CN112778136B - 2, 5-dichloronitrobenzene and microchannel continuous synthesis process thereof - Google Patents
2, 5-dichloronitrobenzene and microchannel continuous synthesis process thereof Download PDFInfo
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Abstract
The invention relates to the field of 2, 5-dichloronitrobenzene synthesis, in particular to a 2, 5-dichloronitrobenzene and a microchannel continuous synthesis process thereof, the microchannel continuous synthesis process of 2, 5-dichloronitrobenzene comprises the following steps: the mixed acid is preheated by a micro-channel reactor preheating module and reacts with p-dichlorobenzene in a molten state in a micro-channel reactor reaction module I, then continuously reacts again in a micro-channel reactor reaction module II containing sulfuric acid to obtain a reaction solution, and after layering, the organic layer is washed and layered by alkali solution to obtain the catalyst; the mixed acid is fuming nitric acid and sulfuric acid. The microchannel continuous synthesis process of 2, 5-dichloronitrobenzene belongs to a solvent-free microchannel process, is green and safe, has a raw material conversion rate of 100wt%, a yield of more than 99.5wt%, a product purity of more than 99.9wt%, and can carry out subsequent reactions without rectification and purification.
Description
Technical Field
The invention relates to the field of 2, 5-dichloronitrobenzene synthesis, in particular to a 2, 5-dichloronitrobenzene and a microchannel continuous synthesis process thereof.
Background
At present, domestic industrial production of 2, 5-dichloronitrobenzene mainly adopts a kettle type intermittent process and a kettle type continuous process, but the traditional kettle type nitration process is a high-risk process, and has the problems of low heat transfer efficiency, more stock, long production period, low production efficiency, high safety risk and the like, and a plurality of safety problems inevitably lead to accidents, such as Jilin petrochemical bispheny factory explosion event, tianjin Yikun fine chemical technology development limited company explosion accident, jiangsu salt city water response "3.21" accident and the like. With the increasing strictness of domestic safety production policies, the traditional kettle type continuous nitrification process is abandoned, so the exploration and research of novel continuous nitrification process with high safety coefficient are urgent.
Disclosure of Invention
In view of some of the problems existing in the prior art, the first aspect of the present invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, comprising: the mixed acid is preheated by a micro-channel reactor preheating module and reacts with p-dichlorobenzene in a molten state in a micro-channel reactor reaction module I, then continuously reacts again in a micro-channel reactor reaction module II containing sulfuric acid to obtain a reaction solution, and after layering, the organic layer is washed and layered by alkali solution to obtain the catalyst; the mixed acid is fuming nitric acid and sulfuric acid.
As a preferable technical scheme of the invention, the temperature of the preheating module, the temperature of the reaction module I and the temperature of the reaction module II are respectively and independently 58-100 ℃.
As a preferable technical scheme of the invention, the fuming nitric acid has the concentration of 95-98wt% and the sulfuric acid has the concentration of 90-98wt%.
As a preferable technical scheme of the invention, the weight ratio of fuming nitric acid to the total amount of sulfuric acid is 1: (3-5).
As a preferable technical scheme of the invention, the molar ratio of fuming nitric acid to paradichlorobenzene is (1-1.1): 1.
As a preferable technical scheme of the invention, the microchannel continuous synthesis process of the 2, 5-dichloronitrobenzene comprises the following steps:
(1) Feeding mixed acid into a preheating module of a micro-channel reactor at a flow rate of 10-35mL/min by adopting a continuous feeding mode, feeding p-dichlorobenzene in a molten state into a first reaction module at a flow rate of 10-35mL/min, and feeding sulfuric acid into a second reaction module at a flow rate of 10-35mL/min for reaction to obtain a reaction solution;
(2) And after layering the reaction solution, washing and layering the organic layer by alkali solution to obtain the organic layer.
As a preferred embodiment of the present invention, the reaction time is 10 to 35s.
As a preferred embodiment of the present invention, the concentration of the alkali solution is 5 to 20wt%.
As a preferable technical scheme of the invention, the microchannel reactor is a microchannel reactor with a G1 specification heart-shaped structure.
The second aspect of the invention provides 2, 5-dichloronitrobenzene prepared by the microchannel continuous synthesis process of 2, 5-dichloronitrobenzene.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method has short reaction time, only needs 10-35s, the conversion rate of the raw material paradichlorobenzene reaches 100wt%, and the product yield reaches more than 99.5 wt%;
(2) The content of 2, 5-dichloronitrobenzene in the nitrified product is more than or equal to 99.95wt percent, and the content of 3, 4-dichloronitrobenzene in the impurity is less than 0.01wt percent, so that the nitrified product does not need to be refined/rectified and purified.
(3) In the reaction of the invention, the molar ratio of fuming nitric acid to paradichlorobenzene (1.02-1.08) is 1, and the consumption of nitric acid is small;
(4) The raw material of the invention is the melted paradichlorobenzene, and the process does not need other solvents or reagents, has simple process and saves resources;
(5) The invention adopts a solvent-free process, is green and low in cost, adopts a micro-channel device, is simple and easy to operate, and can reduce the safety risk of nitration reaction and improve the automation control degree and the production efficiency of the device by using the micro-channel reaction device.
Drawings
FIG. 1 is a flow chart of a continuous synthesis process of 2, 5-dichloronitrobenzene in a micro-channel.
Detailed Description
The first aspect of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, comprising: the mixed acid is preheated by a micro-channel reactor preheating module and reacts with p-dichlorobenzene in a molten state in a micro-channel reactor reaction module I, then continuously reacts again in a micro-channel reactor reaction module II containing sulfuric acid to obtain a reaction solution, and after layering, the organic layer is washed and layered by alkali solution to obtain the catalyst; the mixed acid is fuming nitric acid and sulfuric acid.
In one embodiment, the temperature of the preheating module, the first reaction module and the second reaction module is 58-100 ℃ respectively and independently.
Preferably, the temperature of the preheating module is the same as that of the first reaction module, and is 58-80 ℃; more preferably, the temperature of the preheating module and the first reaction module is 70 ℃.
Preferably, the temperature of the second reaction module is 90-100 ℃; more preferably, the temperature of the second reaction module is 100 ℃.
At the temperature in the preheating module, the first reaction module and the second reaction module, paradichlorobenzene is easier to react completely in the reaction process.
In one embodiment, the fuming nitric acid is at a concentration of 95 to 98wt%.
In one embodiment, the sulfuric acid has a concentration of 90 to 98wt%.
In one embodiment, the weight ratio of fuming nitric acid to the total amount of sulfuric acid is 1: (3-5).
Preferably, the weight ratio of fuming nitric acid to the total amount of sulfuric acid is 1:4.
in one embodiment, the weight ratio of sulfuric acid in the mixed acid to sulfuric acid in the second reaction module is 4:1-1:1.
in one embodiment, the fuming nitric acid to paradichlorobenzene molar ratio is (1-1.1): 1.
Preferably, the molar ratio of fuming nitric acid to paradichlorobenzene is (1.02-1.08): 1.
in experiments, the applicant found that higher paradichlorobenzene conversion rate and 2, 5-dichloronitrobenzene yield can be obtained by increasing the content of fuming nitric acid, however, the use of a large amount of fuming nitric acid not only can cause safety accidents, but also brings burden to the post-treatment stage, and the applicant unexpectedly found that when the molar ratio of fuming nitric acid to paradichlorobenzene is (1.02-1.08): in the process 1, mixed acid is preheated and then reacts with p-dichlorobenzene in a molten state, and sulfuric acid is supplemented again for reaction, so that 100wt% of p-dichlorobenzene conversion rate and the yield of 2, 5-dichloronitrobenzene higher than 99.5wt% can be obtained under the condition of lower fuming nitric acid content, and meanwhile, the purity of the obtained 2, 5-dichloronitrobenzene is higher than 99.9wt%.
In one embodiment, the microchannel continuous synthesis process of 2, 5-dichloronitrobenzene comprises the steps of:
(1) Feeding mixed acid into a preheating module of a micro-channel reactor at a flow rate of 10-35mL/min by adopting a continuous feeding mode, feeding p-dichlorobenzene in a molten state into a first reaction module at a flow rate of 10-35mL/min, and feeding sulfuric acid into a second reaction module at a flow rate of 10-35mL/min for reaction to obtain a reaction solution;
(2) And after layering the reaction solution, washing and layering the organic layer by alkali solution to obtain the organic layer.
In a preferred embodiment, the microchannel continuous synthesis process of 2, 5-dichloronitrobenzene comprises the steps of:
(1) Feeding mixed acid into a preheating module of a micro-channel reactor at a flow rate of 17mL/min by adopting a continuous feeding mode, feeding p-dichlorobenzene in a molten state into a first reaction module at a flow rate of 14mL/min, feeding sulfuric acid into a second reaction module at a flow rate of 11mL/min, and reacting to obtain a reaction solution;
(2) And after layering the reaction solution, washing and layering the organic layer by alkali solution to obtain the organic layer.
Preferably, the reaction time is 10-35s; more preferably, the reaction time is 14-28s.
The reaction time is the total time of the reaction of the paradichlorobenzene in a molten state in the first reaction module and the second reaction module.
Preferably, the concentration of the alkali solution is 5-20wt%; more preferably, the concentration of the alkaline solution is 10wt%.
When the alkali washing is performed at a concentration of 10wt% of the alkali solution, the purity of 2, 5-dichloronitrobenzene can be further improved.
The content of the alkali solution in the present invention is not particularly limited, and may be selected conventionally by those skilled in the art.
In one embodiment, the microchannel reactor is a G1 specification heart-shaped structured microchannel reactor.
The microchannel reactor of the invention was purchased from corning corporation.
Compared with the traditional kettle-type reactor, the micro-channel reactor has the advantages of high mass transfer and heat transfer efficiency, short reaction time, low liquid holdup of a reaction system, small volume of the reactor, no amplification effect from laboratory to industrialization and the like due to the unique structure, is an intrinsically safe continuous reactor, and has application in the fields of medicine, chemical industry and pesticides, and particularly has more application in key supervision dangerous chemical technologies such as hydrogenation reaction, chlorination reaction and nitration reaction.
Examples
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not limitative. The raw materials used in the following examples are all commercially available, unless otherwise specified.
The temperature of the first temperature zone in the following examples is the temperature of the preheating module and the first reaction module; the temperature of the second temperature zone is the temperature of the second reaction module.
Example 1
The embodiment 1 of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, as shown in fig. 1, which comprises the following steps:
(1) Weighing 250g of paradichlorobenzene as a raw material, heating to a molten state to obtain FlowA, weighing 80mL of fuming nitric acid and 140mL of sulfuric acid to prepare mixed acid as FlowB, and weighing 150mL of sulfuric acid as FlowC;
(2) After the preheating of the microchannel reactor is completed, controlling the Flow rate of FlowA to be 14mL/min and feeding the reaction module I, controlling the Flow rate of FlowB to be 17mL/min and feeding the reaction module II, controlling the Flow rate of FlowC to be 11mL/min and feeding the reaction module II, reacting at the temperature of 70 ℃ in the temperature of 100 ℃ in the temperature of the first reaction zone, wherein the mol ratio of paradichlorobenzene to fuming nitric acid is 1:1.05, and the mass ratio of fuming nitric acid to the total amount of sulfuric acid is 1:4, the reaction residence time is 28s; the fuming nitric acid has the concentration of 95wt percent and the sulfuric acid has the concentration of 90wt percent;
(3) After each strand of material in the microchannel reactor reaches a stable state, collecting reaction liquid flowing out of an outlet of the reactor; receiving reaction liquid corresponding to FlowA (200 g of paradichlorobenzene) fed for 10min, separating the reaction liquid, adding 40mL of 10wt% sodium hydroxide solution into an organic layer for washing, separating the solution, drying an oil layer to obtain 257.62g of 2, 5-dichloronitrobenzene product, and performing gas chromatographic analysis to obtain 99.98wt% of purity, 100wt% of paradichlorobenzene conversion rate as a raw material and 99.6wt% of yield, wherein an acid layer separated from the reaction liquid is concentrated for reuse.
Example 2
The embodiment 2 of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, which comprises the following steps:
(1) Weighing 500g of paradichlorobenzene as a raw material, heating to a molten state to obtain a Flow A, weighing 160mL of fuming nitric acid and 280mL of sulfuric acid to prepare a mixed acid as a Flow B, and weighing 300mL of sulfuric acid as a Flow C;
(2) After the preheating of the microchannel reactor is completed, controlling the Flow rate of FlowA to be 28mL/min and feeding the reaction module I, controlling the Flow rate of FlowB to be 34mL/min and feeding the reaction module II, controlling the Flow rate of FlowC to be 19mL/min and feeding the reaction module II, reacting at the temperature of 70 ℃ in the temperature of 100 ℃ in the temperature of the first reaction zone, wherein the mol ratio of paradichlorobenzene to fuming nitric acid is 1:1.05, and the mass ratio of fuming nitric acid to the total amount of sulfuric acid is 1:3.8, a reaction residence time of 14s; the fuming nitric acid has the concentration of 96wt percent and the sulfuric acid has the concentration of 92wt percent;
(3) After each strand of material in the microchannel reactor reaches a stable state, collecting reaction liquid flowing out of an outlet of the reactor; receiving reaction liquid corresponding to FlowA (400 g of paradichlorobenzene) fed for 10min, separating the reaction liquid, adding 80mL of 10wt% sodium hydroxide solution into an organic layer for washing, separating the solution, drying an oil layer to obtain 514.87g of 2, 5-dichloronitrobenzene product, and performing gas chromatographic analysis to obtain 99.95wt% of purity, 100wt% of paradichlorobenzene conversion rate as a raw material and 99.5wt% of yield, wherein an acid layer separated from the reaction liquid is concentrated and then used for application.
Example 3
The embodiment 3 of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, which comprises the following steps:
(1) 250g of paradichlorobenzene as a raw material is weighed and heated to be in a molten state to be taken as Flow A, 80mL of fuming nitric acid and 140mL of sulfuric acid recovered in example 1 are weighed and prepared into mixed acid to be taken as Flow B, and 150mL of sulfuric acid recovered in example 1 is taken as Flow C;
(2) After the preheating of the microchannel reactor is completed, controlling the Flow rate of FlowA to be 14mL/min and feeding the reaction module I, controlling the Flow rate of FlowB to be 17mL/min and feeding the reaction module II, controlling the Flow rate of FlowC to be 11mL/min and feeding the reaction module II, reacting at the temperature of 70 ℃ in the temperature of 100 ℃ in the temperature of the first reaction zone, wherein the mol ratio of paradichlorobenzene to fuming nitric acid is 1:1.05, and the mass ratio of fuming nitric acid to the total amount of recovered sulfuric acid is 1:4, the reaction residence time is 28s; the fuming nitric acid has a concentration of 97wt% and 94wt%;
(3) After each strand of materials in the microchannel reactor reach a stable state, collecting reaction liquid flowing out of an outlet of the reactor, receiving reaction liquid corresponding to FlowA (200 g of paradichlorobenzene) fed for 10min, separating the reaction liquid, adding 40mL of 10wt% sodium hydroxide solution into an organic layer for washing, separating the solution, drying an oil layer to obtain a product 2, 5-dichloronitrobenzene 257.67g, and carrying out gas chromatographic analysis to obtain 99.96wt% of purity, 100wt% of paradichlorobenzene conversion rate of raw materials and 99.6wt% of yield, and continuously applying the separated acid layer after concentrating the reaction liquid.
Example 4
The embodiment 4 of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, which comprises the following steps:
(1) Weighing 250g of paradichlorobenzene as a raw material, heating to a molten state to obtain FlowA, weighing 80mL of fuming nitric acid and 140mL of sulfuric acid to prepare mixed acid as FlowB;
(2) After the preheating of the micro-channel reactor is finished, controlling the flow rate of FlowA to be 14mL/min and feeding the flow rate of FlowB to be 17mL/min, feeding the flow rate of FlowB to the preheating module, and carrying out reaction at the temperature of 70 ℃ in the first reaction temperature zone and 100 ℃ in the second reaction temperature zone, wherein the molar ratio of paradichlorobenzene to fuming nitric acid is 1:1.05, and the reaction residence time is 28s; the fuming nitric acid has the concentration of 96wt percent and the sulfuric acid has the concentration of 98wt percent;
(3) After each strand of material in the microchannel reactor reaches a stable state, collecting reaction liquid flowing out of an outlet of the reactor; receiving reaction liquid corresponding to FlowA (200 g of paradichlorobenzene) fed for 10min, separating the reaction liquid, adding 40mL of 10wt% sodium hydroxide solution into an organic layer for washing, separating the solution, drying an oil layer to obtain the product 2, 5-dichloronitrobenzene, wherein the conversion rate of paradichlorobenzene serving as a raw material is 86wt%, the yield is 90.2wt%, and separating an acid layer from the reaction liquid for reuse after concentrating.
Example 5
The embodiment 5 of the invention provides a microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, which comprises the following steps:
(1) Weighing 250g of paradichlorobenzene as a raw material, heating to a molten state to obtain FlowA, weighing 80mL of fuming nitric acid and 140mL of sulfuric acid to prepare mixed acid as FlowB, and weighing 150mL of sulfuric acid as FlowC;
(2) After the preheating of the microchannel reactor is completed, controlling the Flow rate of FlowA to be 14mL/min and feeding the reaction module I, controlling the Flow rate of FlowB to be 17mL/min and feeding the reaction module II, controlling the Flow rate of FlowC to be 11mL/min and feeding the reaction module II, reacting at the temperature of 70 ℃ in the temperature of 90 ℃ in the temperature of the first reaction zone, wherein the mol ratio of paradichlorobenzene to fuming nitric acid is 1:1.05, and the mass ratio of fuming nitric acid to the total amount of sulfuric acid is 1:4, the reaction residence time is 28s; the fuming nitric acid has the concentration of 96wt percent and the sulfuric acid has the concentration of 95wt percent;
(3) After each strand of material in the microchannel reactor reaches a stable state, collecting reaction liquid flowing out of an outlet of the reactor; receiving a reaction solution corresponding to FlowA (200 g of paradichlorobenzene) fed for 10min, separating the reaction solution, adding 40mL of 10wt% sodium hydroxide solution into an organic layer for washing, separating the solution, drying an oil layer to obtain the product 2, 5-dichloronitrobenzene, and carrying out gas chromatographic analysis to obtain 99.23wt% of purity, 100wt% of paradichlorobenzene conversion rate of raw materials and 98.9wt% of yield, wherein an acid layer separated from the reaction solution is concentrated for reuse.
The foregoing examples are illustrative only and serve to explain some features of the method of the invention. The appended claims are intended to claim the broadest possible scope and the embodiments presented herein are merely illustrative of selected implementations based on combinations of all possible embodiments. It is, therefore, not the intention of the applicant that the appended claims be limited by the choice of examples illustrating the features of the invention. Some numerical ranges used in the claims also include sub-ranges within which variations in these ranges should also be construed as being covered by the appended claims where possible.
Claims (7)
1. A microchannel continuous synthesis process of 2, 5-dichloronitrobenzene, which is characterized by comprising the following steps: the mixed acid is preheated by a micro-channel reactor preheating module and reacts with p-dichlorobenzene in a molten state in a micro-channel reactor reaction module I, then continuously reacts again in a micro-channel reactor reaction module II containing sulfuric acid to obtain a reaction solution, and after layering, the organic layer is washed and layered by alkali solution to obtain the catalyst; the mixed acid is fuming nitric acid and sulfuric acid;
the molar ratio of fuming nitric acid to paradichlorobenzene is (1.02-1.08): 1, a step of;
the temperature of the preheating module is 58-80 ℃ as same as that of the first reaction module, and the temperature of the second reaction module is 100 ℃.
2. The microchannel continuous synthesis process of 2, 5-dichloronitrobenzene according to claim 1, wherein the concentration of fuming nitric acid is 95-98wt% and the concentration of sulfuric acid is 90-98wt%.
3. The microchannel continuous synthesis process of 2, 5-dichloronitrobenzene according to claim 2, wherein the weight ratio of fuming nitric acid to the total amount of sulfuric acid is 1: (3-5).
4. A microchannel continuous synthesis process for 2, 5-dichloronitrobenzene according to any one of claims 1-3, comprising the steps of:
(1) Feeding mixed acid into a preheating module of a micro-channel reactor at a flow rate of 10-35mL/min by adopting a continuous feeding mode, feeding p-dichlorobenzene in a molten state into a first reaction module at a flow rate of 10-35mL/min, and feeding sulfuric acid into a second reaction module at a flow rate of 10-35mL/min for reaction to obtain a reaction solution;
(2) And after layering the reaction solution, washing and layering the organic layer by alkali solution to obtain the organic layer.
5. The continuous synthesis process for 2, 5-dichloronitrobenzene according to claim 4, wherein the reaction time is from 10 to 35s.
6. The process for continuous synthesis of 2, 5-dichloronitrobenzene according to claim 5, wherein the concentration of the alkaline solution is 5-20wt%.
7. The continuous synthesis process of 2, 5-dichloronitrobenzene according to claim 6, wherein the microchannel reactor is a G1-specification heart-shaped microchannel reactor.
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