CN114100168A - Reactive distillation device and method for producing peroxycarboxylic acid - Google Patents
Reactive distillation device and method for producing peroxycarboxylic acid Download PDFInfo
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- CN114100168A CN114100168A CN202010904683.9A CN202010904683A CN114100168A CN 114100168 A CN114100168 A CN 114100168A CN 202010904683 A CN202010904683 A CN 202010904683A CN 114100168 A CN114100168 A CN 114100168A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C407/00—Preparation of peroxy compounds
- C07C407/003—Separation; Purification; Stabilisation; Use of additives
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Abstract
The invention relates to the technical field of rectification, and discloses a reactive rectification device and a preparation method of peroxycarboxylic acid, wherein the reactive rectification device comprises a reactor and a rectification tower, a reaction chamber for reacting a reaction material and a heat exchange chamber separated from the reaction chamber are arranged in the reactor, the heat exchange chamber can be communicated with a heat exchange medium for exchanging heat with the reaction material, and the reactor is provided with a material inlet for allowing the reaction material to enter the reaction chamber and a material outlet for discharging a mixture containing a product material obtained by reaction; the rectifying tower is arranged to be communicated with the material outlet and can separate the received mixture. The reaction rectifying device is provided with a reactor for reacting reaction materials and a rectifying tower capable of separating a mixture containing product materials obtained by reaction, so that continuous production is realized, the products are separated in time, and side reactions are reduced.
Description
Technical Field
The invention relates to the technical field of rectification, in particular to a reactive rectification device and a preparation method of peroxycarboxylic acid.
Background
The peroxycarboxylic acids are generally obtained by reacting the corresponding anhydrides with hydrogen peroxide in the presence of a catalyst. At present, the peroxycarboxylic acid is produced by an intermittent mode basically, however, the intermittent mode has low efficiency, a plurality of byproducts and an unstable reaction process.
Disclosure of Invention
The invention aims to provide a reaction rectifying device which is provided with a reactor for reacting reaction materials and a rectifying tower capable of separating a mixture containing product materials obtained by reaction, so that continuous production is realized, the products are separated in time, the reaction stability is improved, and side reactions are reduced.
In order to achieve the above object, an aspect of the present invention provides a reactive distillation apparatus comprising:
the reactor is internally provided with a reaction chamber for reacting a reaction material and a heat exchange chamber separated from the reaction chamber, the heat exchange chamber can be communicated with a heat exchange medium for exchanging heat with the reaction material, and the reactor is provided with a material inlet for allowing the reaction material to enter the reaction chamber and a material outlet for discharging a mixture containing a product material obtained by the reaction; and
the rectifying tower is set to be communicated with the material outlet and can separate the received mixture.
Above-mentioned technical scheme, through setting up the reactor and the rectifying column that is linked together with the reactor, wherein set up reaction chamber and the heat transfer cavity that separates each other in the reactor, thereby can make reaction material react in order to obtain the mixture that contains the product material in the reactor, and the mixture that contains the product material that the reaction obtained in time enters into the rectifying column and carries out the rectification separation, like this, can let in reaction material in order to react in succession to the reactor, not only realize serialization production, reaction efficiency is improved, and because the product can in time be discharged into the rectifying column and carry out the rectification separation, whole reaction process controllable degree is high, the reaction is stable, the side reaction is less, product purity and yield have been improved.
Preferably, the rectifying tower comprises a shell and a separation layer arranged in the shell, and an inlet which can be communicated with the material outlet so that the mixture flows to the separation layer is arranged on the shell.
Preferably, the reactor is provided with a return port communicated with the reaction chamber;
the shell is provided with an outlet through which materials accumulated in the separation layer can be discharged, and the outlet is communicated with the return port.
Preferably, a group of inlets and a group of outlets corresponding to the separation layer are arranged on the shell, wherein the group of inlets comprises a plurality of inlets, and the group of outlets comprises a plurality of outlets respectively corresponding to the corresponding inlets;
the reactive distillation device comprises a group of reactors, each group of reactors comprises a plurality of reactors, the material outlets of the reactors are communicated with the corresponding inlets, and the return ports of the reactors are communicated with the corresponding outlets.
Preferably, the rectifying tower comprises a plurality of separating layers which are distributed at intervals along the height direction of the shell, and the shell is provided with a plurality of groups of inlets and a plurality of groups of outlets which respectively correspond to the corresponding separating layers;
the reactive distillation device comprises a plurality of groups of reactors corresponding to the corresponding separating layers respectively, the material outlets of the reactors in the same group of reactors are communicated with the corresponding inlets in the same group of inlets, and the return ports of the reactors are communicated with the corresponding outlets in the same group of outlets.
Preferably, a plurality of said reactors in the same set of reactors are arranged around the same said separation layer.
Preferably, the spacing between adjacent separating layers is 0.1-0.5 of the height of the shell.
Preferably, the reactor comprises a reactor shell and a plurality of tubes disposed within the reactor shell, wherein: the material inlet, the material outlet and the return port are all arranged in the reactor shell, two ends of the pipe are respectively communicated with the material inlet and the material outlet, the pipe is communicated with the return port, the inner space of the pipe is formed into the reaction chamber, and the inner space of the reactor shell is formed into the heat exchange chamber.
Preferably, a catalyst layer capable of promoting the reaction of the reaction materials is arranged in the tube; or
A catalyst layer capable of promoting the reaction of the reaction materials is arranged in the tube, wherein: the thickness of the catalyst layer is 0.2-0.8 of the length of the respective tube.
In a second aspect, the present invention provides a process for the preparation of peroxycarboxylic acids comprising the steps of:
step S10: mixing a first reactant and a second reactant to form a reaction mass, wherein; the first reactant is one or more of carboxylic acid and anhydride, and the second reactant is an oxidant;
step S20: exchanging heat with the reaction material to enable the reaction material to reach a preset temperature, and reacting under the condition of the preset temperature to obtain a mixture containing peroxycarboxylic acid;
step S30: the mixture containing peroxycarboxylic acid obtained in step S20 is subjected to rectification.
Preferably, the carboxylic acid is R-COOH, wherein: r is hydrogen or alkyl with 1-10 carbon atoms;
the acid anhydride is formic anhydride or R1-CO-O-CO-R2Wherein: r1Is alkyl with 1-10 carbon atoms, R2Is alkyl with 1-10 carbon atoms;
the oxidant is peroxide.
Preferably, in the step S20, the feeding flow rate of the reaction materials is 10-1000 kg/h.
Preferably, in the step S20, the preset temperature is 40-100 ℃; and/or
In the step S20, the reaction mass is reacted under the action of a catalyst, wherein: the catalyst is a solid acid.
Preferably, in the step S30, the material stored in the rectification is returned to the step S20 to continue the reaction.
Preferably, in the step S30, when the rectification operation is performed, the reflux ratio is set to 2 to 10; and/or
In the step S10, the reaction materials are divided into a plurality of groups to be reacted separately.
Preferably, in the step S20, the reaction mass is reacted under the pressure condition of 1-50 kPa; and/or
In the step S30, the rectification operation is performed under the pressure condition of 1-50 kPa.
Drawings
FIG. 1 is a schematic view of the overall structure of a reactive distillation apparatus according to a preferred embodiment of the present invention.
Description of the reference numerals
10-a reactive distillation device; 12-a rectification column; 120-a separation layer; 122-a housing; 124-a condenser; 14-a reactor; 160-product takeoff line; 161-return line; 162-a feed line; 163-light fraction takeoff line; 164-a return line; 165-return line; 166-bottom export line.
Detailed Description
In the present invention, the use of directional terms such as "upper, lower, left and right" in the absence of a contrary explanation generally means that the directions shown in the drawings and the practical application are considered to be the same, and "inner and outer" mean the inner and outer of the outline of the component.
The present invention provides a reactive distillation apparatus, as shown in fig. 1, a reactive distillation apparatus 10 includes a reactor 14 and a distillation column 12. Wherein, a reaction chamber for reacting the reaction materials and a heat exchange chamber separated from the reaction chamber are arranged in the reactor 14, the heat exchange chamber can be circulated with a heat exchange medium for exchanging heat with the reaction materials, for example, a heat exchange medium such as steam or a liquid with a certain temperature can exchange heat with the reaction material to heat the reaction material after entering the heat exchange chamber, so that the reaction material reaches a preset temperature, reacting the reaction mass at a predetermined temperature to obtain a mixture containing a product material such as peroxycarboxylic acid, it can be understood that the reactor 14 is provided with a heat exchange medium inlet and a heat exchange medium outlet for the heat exchange medium to enter and exit the heat exchange chamber respectively, in addition, the reactor 14 is provided with a material inlet for the reaction material to enter the reaction chamber and a material outlet for discharging the mixture containing the product material obtained by the reaction; the rectifying column 12 is arranged to be able to communicate with the material outlet, the rectifying column 12 being able to separate the received mixture, so that the mixture discharged from the material outlet can be separated and purified in the rectifying column 12 to obtain the product material (heavy component) and the light component, such as unreacted reaction material. Through setting up reactor 14 and the rectifying column 12 that is linked together with reactor 14, wherein set up reaction chamber and the heat transfer cavity that separates each other in reactor 14, thereby can make reaction material react in reactor 14 in order to obtain the mixture that contains the product material, and the mixture that contains the product material that the reaction obtained in time enters into rectifying column 12 and carries out the rectification separation, like this, can let in reaction material in reactor 14 in succession in order to react, not only realize serialization production, the reaction efficiency is improved, and because the product can in time be discharged into rectifying column 12 and carry out the rectification separation, whole reaction sequence controllable degree is high, the reaction is stable, the side reaction is less, product purity and productivity have been improved. The reactive distillation apparatus 10 is particularly suitable for the production of peroxycarboxylic acids. When the reaction rectification apparatus 10 is used to produce peroxycarboxylic acid, the peroxycarboxylic acid obtained by the reaction is a heavy component, and an oxidizing agent such as hydrogen peroxide is a light component.
In addition, the pressure in the reactor 14 may be adjusted so that a preset pressure is provided in the reactor 14, that is, a certain pressure state may be maintained in the reactor 14; preferably, the pressure in the reactor 14 may be made to be 1 to 50 kPa; further preferably, the pressure in the reactor 14 may be made to be 3 to 40 kPa; even more preferably, the pressure in the reactor 14 may be made to be 10-25 kPa.
The rectification column 12 may include a shell 122 and a separation layer 120 disposed in the shell 122, the separation layer 120 may be a packing layer or a tray, the shell 122 is provided with an inlet capable of communicating with the material outlet, the inlet is capable of allowing the mixture to flow to the separation layer 120, and thus, the mixture obtained by the reaction may be discharged onto the separation layer 120 for separation. Here, the position of the inlet is not particularly limited as long as the mixture can be guided to the separation layer 120, and for example, the inlet may be disposed above the bottom wall of the separation layer 120. It will be appreciated that a product outlet line 160 may be provided connecting the inlet and the material outlet; in addition, after the mixture reaches the separation layer 120, under the condition that the heat source is provided in the rectifying column 12, for example, the temperature in the rectifying column 12 may be set to 40 to 80 ℃, the product material separated from the mixture, i.e., the heavy components, may flow toward the bottom of the rectifying column 12 through the holes provided in the separation layer 120, and the separated light components may flow toward the top of the rectifying column 12 through the holes provided in the separation layer 120, and in addition, unreacted reaction materials may be accumulated on the separation layer 120.
In order to better rectify the rectified gas in the rectification column 12, the pressure in the shell 122 may be adjusted to make the shell 122 have a preset pressure, that is, a certain pressure state may be maintained in the shell 122; preferably, the pressure in the housing 122 may be made to be 1-50 kPa; further preferably, the pressure in the housing 122 may be made to be 3-40 kPa; still more preferably, the pressure within the housing 122 may be made to be 10-25 kPa. Preferably, the pressure within the shell 122 may be maintained consistent with the pressure within the reactor 14.
It should be noted that a product discharge outlet may be provided at the bottom of the housing 122, and correspondingly, a bottom outlet conduit 166 may be provided at the product discharge outlet for discharging separated product material, i.e., heavies; in addition, a light component discharge port may be provided at the top of the housing 122 to discharge the separated light component.
Furthermore, a condenser 124 may be provided outside the casing 122, the condenser 124 may cool the light components discharged from the rectifying column 12, the light components may be led out into the condenser 124 through a light component lead-out line 163, the light component lead-out line 163 may be provided at a light component outlet, a part of the condensate condensed by the condenser 124 is introduced into the rectifying column 12 as reflux through a reflux line 161, and the remaining condensate may be introduced into the corresponding reactor 14 through a return line 165 to participate in the reaction as a reaction material.
In addition, a return port communicating with the reaction chamber may be provided on the reactor 14; accordingly, an outlet port through which the material accumulated in the separation layer 120 can be discharged may be provided in the casing 122, and the outlet port is communicated with the return port, so that the unreacted reaction material in the accumulated material can be returned to the reactor 14 through the return port to continue the reaction, thereby not only avoiding the waste of the material, but also reducing the interference with the separation process and improving the purity of the reaction product. It will be appreciated that a return line 164 may be provided between the return port and the outlet port communicating the return port and the outlet port. The position of the outlet is not particularly limited as long as the accumulated material can be guided out of the separation layer 120, for example, the outlet may be disposed above the bottom wall of the separation layer 120, and preferably, the outlet may be disposed below the inlet.
A set of inlets and a set of outlets corresponding to the separation layers 120 may be provided on the casing 122, that is, the same set of inlets and the same set of outlets are provided at positions of the casing 122 close to the respective separation layers 120, wherein: a set of inlets includes a plurality of said inlets and a set of outlets includes a plurality of said outlets respectively corresponding to respective said inlets.
The reactive distillation apparatus 10 may comprise a set of reactors, which may comprise a plurality of reactors 14, said material outlets of the reactors 14 being in communication with respective said inlets, and said return ports of the reactors 14 being in communication with respective said outlets, it being understood that in the same set of reactors, said material outlet of each reactor 14 may be in communication with a respective inlet of the same set, and said return port of each reactor 14 may be in communication with a respective outlet of the same set. Through the arrangement of the group of reactors which can be communicated with the same separation layer 120, reaction materials can be divided into a plurality of parts, and each part of reaction materials can enter the corresponding separation layer 120 after reacting in the corresponding reactor 14 to obtain a mixture containing product materials, so that the reaction stability of the reaction materials is further improved, the side reactions are reduced, and the mixtures obtained by the reaction can enter the rectifying tower 12 respectively, so that the separation and purification efficiency and the stability of the separation and purification process can also be improved.
In order to further improve the reaction stability, as shown in fig. 1, a plurality of separation layers 120 may be provided, the plurality of separation layers 120 may be spaced apart from each other in the height direction of the casing 122, and a plurality of sets of inlets and a plurality of sets of outlets, which correspond to the respective separation layers 120, may be provided on the casing 122, and it is understood that the same set of inlets and the same set of outlets may correspond to the same separation layer 120.
The reactive distillation apparatus 10 may comprise a plurality of sets of reactors corresponding to the respective separation layers 120, the material outlets of the reactors 14 in the same set of reactors being in communication with the respective inlets in the same set of inlets, and the return ports of the reactors 14 being in communication with the respective outlets in the same set of outlets.
To facilitate the ingress and egress of materials, multiple reactors 14 in the same set of reactors may be arranged around the same separation layer 120. By having a plurality of reactors 14 in the same set of reactors arranged around the same separation layer 120, it is facilitated that not only the mixture containing the product material enters the respective separation layer 120 through the respective inlet, but also the unreacted material on the respective separation layer 120 is returned to the respective reactor 14 through the respective outlet.
The spacing between adjacent separation layers 120 is preferably 0.1-0.5 of the height of the shell 122, which allows the rectification column 12 to have a suitable number of separation layers 120 for easy operation, while improving separation efficiency and product material purity. Further preferably, the spacing between adjacent separation layers 120 is preferably 0.2-0.4 of the height of the shell 122.
The reactor 14 may include a reactor shell 140 and a plurality of tubes disposed within the reactor shell 140, wherein: the material inlet, the material outlet, and the return port may be provided in the reactor case 140, and in addition, the heat exchange medium inlet and the heat exchange medium outlet may be provided in the reactor case 140, both ends of the tube are respectively communicated with the material inlet and the material outlet, so that the reaction material enters each tube from the material inlet, the mixture containing the product material obtained after the reaction is completed is discharged from each tube and is discharged from the material outlet, and the tube is communicated with the return port, so that the material accumulated in the separation layer 120 can be discharged into each tube from the return port; wherein: the inner space of the tube may be formed as the reaction chamber and the inner space of the reactor housing 140 may be formed as the heat exchange chamber. The reaction materials enter the tubes respectively to react, so that the reactions in the tubes are mutually independent and do not interfere with each other, thereby further improving the stability of the reaction and greatly reducing the generation of side reactions.
A catalyst layer capable of promoting the reaction of the reaction materials may be disposed within the tube, wherein the catalyst may be a solid acid such as boric acid when synthesis of peroxycarboxylic acid is desired. Preferably, the thickness of the catalyst layer may be 0.2 to 0.8 of the length of the corresponding tube, that is, the thickness of the catalyst layer disposed in the corresponding tube is preferably 0.3 to 0.5 of the length of the corresponding tube, so that not only a good catalytic effect of the catalyst layer is ensured, but also the catalyst layer has a suitable height to reduce costs and space occupancy.
The invention also provides a preparation method of peroxycarboxylic acid, which can preferably utilize the reaction rectification device 10 provided by the invention to carry out reaction, and the preparation method of peroxycarboxylic acid comprises the following steps: step S10: mixing a first reactant and a second reactant to form a reaction mass, wherein; the first reactant is one or more of carboxylic acid and anhydride, and the second reactant is an oxidant; step S20: the reaction mass is brought to a predetermined temperature by heat exchange with the reaction mass, and under the predetermined temperature conditions, a mixture containing peroxycarboxylic acid is obtained, wherein the mixture further contains a light component such as the second reactant, and the molar ratio of the first reactant to the second reactant is preferably the first reactant: second reactant ═ (3-6): 1; step S30: and (4) rectifying the mixture containing the peroxycarboxylic acid obtained in the step S20 to obtain a product material, namely peroxycarboxylic acid (heavy component) and a light component, namely a second reactant. The mixture containing the peroxycarboxylic acid obtained by the reaction is rectified in time, so that the product material can be separated in time, the purity of the product is improved, and the yield is improved, for example, the yield of the peroxycarboxylic acid can reach over 90 percent, and in addition, the purity of the peroxycarboxylic acid can reach over 95 percent.
Wherein the carboxylic acid is R-COOH, wherein: r is hydrogen or alkyl with 1-10 carbon atoms, wherein, R is preferably alkanyl; further preferably, R may be an alkyl group having 1 to 5 carbon atoms, for example, R may be selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl, tert-butyl, pentyl, isopentyl, neopentyl or tert-pentyl.
In addition, the acid anhydride is formic anhydride or R1-CO-O-CO-R2Wherein: r1Is alkyl with 1-10 carbon atoms, wherein R1Preferably a chain alkyl group; further preferably, R1May be an alkyl group having 1 to 4 carbon atoms, e.g. R1Can be selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl or tert-butyl; r2Can be alkyl with 1-10 carbon atoms, wherein R2Preferably a chain alkyl group; further preferably, R2May be an alkyl group having 1 to 4 carbon atoms, e.g. R2Can be selected from methyl, ethyl, propyl, isopropyl, butyl, isobutyl, sec-butyl or tert-butyl.
The oxidizing agent may be a peroxide, for example the oxidizing agent may be hydrogen peroxide, preferably the peroxide may be added in the form of a solution, for example aqueous hydrogen peroxide may be used as the second reactant. Wherein, the concentration of the hydrogen peroxide aqueous solution is preferably 30-70% by mass, and the hydrogen peroxide aqueous solution with the concentration is selected as the second reactant, so that the stability of the reaction can be further improved, and the generation of side reactions can be reduced, and the concentration of the hydrogen peroxide aqueous solution is preferably 35-50% by mass.
In the step S10, the reaction materials are preferably divided into a plurality of groups to react respectively, that is, each group of reaction materials can react independently without interference, for example, each group of reaction materials can react in the corresponding reactor 14, thereby allowing the reaction to proceed smoothly and reducing side reactions, wherein the ratio of each group of reaction materials is not particularly limited and can be selected according to actual needs. It should be noted that the mixture containing peroxycarboxylic acid obtained after the reaction of each group of reaction materials is conducted to the distillation column 12 for separation and purification.
In the step S20, the feeding flow rate of the reaction materials is preferably 10 to 1000kg/h, and it is understood that the feeding flow rate of the reaction materials into the corresponding separation layer 120 is preferably 10 to 1000kg/h, so that the reaction can be smoothly performed without releasing excessive heat, and the entire reaction can be properly progressed, that is, the entire reaction can be completed in a proper time with good reaction efficiency. Preferably, the feeding flow rate of the reaction materials can be 80-800kg/h, and further preferably, the feeding flow rate of the reaction materials can be 120-600 kg/h.
In the step S20, the preset temperature is preferably 40 to 100 ℃, and more preferably, the preset temperature may be 40 to 80 ℃.
In step S20, the reaction mass may preferably be reacted under the action of a catalyst, wherein: the catalyst is a solid acid, for example boric acid may be used as catalyst.
In the step S20, the reaction mass may be reacted under a pressure condition of 1 to 50kPa, and the reaction is performed under such a pressure condition that not only the reaction efficiency is further improved but also the yield of the product mass obtained by the reaction is further improved, it is understood that the pressure in the reactor 14 may be maintained at 1 to 50 kPa. Further preferably, the reaction mass can be reacted under pressure conditions of 5 to 45 kPa; still more preferably, the reaction mass is reacted under pressure conditions of 10 to 30 kPa.
In the step S30, the material accumulated in the rectification can be returned to the step S20 to continue the reaction, and it should be noted that, after the mixture containing the peroxycarboxylic acid obtained in the step S20 reaches the separation layer 120, the heavy fraction of the peroxycarboxylic acid separated from the mixture flows toward the bottom of the rectification column 12 through the holes provided in the separation layer 120 under the condition that the rectification column 12 supplies the heat source, while the separated light fraction flows toward the top of the rectification column 12 through the holes provided in the separation layer 120, and unreacted reaction material is accumulated in the separation layer 120, so that the material accumulated in the rectification can be returned to the step S20 to continue the reaction, thereby improving the utilization rate of the material and further improving the purity of the product, i.e., peroxycarboxylic acid.
In step S30, when the rectification operation is performed, the reflux ratio is set to 2 to 10, so that the rectification effect can be greatly improved. Further preferably, the reflux ratio may be set to 3 to 8; still further preferably, the reflux ratio may be set to 4 to 6.
In the step S30, the rectification operation is performed under the pressure condition of 1-50kPa, and the rectification operation is performed under the pressure condition of 1-50kPa, thereby improving the separation effect. It will be appreciated that the pressure within the rectification column 12, i.e. the shell 122, may be maintained at 1-50 kPa. Further preferably, the rectification operation can be carried out under the pressure condition of 5-45 kPa; still more preferably, the rectification is carried out under a pressure of 10 to 30 kPa.
In the step S30, the rectification operation is performed at a temperature of 40 to 80 ℃.
The effects of the present invention will be further illustrated by examples.
Examples
Example 1Preparation of Peroxyacetic acid
Peroxyacetic acid was produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 20 trays are arranged in the shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, and a group of inlets and a group of outlets corresponding to the trays are arranged at the 10 th tray from the top to the bottom of the shell 122, wherein the group of inlets comprises 8 inlets, and the group of outlets comprises 8 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 8 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 5cm, the length of each pipe is 100cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing acetic anhydride and 50% by mass of aqueous hydrogen peroxide to form a reaction material, wherein the molar ratio of acetic anhydride to hydrogen peroxide in the aqueous hydrogen peroxide is acetic anhydride: hydrogen peroxide ═ 3: 1;
step S20: dividing the reaction materials into 8 parts and respectively introducing the 8 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 10kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 50 ℃, and setting the pressure in the reactors 14 to be 10kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing peroxyacetic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxyacetic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 5, the pressure in the rectification column 12 was set to 10kPa, and the temperature in the rectification column 12 was set to 40 ℃.
The purity of the obtained peroxyacetic acid is 95 percent and the yield of the peroxyacetic acid is 90 percent.
Example 2Preparation of Peroxyacetic acid
Peroxyacetic acid was produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 40 trays are arranged in the shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, and a group of inlets and a group of outlets corresponding to the trays are arranged at the 20 th tray from the top to the bottom of the shell 122, wherein the group of inlets comprises 6 inlets, and the group of outlets comprises 6 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 6 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 10cm, the length of each pipe is 50cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing acetic anhydride and 50% by mass of aqueous hydrogen peroxide to form a reaction material, wherein the molar ratio of acetic anhydride to hydrogen peroxide in the aqueous hydrogen peroxide is acetic anhydride: hydrogen peroxide ═ 4: 1;
step S20: dividing the reaction materials into 6 parts and respectively introducing the 6 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 50kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 60 ℃, and enabling the pressure in the reactors 14 to be set to be 20kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing peroxyacetic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxyacetic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 6, the pressure in the rectification column 12 was set to 20kPa, and the temperature in the rectification column 12 was set to 50 ℃.
The purity of the obtained peroxyacetic acid is detected to be 94%, and the yield of the peroxyacetic acid is detected to be 90%.
Example 3Preparation of Peroxyacetic acid
Peroxyacetic acid was produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 10 packing layers are arranged in a shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, the height of each packing layer is 1.5m, and a group of inlets and a group of outlets corresponding to the packing layers are arranged at the 5 th packing layer from the top to the bottom of the shell 122, wherein each group of inlets comprises 4 inlets, and each group of outlets comprises 4 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 4 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 10cm, the length of each pipe is 70cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing acetic anhydride and 50% by mass of aqueous hydrogen peroxide to form a reaction material, wherein the molar ratio of acetic anhydride to hydrogen peroxide in the aqueous hydrogen peroxide is acetic anhydride: hydrogen peroxide ═ 5: 1;
step S20: dividing the reaction materials into 4 parts and respectively introducing the 4 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 20kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 100 ℃, and setting the pressure in the reactors 14 to be 30kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing peroxyacetic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxyacetic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 3, the pressure in the rectification column 12 was set to 30kPa, and the temperature in the rectification column 12 was set to 50 ℃.
The purity of the obtained peroxyacetic acid is 95.2 percent and the yield of the peroxyacetic acid is 91.0 percent.
Example 4Preparation of Peroxyacetic acid
Peroxyacetic acid was produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 20 packing layers are arranged in a shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, the height of each packing layer is 0.5m, and a group of inlets and a group of outlets corresponding to the packing layers are arranged at the 10 th packing layer from the top to the bottom of the shell 122, wherein one group of inlets comprises 6 inlets, and one group of outlets comprises 6 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 6 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 8cm, the length of each pipe is 80cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing acetic anhydride and 50% aqueous solution by mass to form a reaction material, wherein the molar ratio of acetic anhydride to hydrogen peroxide in the aqueous hydrogen peroxide solution is acetic anhydride: hydrogen peroxide ═ 4: 1;
step S20: dividing the reaction materials into 6 parts and respectively introducing the 6 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 50kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 70 ℃, and enabling the pressure in the reactors 14 to be set to be 40kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing peroxyacetic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxyacetic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 7, the pressure in the rectification column 12 was set to 40kPa, and the temperature in the rectification column 12 was set to 60 ℃.
The purity of the obtained peroxyacetic acid is detected to be 95.2%, and the yield of the peroxyacetic acid is detected to be 91.3%.
Example 5Preparation of Peroxyacetic acid
Peroxyacetic acid was produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 15 packing layers are arranged in a shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, the height of each packing layer is 1m, and a group of inlets and a group of outlets corresponding to the packing layers are arranged at the 7 th packing layer from the top to the bottom of the shell 122, wherein one group of inlets comprises 2 inlets, and one group of outlets comprises 2 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 2 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are arranged on each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 10cm, the length of each pipe is 100cm, the thickness of a catalyst layer filled in each pipe is 50cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing acetic anhydride and aqueous hydrogen peroxide solution with the mass percentage concentration of 50% to form a reaction material, wherein the molar ratio of the acetic anhydride to the aqueous hydrogen peroxide solution is acetic anhydride: hydrogen peroxide ═ 6: 1;
step S20: dividing the reaction materials into 2 parts and respectively introducing the 2 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 100kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 80 ℃, and setting the pressure in the reactors 14 to be 10kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing peroxyacetic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxyacetic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 10, the pressure in the rectification column 12 was set to 10kPa, and the temperature in the rectification column 12 was set to 55 ℃.
The purity of the obtained peroxyacetic acid is detected to be 95.5%, and the yield of the peroxyacetic acid is detected to be 92.0%.
Example 6Preparation of peroxypropionic acid
The production of peroxypropionic acid is carried out using a reactive distillation apparatus 10 as shown in figure 1, wherein: 20 trays are arranged in the shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, and a group of inlets and a group of outlets corresponding to the trays are arranged at the 10 th tray from the top to the bottom of the shell 122, wherein the group of inlets comprises 8 inlets, and the group of outlets comprises 8 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 8 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 5cm, the length of each pipe is 100cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing propionic anhydride and aqueous hydrogen peroxide with the mass percent concentration of 50% to form a reaction material, wherein the molar ratio of the propionic anhydride to the hydrogen peroxide in the aqueous hydrogen peroxide is propionic anhydride: hydrogen peroxide ═ 5: 1;
step S20: dividing the reaction materials into 8 parts and respectively introducing the 8 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 10kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 50 ℃, and setting the pressure in the reactors 14 to be 20kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing the peroxypropionic acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxypropionic acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 5, the pressure in the rectification column 12 was set to 20kPa, and the temperature in the rectification column 12 was set to 65 ℃.
The purity of the obtained peroxopropionic acid is 95.2 percent and the yield of the peroxopropionic acid is 91.0 percent.
Example 7Preparation of peroxybutyric acid
Peroxybutyric acid is produced using a reactive distillation apparatus 10 as shown in fig. 1, wherein: 40 trays are arranged in the shell 122 of the rectifying tower 12 at intervals along the height direction of the shell 122, and a group of inlets and a group of outlets corresponding to the trays are arranged at the 20 th tray from the top to the bottom of the shell 122, wherein the group of inlets comprises 6 inlets, and the group of outlets comprises 6 outlets; the group of reactors is arranged around the tower plate, the group of reactors comprises 6 reactors 14, each reactor 14 comprises a reactor shell 140, a plurality of pipes are arranged in each reactor shell 140, a material inlet, a material outlet and a return port are formed in each reactor shell 140, two ends of each pipe are respectively communicated with the material inlet and the material outlet, the pipes are communicated with the return ports, the diameter of each pipe is 10cm, the length of each pipe is 50cm, the thickness of a catalyst layer filled in each pipe is 30cm, the catalyst is boric acid, the material outlet of each reactor shell 140 is communicated with the corresponding inlet, and the return port of each reactor shell 140 is communicated with the corresponding outlet.
The preparation process comprises the following steps:
step S10: mixing butyric anhydride and 50% aqueous hydrogen peroxide solution by mass percent to form a reaction material, wherein the molar ratio of the butyric anhydride to the aqueous hydrogen peroxide solution is butyric anhydride: hydrogen peroxide ═ 4: 1;
step S20: dividing the reaction materials into 6 parts and respectively introducing the 6 parts into the corresponding reactors 14, wherein the feeding flow rate of each part is 600kg/h, heating the corresponding part of the reaction materials by utilizing a heating pipe to enable the part of the reaction materials to reach 60 ℃, and setting the pressure in the reactors 14 to be 10kPa, and reacting under the conditions of the temperature and the pressure to obtain a mixture containing the peroxybutyric acid;
step S30: the mixture reaches a corresponding tower plate of the rectifying tower 12 through an inlet, the mixture is separated on the tower plate to obtain peroxybutyric acid (heavy component) and light component, the light component flows to the top of the rectifying tower 12, and the heavy component flows to the bottom of the rectifying tower 12; the reflux ratio during the rectification operation was set to 6, the pressure in the rectification column 12 was set to 10kPa, and the temperature in the rectification column 12 was set to 80 ℃.
The purity of the obtained peroxybutyric acid is 95% and the yield of the peroxybutyric acid is 91% by detection.
The preferred embodiments of the present invention have been described in detail above with reference to the accompanying drawings, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, numerous simple modifications can be made to the technical solution of the invention, including combinations of the individual specific technical features in any suitable way. The invention is not described in detail in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (16)
1. A reactive distillation apparatus, characterized in that the reactive distillation apparatus (10) comprises:
the reactor (14) is internally provided with a reaction chamber for reacting a reaction material and a heat exchange chamber separated from the reaction chamber, the heat exchange chamber can be communicated with a heat exchange medium for exchanging heat with the reaction material, and the reactor (14) is provided with a material inlet for allowing the reaction material to enter the reaction chamber and a material outlet for discharging a mixture containing a product material obtained by the reaction; and
rectifying column (12), rectifying column (12) set up to be able with the material export is linked together, rectifying column (12) can be to receiving the mixture separates.
2. The reactive rectification apparatus according to claim 1, characterized in that the rectification column (12) comprises a shell (122) and a separation layer (120) arranged within the shell (122), wherein an inlet capable of communicating with the material outlet for flowing the mixture to the separation layer (120) is arranged on the shell (122).
3. The reactive rectification apparatus according to claim 2, characterized in that the reactor (14) is provided with a return port communicating with the reaction chamber;
the shell (122) is provided with an outlet through which the materials accumulated in the separation layer (120) can be discharged, and the outlet is communicated with the return port.
4. The reactive distillation apparatus according to claim 3, wherein a set of inlets and a set of outlets are provided on said shell (122) corresponding to said separation layer (120), a set of inlets comprising a plurality of said inlets and a set of outlets comprising a plurality of said outlets corresponding to respective said inlets;
the reactive distillation device (10) comprises a group of reactors, each group of reactors comprises a plurality of reactors (14), the material outlets of the reactors (14) are communicated with the corresponding inlets, and the return ports of the reactors (14) are communicated with the corresponding outlets.
5. The reactive distillation apparatus according to claim 4, wherein the distillation column (12) comprises a plurality of the separation layers (120) spaced apart from each other along the height direction of the shell (122), and the shell (122) is provided with a plurality of sets of inlets and a plurality of sets of outlets respectively corresponding to the respective separation layers (120);
the reactive distillation device (10) comprises a plurality of groups of reactors corresponding to the corresponding separating layers (120), the material outlets of the reactors (14) in the same group of reactors are communicated with the corresponding inlets in the same group of inlets, and the return ports of the reactors (14) are communicated with the corresponding outlets in the same group of outlets.
6. The reactive distillation apparatus of claim 5, wherein a plurality of said reactors (14) in a same set of reactors are arranged around a same said separation layer (120).
7. The reactive rectification apparatus according to claim 5, characterized in that a spacing between adjacent separation layers (120) is 0.1 to 0.5 of a height of the shell (122).
8. The reactive distillation apparatus of any of claims 3-7, wherein the reactor (14) comprises a reactor housing (140) and a plurality of tubes disposed within the reactor housing (140), wherein: the material inlet, the material outlet and the return port are provided in the reactor case (140), both ends of the tube are respectively communicated with the material inlet and the material outlet, and the tube is communicated with the return port, an inner space of the tube is formed as the reaction chamber, and an inner space of the reactor case (140) is formed as the heat exchange chamber.
9. The reactive distillation apparatus of claim 8, wherein a catalyst layer capable of promoting the reaction of the reaction materials is disposed inside the tubes; or
A catalyst layer capable of promoting the reaction of the reaction materials is arranged in the tube, wherein: the thickness of the catalyst layer is 0.2-0.8 of the length of the respective tube.
10. A process for the preparation of peroxycarboxylic acids, comprising the steps of:
step S10: mixing a first reactant and a second reactant to form a reaction mass, wherein; the first reactant is one or more of carboxylic acid and anhydride, and the second reactant is an oxidant;
step S20: exchanging heat with the reaction material to enable the reaction material to reach a preset temperature, and reacting under the condition of the preset temperature to obtain a mixture containing peroxycarboxylic acid;
step S30: the mixture containing peroxycarboxylic acid obtained in step S20 is subjected to rectification.
11. The process for producing peroxycarboxylic acid of claim 10 wherein,
the carboxylic acid is R-COOH, wherein: r is hydrogen or alkyl with 1-10 carbon atoms;
the acid anhydride is formic anhydride or R1-CO-O-CO-R2Wherein: r1Is alkyl with 1-10 carbon atoms, R2Is alkyl with 1-10 carbon atoms;
the oxidant is peroxide.
12. The process for producing peroxycarboxylic acid of claim 10 wherein the reaction mass is fed at a flow rate of 10 to 1000kg/h in step S20.
13. The process for producing peroxycarboxylic acid of claim 10 wherein, in the step S20, the preset temperature is 40-100 ℃; and/or
In the step S20, the reaction mass is reacted under the action of a catalyst, wherein: the catalyst is a solid acid.
14. The process according to claim 10, wherein in step S30, the reaction is continued by returning a material accumulated in the rectification to step S20.
15. The process according to claim 10, wherein in the step S30, the reflux ratio is set to 2 to 10 when the rectification is performed; and/or
In the step S10, the reaction materials are divided into a plurality of groups to be reacted separately.
16. The process for producing a peroxycarboxylic acid of any of claims 10 to 15 wherein in step S20, the reaction mass is reacted under pressure conditions of 1 to 50 kPa; and/or
In the step S30, the rectification operation is performed under the pressure condition of 1-50 kPa.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101466660A (en) * | 2006-06-23 | 2009-06-24 | 赢创罗姆有限责任公司 | Method for the continuous production of unsaturated carboxylic acid anhydrides |
| CN206318904U (en) * | 2016-10-26 | 2017-07-11 | 湖南聚仁化工新材料科技有限公司 | A kind of device for preparing anhydrous peroxide organic carboxyl acid solution |
| CN206318905U (en) * | 2016-11-04 | 2017-07-11 | 湖南聚仁化工新材料科技有限公司 | A kind of utilization cyclonic separation prepares the device of anhydrous peroxide organic carboxyl acid solution |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101466660A (en) * | 2006-06-23 | 2009-06-24 | 赢创罗姆有限责任公司 | Method for the continuous production of unsaturated carboxylic acid anhydrides |
| CN206318904U (en) * | 2016-10-26 | 2017-07-11 | 湖南聚仁化工新材料科技有限公司 | A kind of device for preparing anhydrous peroxide organic carboxyl acid solution |
| CN206318905U (en) * | 2016-11-04 | 2017-07-11 | 湖南聚仁化工新材料科技有限公司 | A kind of utilization cyclonic separation prepares the device of anhydrous peroxide organic carboxyl acid solution |
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