase ester enters the reaction tube 30 by gravity and forms a continuous liquid phase to fill the entire reaction tube 30.
In order to detect the liquid level of the liquid lipid in the liquid inlet cavity 21 and ensure that the ammonolysis reaction is fully performed, a liquid level detection interface 211 is further arranged on the side wall of the liquid inlet cavity 21, and two liquid level detection interfaces 211 are generally arranged at intervals in the height direction of the liquid inlet cavity 21 so as to judge whether the liquid level in the liquid inlet cavity 21 is in a set range.
To facilitate connection to a cooling medium circulation system, the reaction chamber 24 is fitted with a cooling medium inlet 28 and a cooling medium outlet 29; the cooling medium inlet 28 is located at the lower end of the reaction chamber 24, and the cooling medium outlet 29 is located at the upper end of the reaction chamber 24, so that the cooling medium sufficiently cools the reaction tube 30, thereby removing heat through the cooling medium, facilitating the ammonolysis reaction, ensuring the conversion rate and reducing the safety risk.
For the cooling medium in the cooling medium circulation system, the cooling medium circulation system is determined according to the optimal reaction temperature, the adiabatic reaction temperature rise, the reactant heat sensitivity, the influence degree of the temperature on side reaction and other factors, such as the introduction of a refrigerant such as circulating cooling water, chilled water, heat conducting oil, boiler water, steam and the like, and a flow-around component such as a baffle plate and the like can be arranged in the shell 20 for enhancing heat transfer, so that the cooling medium is fully contacted with the reaction tube 30.
The vaporization distributor 40 may be a normal temperature distributor which can vaporize and feed the liquid ammonia into each reaction tube 30, and has a low temperature required for vaporization of the liquid ammonia and releases heat in the ammonolysis reaction. The upper end of the distributor is provided with a plurality of air outlets which are connected with the corresponding reaction pipes 30, so that liquid can be discharged from overflow channels 31 at the lower ends of the reaction pipes 30.
When the ammonolysis reactor provided by the embodiment is used, liquid-phase ester enters the liquid inlet cavity 21 through the liquid-phase ester feed nozzle 22, meanwhile, a cooling working medium is circularly fed into the reaction cavity 24 through a cooling working medium circulation system matched with the reaction cavity 24, the reaction cavity 24 is cooled, and liquid ammonia is vaporized by the vaporization distributor 40 in the liquid outlet cavity 25 and then enters the reaction tube 30, so that ammonia is in countercurrent in the reaction tube 30, and the ammonolysis reaction is efficient. The product generated by the reaction is discharged to the bottom of the liquid outlet cavity 25 through the overflow channel 31 at the lower end of the reaction tube 30, is discharged and collected through the product discharge nozzle 26 at the bottom of the liquid outlet cavity 25, and the gas which is not completely reacted is discharged through the gas discharge nozzle 23 at the top of the liquid inlet cavity 21.
Therefore, the liquid level in the liquid inlet cavity 21 is controlled by a valve on a pipeline of the product discharge nozzle 26, and can be regulated according to the static pressure head of the liquid ammonia for feeding, so that the reaction is ensured to be carried out efficiently; the pressure of the ammonolysis reaction is precisely controlled by controlling the pressure of the pipeline of the exhaust nozzle 23.
In summary, the ammonolysis reactor provided in this embodiment does not need to connect a plurality of reaction kettles 10 in series, and the reactor shell 20 is vertically arranged, so that investment of equipment can be reduced, the occupied area of the equipment is reduced, the production cost of amide is reduced, and land resources are saved; the liquid ammonia enters the reaction tube 30 for countercurrent after being vaporized and uniformly distributed by the vaporization distributor 40, the resistance of liquid phase ester in the reaction tube 30 can be overcome by the pressure of the vaporized liquid ammonia, the concentration of the ammonia in the reaction tube 30 for each point in the axial direction is kept approximate, the conversion rate of ammonolysis reaction in the reaction tube 30 can be ensured, and meanwhile, the local overheating of the reaction tube 30 is avoided; liquid phase ester feeding forms the liquid level in feed liquor chamber 21 to be full of reaction tube 30, in order to seal ammonia through liquid phase ester liquid, prevent ammonia escape when guaranteeing that the reaction is gone on with high efficiency, can reduce ammonia escape rate by a wide margin, not only practice thrift manufacturing cost, but also can protect the environment.
Example 2
Referring to fig. 2, this embodiment provides an ammonolysis reactor, based on the structure and principle described in embodiment 1, a first liquid phase distributor 50 is disposed at the upper portion of the liquid inlet chamber 21, and the liquid inlet end of the first liquid phase distributor 50 is connected to the discharge end of the liquid phase ester feeding nozzle 22, so as to disperse the liquid phase ester entering the liquid inlet chamber 21, and thus absorb the ammonia gas penetrating the liquid level.
Further, a second liquid phase distributor 60 is further disposed at the upper portion of the liquid inlet cavity 21, and the second liquid phase distributor 60 is located below the first liquid phase distributor 50 to disperse the liquid phase ester dispersed in the first liquid phase distributor 50, so as to form droplets with smaller particle diameters, thereby increasing the contact area between the liquid phase ester and ammonia, improving the reaction efficiency and the capture rate of ammonia penetrating through the liquid level, and further reducing the escape rate of ammonia.
It will be appreciated that the first liquid distributor 50 may be a primary distributor, and may be a straight pipe or a circular pipe with a mesh, or a distributor plate. When the distribution plate is used as the first liquid-phase distributor 50, it is necessary to ensure that an air passage is provided between the first liquid-phase distributor 50 and the side wall of the liquid inlet chamber 21 or the first liquid-phase distributor 50 itself, so that the gas which is not completely reacted can be discharged out of the housing 20, and the production safety is ensured.
For the second liquid-phase distributor 60, a structure capable of forming liquid-phase ester into mist drops, such as a fine-pore screen, is adopted, so that the liquid flow passes through the second liquid-phase distributor 60 to form continuous mist droplets with the diameter less than or equal to 2mm, the contact area between the liquid-phase distributor and ammonia gas penetrating through the liquid level of the liquid inlet cavity 21 is increased, and the ammonia gas escape is reduced.
Example 3
In connection with fig. 2, this embodiment provides an ammonolysis reactor, based on the structure and principle described in embodiment 1 or 2, a foam remover 70, such as a mesh-plate foam remover 70, a wire-mesh foam remover 70, a sponge foam remover 70, etc., is adapted to the upper portion of the liquid inlet chamber 21 to break bubbles through the foam remover 70, so as to avoid that the gas discharged from the gas outlet nozzle 23 brings liquid phase ester out of the reactor.
It should be noted that, the demister 70 should be disposed at the air inlet end of the air outlet nozzle 23, that is, when the first liquid phase distributor 50 is disposed in the liquid inlet chamber 21, the demister 70 is located above the first liquid phase distributor 50.
Example 4
In combination with fig. 3 and 4, this embodiment provides an ammonolysis reactor, and the vaporization distributor 40 has a butterfly-shaped box-type structure based on the structure and principle described in any one of embodiments 1-3, so as to ensure that the liquid ammonia is vaporized in the distributor and uniformly distributed to each outlet.
It should be appreciated that the vaporization distributor 40 adopts a disc-shaped box type structure, and the distributor gradually flattens from the center along the radial direction to ensure that the gas phase speeds at all positions are equal, so that the vaporization pressures at all points with different distances from the center position in the distributor are the same, the flow is the same, and the problem of bias flow in the reaction tube 30 is avoided.
On this basis, the vaporization distributor 40 is vertically provided with a plurality of liquid-dropping channels 41, so as to ensure that the liquid amide generated by the reaction smoothly enters the bottom of the liquid outlet cavity 25 through the vaporization distributor 40 and does not contact with the gas-liquid phase ammonia raw material in the vaporization distributor 40.
Referring to fig. 4, the liquid outlet end of the vaporizing distributor 40 is connected with a plurality of pulse distribution pipes 42, and the gas outlet end of the pulse distribution pipes 42 is connected with the lower end of the reaction pipe 30, so as to connect the vaporizing distributor 40 and the reaction pipe 30 through pulse distribution. To simplify the structure of the reaction tube 30, the upper end of the pulse distribution tube 42 is in clearance fit with the lower end of the reaction tube 30, and the clearance between the upper end of the pulse distribution tube 42 and the lower end of the reaction tube 30 is used as the spillway 31.
Referring to fig. 5, the outlet of the pulse distribution pipe 42 is a necking port, so as to increase the initial velocity of the ammonia gas entering the reaction pipe 30, increase the distribution rate of the ammonia gas in the reaction pipe 30, and effectively prevent the liquid phase ester from flowing backward from the inlet of the pulse distribution pipe 42 into the vaporization distributor 40.
According to the vaporization distributor 40 provided by the embodiment, when liquid ammonia enters the vaporization distributor 40 to vaporize and uniformly distribute the liquid ammonia to each pulse branch pipe, ammonia is accelerated by the pulse branch pipes and then is sent into the reaction pipe 30, so that the ammonia in the reaction pipe 30 can be axially lifted and uniformly distributed along with the reaction pipe 30; and the liquid ammonia is vaporized and is in countercurrent contact in the reaction tube 30 for ammonolysis reaction after pulse acceleration, the liquid phase is continuous phase and fills the whole reaction tube 30, the gas phase is pushed by pressure to move upwards along the axial direction as a disperse phase, the thrust of the disperse phase in the reactor can be controlled by controlling the pressure of a gas phase pipeline at the outlet of the reactor, the consistent reaction depth of each axial point in the reaction tube 30 is satisfied, and the reaction efficiency is fully improved.
Example 5
The present example provides a process for the preparation of amides, based on the ammonolysis reactor and ammonolysis process provided by the previous implementation, comprising the following steps:
s1, feeding liquid phase amide into a liquid inlet cavity 21 at the upper end of a reactor shell 20, wherein the shell 20 is vertically arranged, the inner cavity of the shell 20 is sequentially divided into the liquid inlet cavity 21, a reaction cavity 24 and a liquid outlet cavity 25 from top to bottom, and the liquid inlet cavity 21 is communicated with the liquid outlet cavity 25 through a reaction tube 30 inserted into the reaction cavity 24.
Specifically, the liquid-phase ester feed nozzle 22 is connected with the liquid-phase ester supply device, so that the liquid-phase ester enters the liquid inlet cavity 21 through the liquid-phase ester feed nozzle 22 to form a liquid level in the liquid inlet cavity 21; because the reaction tube 30 communicates with the liquid inlet chamber 21 and the liquid outlet chamber 25, a part of the liquid phase ester enters the reaction tube 30 by gravity and forms a continuous liquid phase to fill the entire reaction tube 30.
S2, connecting a cooling system with the reaction cavity 24, and cooling the reaction tube 30 through a cooling working medium.
Specifically, the cooling medium in the cooling medium circulation system is determined according to various factors such as optimal reaction temperature, adiabatic reaction temperature rise, reactant heat sensitivity, influence degree of temperature on side reaction, and the like, for example, coolant such as circulating cooling water, chilled water, heat conducting oil, boiler water, steam, and the like is introduced, and a flow-around component such as a baffle plate can be arranged in the shell 20 for enhancing heat transfer, so that the cooling medium is fully contacted with the reaction tube 30.
S3, sending liquid-phase ammonia into a vaporization distributor 40 in the liquid outlet cavity 25, and sending the liquid-phase ammonia into the reaction tube 30 through the vaporization distributor 40 for ammonolysis reaction to generate amide.
Specifically, the liquid ammonia is vaporized by the vaporization distributor 40 in the liquid outlet cavity 25 and then enters the reaction tube 30, so that the ammonia gas is countercurrent in the reaction tube 30, and the efficient ammonolysis reaction is realized.
In order to facilitate understanding of the beneficial technical effects of the present embodiment, experimental comparison is performed with specific production examples and comparative examples, and the following are specific:
production example:
based on the ammonolysis reactor (figure 2), 2.0MPa (G), about 2700kg/h of raw material liquid ammonia at 30 ℃ enters a vaporization distributor 40 from a liquid ammonia feeding nozzle 27, is vaporized by the vaporization distributor 40 and enters the bottom of a countercurrent reaction tube 30 from a pulse distribution tube 42; about 9500kg/h of methyl formate at the temperature of 0.3MPa (G) and 30 ℃ enters the first liquid-phase distributor 50 from the liquid-phase ester feed inlet, and then the methyl formate is dispersed into uniform small liquid drops with the diameter less than or equal to 2mm through the second liquid-phase distributor 60, and the reaction tube 30 is gradually filled to form the liquid level in the liquid inlet cavity 21. The reaction products flow downwardly by gravity to the bottom of the feed chamber 21 and are discharged through the product discharge nozzle 26. Meanwhile, circulating cooling water at 32 ℃ and 0.4MPa (G) enters the reaction cavity 24 from the cooling working medium inlet 28, and 0.35MPa (G) leaves the reaction cavity 24 from the cooling working medium outlet 29 at 40 ℃.
Wherein the formamide reactor capacity is about 7200kg/h, the reactor dimensions are as follows: the reactor tube 30 (9 m high in the countercurrent reaction section) had an inner diameter of 1.8 m. The per pass conversion in the reaction is about 98.3 percent, and the ammonia escape rate is less than or equal to 0.1 percent (wt%). The amount of circulating cooling water is about 340t/h.
Comparative example:
based on the prior multistage kettle type ammonolysis reactor for producing formamide, three kettle type serial ammonolysis reactors and one aging tank 12 are arranged in combination with fig. 1, the kettle type ammonolysis reactors are provided with an electric stirrer 11, a cooling water jacket and a chilled water sleeve, and the aging tank 12 is a horizontal container.
2.0MPa (G), about 2000kg/h of raw material liquid ammonia at 30 ℃ enters the primary reaction kettle 10 from a liquid ammonia feeding pipeline, 0.3MPa (G), about 9500kg/h of raw material methyl formate at 30 ℃ enters the primary reaction kettle 10 from a methyl formate feeding pipeline, raw materials are mixed in the primary reaction kettle 10 and continuously stirred by a stirrer 11, meanwhile, an outside cooling water jacket is filled with 32 ℃ and 0.4MPa (G) circulating cooling water, an inside chilled water sleeve is filled with 0 ℃ and 0.4MPa (G) chilled water is used for heat transfer.
The reaction mixture flows into the secondary reaction kettle 10 from the outlet of the primary reaction kettle 10, and at the same time, about 700kg/h of liquid ammonia enters the secondary reaction kettle 10 from a liquid ammonia feeding pipeline, the secondary reaction kettle 10 is also stirred by a stirrer 11, cooling water and chilled water are used for heat transfer, the reaction mixture flows into the final reaction kettle 10 from the outlet of the secondary reaction kettle 10, the final reaction kettle 10 is stirred by the stirrer 11, the cooling water and the chilled water are used for heat transfer, and the reaction is sent into an aging tank 12 from an outlet pipeline for standing and aging, so that the whole reaction process is completed.
Wherein, in order to reduce ammonia escape during the reaction, a nitrogen pressurizing pipeline is added at the upper part of the reactor.
This comparative example was about 7200kg/h of formamide reaction scheme, the reactor dimensions were as follows: the volumes of the three reaction kettles 10 are 40m 3 The inner diameter is about 2.8 meters and the height is about 6.5 meters. The volume of the aging tank 12 is about m 3 The inner diameter is about 3 meters and the tangential line is about 13.2 meters long. The conversion per pass in the reaction is about 98.5 percent, and the ammonia escape rate is less than or equal to 1 percent (wt%). The consumption of circulating cooling water is about 120t/h, and the consumption of chilled water is about 280t/h.
In comparison, the method and the device for extracting work in the embodiment have equivalent single-pass conversion rate in the reaction, and the ammonia escape rate is one tenth of that in the prior art.
In summary, the ammonolysis reactor provided in this embodiment does not need to connect a plurality of reaction kettles 10 in series, and the reactor shell 20 is vertically arranged, so that investment of equipment can be reduced, the occupied area of the equipment is reduced, the production cost of amide is reduced, and land resources are saved; greatly reduces the ammonia escape rate, saves the production cost and protects the environment.
The foregoing description is only of the preferred embodiments of the invention, and is not intended to limit the invention in any way, but is intended to cover all modifications, equivalents, improvements and alternatives falling within the spirit and principles of the invention.

Claims (5)

1. The ammonolysis reactor is characterized by comprising a shell (20) which is vertically arranged, wherein the inner cavity of the shell (20) is sequentially divided into a liquid inlet cavity (21), a reaction cavity (24) and a liquid outlet cavity (25) from top to bottom;
the liquid inlet cavity (21) is adapted with a liquid phase ester feeding nozzle (22), and the top of the liquid inlet cavity (21) is provided with an exhaust nozzle (23);
the reaction cavity (24) is adapted with a cooling working medium circulating system, a plurality of reaction pipes (30) are arranged in the reaction cavity (24), and the reaction pipes (30) are communicated with the liquid inlet cavity (21) and the liquid outlet cavity (25);
a vaporization distributor (40) is arranged in the liquid outlet cavity (25), each air outlet end of the vaporization distributor (40) is connected with the lower end of the corresponding reaction tube (30), and an overflow channel (31) is arranged at the lower end of the reaction tube (30);
the lower end of the liquid outlet cavity (25) is provided with a product discharging nozzle (26) and an ammonia liquid feeding nozzle, and the ammonia liquid feeding nozzle is connected with the feeding end of the vaporization distributor (40);
the liquid outlet end of the vaporization distributor (40) is connected with a plurality of pulse distribution pipes (42), and the gas outlet end of the pulse distribution pipes (42) is connected with the lower end of the reaction pipe (30);
the upper part of the liquid inlet cavity (21) is provided with a first liquid phase distributor (50), and the liquid inlet end of the first liquid phase distributor (50) is connected with the discharge end of the liquid phase ester feed nozzle (22);
the vaporization distributor (40) is of a butterfly box type structure;
the outlet of the pulse distribution pipe (42) is a necking port;
the upper end of the pulse distribution pipe (42) is in clearance fit with the lower end of the reaction pipe (30), a clearance between the upper end of the pulse distribution pipe (42) and the lower end of the reaction pipe (30) is used as an overflow channel (31), and a product generated by the reaction enters the overflow channel (31) at the lower end of the reaction pipe (30) and is discharged to the bottom of the liquid outlet cavity (25);
the vaporization distributor (40) is vertically provided with a plurality of liquid dropping channels (41) so as to ensure that liquid amide generated by the reaction smoothly enters the bottom of the liquid outlet cavity (25) through the vaporization distributor (40) and does not contact with the gas-liquid phase ammonia raw material in the vaporization distributor (40);
the liquid phase ester feed forms a liquid level in the liquid inlet chamber (21) and fills the reaction tube (30) to seal ammonia gas liquid through the liquid phase ester.
2. Ammonolysis reactor according to claim 1, characterized in that the upper part of the liquid inlet chamber (21) is further provided with a second liquid phase distributor (60), the second liquid phase distributor (60) being located below the first liquid phase distributor (50).
3. Ammonolysis reactor according to claim 1 or 2, characterized in that the upper part of the feed chamber (21) is fitted with a demister (70).
4. Ammonolysis reactor according to claim 1, characterized in that the reaction chamber (24) is adapted with a cooling medium inlet (28) and a cooling medium outlet (29);
the cooling working medium inlet (28) is positioned at the lower end of the reaction cavity (24), and the cooling working medium outlet (29) is positioned at the upper end of the reaction cavity (24).
5. A process for producing an amide using the ammonolysis reactor according to claim 1, comprising the steps of:
s1, delivering liquid-phase amide into a liquid inlet cavity (21) at the upper end of a reactor shell (20), wherein the shell (20) is vertically arranged, the inner cavity of the shell (20) is sequentially divided into the liquid inlet cavity (21), a reaction cavity (24) and a liquid outlet cavity (25) from top to bottom, and the liquid inlet cavity (21) and the liquid outlet cavity (25) are communicated through a reaction tube (30) inserted into the reaction cavity (24);
s2, connecting a cooling system with the reaction cavity (24), and cooling the reaction tube (30) through a cooling working medium;
s3, delivering liquid-phase ammonia into a vaporization distributor (40) in the liquid outlet cavity (25), and delivering the liquid-phase ammonia into the reaction tube (30) through the vaporization distributor (40) to carry out ammonolysis reaction to generate amide.
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