CN112920060A - Synthesis device and application of 2, 6-dichloro-4-aminophenol - Google Patents
Synthesis device and application of 2, 6-dichloro-4-aminophenol Download PDFInfo
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Abstract
A synthesis device of 2, 6-dichloro-4-aminophenol comprises a first raw material storage tank group, a mixing kettle, a first raw material storage tank, a kettle type reactor, a first solid-liquid separator, a drying tower, a second raw material storage tank group, a second raw material storage tank, a tower type reactor, a second solid-liquid separator and a distillation tower; the discharge hole of the first raw material storage tank group is connected with the feed hole of the mixing kettle; the discharge ports of the mixing kettle and the first raw material storage tank are both connected with the feed port of the kettle-type reactor; a discharge hole of the kettle reactor is connected to a feed hole of the first solid-liquid separator; the solid phase outflow port of the first solid-liquid separator is connected with the feed inlet of the tower reactor, and a drying tower is arranged between the solid phase outflow port of the first solid-liquid separator and the feed inlet of the tower reactor; the discharge ports of the second raw material storage tank group and the second raw material storage tank are connected with the feed port of the tower reactor; the discharge hole of the tower reactor is connected to the feed hole of the second solid-liquid separator, and a liquid phase flow outlet of the second solid-liquid separator is provided with a distillation tower. The method has the effect of efficiently and continuously synthesizing the 2, 6-dichloro-4-aminophenol with high purity and high yield.
Description
Technical Field
The invention relates to the field of organic chemical industry, in particular to a synthesis device of 2, 6-dichloro-4-aminophenol and application thereof.
Background
2, 6-dichloro-4-aminophenol is an important intermediate for synthesizing hexaflumuron. Hexaflumuron is a benzoyl urea insecticide, which is a chemical product with stable chemical properties and is dissolved in acetone and dichloromethane. It is a chitin synthesis inhibitor, has high insecticidal and ovicidal activity, and is quick-acting, especially for preventing and treating bollworm.
Currently, the main synthesis process of 2, 6-dichloro-4-aminophenol is as follows: taking p-nitrophenol as a raw material, carrying out chlorination reaction with chlorine in hydrochloric acid to generate 2, 6-dichloro-4-nitrophenol, and reducing the 2, 6-dichloro-4-nitrophenol by a reducing agent at high temperature to generate the 2, 6-dichloro-4-aminophenol.
Aiming at the technology, as the chlorine atom in the chlorine can not be ensured to stably attack the ortho position of the p-nitrophenol hydroxyl, in the production process adopting the technology, various isomers and monochloro-nitrophenol can be generated, so that the separation of a target product is difficult, and the yield and the purity of the product are reduced.
Another existing synthesis process of 2, 6-dichloro-4-aminophenol comprises the following steps: 2, 6-dichlorophenol is taken as a raw material and mixed with nitric acid for nitration reaction to generate 2, 6-dichloro-4-nitrophenol, and then the 2, 6-dichloro-4-aminophenol is generated by hydrazine hydrate reduction at high temperature.
By adopting the process, the nitro attack position is clear, the by-products generated in the production process are few, the target product is easy to separate, the yield and the purity of the 2, 6-dichloro-4-aminophenol are favorably improved, and meanwhile, most of the solvent and the catalyst used in the process can be recycled and the recovery rate is higher.
Disclosure of Invention
The invention aims to provide a synthesis device of 2, 6-dichloro-4-aminophenol, which is beneficial to improving the yield and purity of 2, 6-dichloro-4-aminophenol.
The invention also aims to provide a synthesis device of 2, 6-dichloro-4-aminophenol, which can recycle part of the solvent and the auxiliary agent used in the synthesis process.
The invention also aims to provide the application of the synthesis device of the 2, 6-dichloro-4-aminophenol, and the application method can realize the continuous synthesis of the 2, 6-dichloro-4-aminophenol and improve the production efficiency.
The technical purpose of the invention is realized by the following technical scheme:
a synthesis device of 2, 6-dichloro-4-aminophenol comprises a first raw material storage tank group, a mixing kettle, a first raw material storage tank, a kettle type reactor, a first solid-liquid separator, a drying tower, a second raw material storage tank group, a second raw material storage tank, a tower type reactor, a second solid-liquid separator and a distillation tower; the discharge hole of the first raw material storage tank group is connected with the feed hole of the mixing kettle; the discharge ports of the mixing kettle and the first raw material storage tank are both connected with the feed port of the kettle-type reactor; a discharge hole of the kettle reactor is connected to a feed hole of the first solid-liquid separator; the solid phase outflow port of the first solid-liquid separator is connected with the feed inlet of the tower reactor, and a drying tower is arranged between the solid phase outflow port of the first solid-liquid separator and the feed inlet of the tower reactor; the discharge ports of the second raw material storage tank group and the second raw material storage tank are connected with the feed port of the tower reactor; the discharge hole of the tower reactor is connected to the feed hole of the second solid-liquid separator, and a liquid phase flow outlet of the second solid-liquid separator is provided with a distillation tower.
By adopting the technical scheme, the synthesis of the 2, 6-dichloro-4-aminophenol is completed in two stages: taking easily obtained 2, 6-dichlorophenol as a raw material, and carrying out nitration reaction in a kettle type reactor to prepare an intermediate 2, 6-dichloro-4-nitrophenol; 2, 6-dichloro-4-nitrophenol is subjected to reduction reaction in a tower reactor to prepare 2, 6-dichloro-4-aminophenol. In the first-stage reaction, the nitro attack position is clear, the hydrogen at the hydroxyl para position in the 2, 6-dichlorophenol is stably substituted, the generation of isomers and byproducts is reduced, the nitration efficiency of the 2, 6-dichlorophenol is improved, the proportion of the 2, 6-dichloro-4-nitrophenol in the product is increased, and the yield and the purity of the 2, 6-dichloro-4-aminophenol generated by the subsequent reduction reaction of the 2, 6-dichloro-4-nitrophenol are further improved.
Further, a reflux tank is connected to the tower reactor.
By adopting the technical scheme, the reflux tank is additionally arranged, and the reaction liquid is repeatedly distilled in the reduction reaction of the 2, 6-dichloro-4-nitrophenol, so that the reaction is fully carried out, the conversion efficiency is improved, and the yield and the purity of the 2, 6-dichloro-4-aminophenol are further improved.
And furthermore, rotor flow meters are arranged on the discharge pipelines of the first raw material storage tank and the second raw material storage tank.
Through adopting above-mentioned technical scheme, utilize rotameter, the ejection of compact speed of nitric acid in the monitoring first raw materials storage tank and the ejection of compact speed of hydrazine hydrate in the second raw materials storage tank, and then ensure that nitration reaction and reduction reaction go on steadily.
Further, the second solid-liquid separator is a jacket heat-preservation solid-liquid separator.
By adopting the technical scheme, the thermal filtration of the reduction reaction product is realized, the phenomenon that the generation amount of byproducts is increased due to temperature reduction is avoided, and the yield and the purity of the 2, 6-dichloro-4-aminophenol are further improved.
Further, a standing pool is arranged in the liquid phase outflow direction of the first solid-liquid separator.
By adopting the technical scheme, the layering treatment of the liquid phase flowing out of the first solid-liquid separator is realized by utilizing the standing tank, so that the solvent component in the nitration reaction is convenient to recover.
Further, a washing tower is arranged in the solid phase outflow direction of the second solid-liquid separator.
By adopting the technical scheme, the washing treatment of the solid phase flowing out of the second solid-liquid separator is realized by utilizing the washing tower, so that the catalyst component in the reduction reaction is convenient to recover.
The application of the synthesis device of 2, 6-dichloro-4-aminophenol comprises the following steps:
s1, preparation of 2, 6-dichloro-4-nitrophenol from 2, 6-dichlorophenol:
s1-1, feeding the 2, 6-dichlorophenol, the tetrachloroethylene and the water absorbent stored in the first raw material storage tank group into a mixing kettle, uniformly mixing, and stirring until the mixture is completely dissolved to obtain a mixture a;
s1-2, feeding the mixture a into a kettle type reactor, heating to a first reaction temperature, feeding nitric acid in a first raw material storage tank into the kettle type reactor, and keeping the first reaction temperature for reaction for a period of time to obtain a reaction solution a;
s1-3, cooling, and allowing the reaction liquid a to flow into a first solid-liquid separator from the kettle type reactor for solid-liquid separation treatment;
s1-4, after solid-liquid separation, the solid phase enters a drying tower, and 2, 6-dichloro-4-nitrophenol is obtained after drying;
s2 preparation of 2, 6-dichloro-4-aminophenol from 2, 6-dichloro-4-nitrophenol:
s2-1, feeding ethanol and a catalyst in the second raw material storage tank group and the 2, 6-dichloro-4-nitrophenol prepared by the S1 into a tower reactor together, heating to a second reaction temperature, and mixing to obtain a mixture b;
s2-2, enabling hydrazine hydrate in a second raw material storage tank to enter a tower reactor, and reacting with the mixture b for a period of time at a second reaction temperature to obtain a reaction liquid b;
s2-3, feeding the reaction liquid b into a second solid-liquid separator, keeping the second reaction temperature, and performing thermal filtration treatment;
and S2-4, filtering, feeding the liquid phase into a distillation tower, and distilling off ethanol to obtain the 2, 6-dichloro-4-aminophenol.
By adopting the technical scheme, 2, 6-dichlorophenol as a raw material is dissolved in tetrachloroethylene and mixed with concentrated sulfuric acid as a water absorbent in a mixing kettle, the mixture is uniformly mixed and flows into a kettle-type reactor to carry out nitration reaction with nitric acid, solid-liquid separation treatment is carried out on reaction liquid a, and 2, 6-dichloro-4-nitrophenol is obtained after the solid phase is dried; and 2, 6-dichloro-4-nitrophenol enters a tower reactor, is dissolved in ethanol, is subjected to reduction reaction with hydrazine hydrate, is subjected to solid-liquid separation treatment on reaction liquid b, and is evaporated to dryness to obtain the 2, 6-dichloro-4-aminophenol. In the application process, less isomers and byproducts are generated in the reaction, the separation operation of the target product is convenient, and the target product has high yield and high purity.
Furthermore, in the step S1, the molar ratio of the 2, 6-dichlorophenol to the nitric acid is 1 (1.2-1.6).
By adopting the technical scheme, the amount of the nitric acid is slightly more than that of the 2, 6-dichlorophenol, so that the 2, 6-dichlorophenol is completely nitrified, and the effect of improving the yield of the intermediate 2, 6-dichloro-4-nitrophenol is achieved.
Furthermore, in the step S2, the molar ratio of the 2, 6-dichloro-4-nitrophenol to the hydrazine hydrate is 1 (1.8-2.2).
By adopting the technical scheme, N in hydrazine hydrate is obtained according to the molar ratio2H4The molar weight of the compound is slightly more than that of the 2, 6-dichloro-4-nitrophenol, so that the reduction reaction is fully carried out, and the effect of improving the yield of the 2, 6-dichloro-4-aminophenol is achieved. And meanwhile, the hydrazine hydrate is prevented from being excessively fed, and the material flushing risk is avoided.
Further, the first reaction temperature in the step S1 is 34-36 ℃; the second reaction temperature in the step S2 is 72 to 76 ℃.
By adopting the technical scheme, the reaction efficiency of the nitration reaction and the reduction reaction is higher, the number of byproducts is less, the subsequent separation difficulty of the target product is further reduced, and the yield and the purity of the target product are improved.
Drawings
FIG. 1 is a flow diagram of an apparatus for synthesizing 2, 6-dichloro-4-aminophenol.
The reference numbers in the figures illustrate: 1. a first raw material storage tank group; 2. a mixing kettle; 3. a first feedstock storage tank; 4. a kettle reactor; 5. a first solid-liquid separator; 6. standing in a pool; 7. a drying tower; 8. a second raw material storage tank group; 9. a second raw material storage tank; 10. a tower reactor; 11. a second solid-liquid separator; 12. a distillation column; 13. a purification tower; 14. and (7) refluxing the tank.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
as shown in fig. 1, a synthesis apparatus for 2, 6-dichloro-4-aminophenol comprises a first raw material storage tank group 1, a mixing kettle 2, a first raw material storage tank 3, a kettle-type reactor 4, a first solid-liquid separator 5, a standing tank 6, a drying tower 7, a second raw material storage tank group 8, a second raw material storage tank 9, a tower-type reactor 10, a second solid-liquid separator 11, a distillation tower 12, a purification tower 13 and a reflux tank 14.
2, 6-dichlorophenol with industrial purity of 99.5%, tetrachloroethylene with industrial purity of 99.5% and concentrated sulfuric acid with industrial purity of 98% are stored in a first raw material storage tank group 1 in an isolated manner, and a discharge port of the first raw material storage tank group 1 is connected with a feed port of a mixing kettle 2 through a pipeline with a valve; the discharge port of the mixing kettle 2 is connected with the feed port of the kettle type reactor 4 through a pipeline with a valve.
In first raw materials storage tank 3, store 68% of industrial purity's nitric acid, the discharge gate of first raw materials storage tank 3 is through the pipeline that has the valve, connects in the feed inlet of cauldron formula reactor 4, and simultaneously, install rotameter on the pipeline between first raw materials storage tank 3 and cauldron formula reactor 4.
The discharge hole of the kettle reactor 4 is connected to the feed hole of the first solid-liquid separator 5 through a pipeline with a valve.
A drying tower 7 is arranged in the solid phase outflow direction of the first solid-liquid separator 5, and a discharge hole of the drying tower 7 is connected with a feed inlet of the tower reactor 10 through a pipeline with a valve; a standing pool 6 is arranged in the liquid phase outflow direction of the first solid-liquid separator 5, and a discharge port of the standing pool 6 is connected with a discharge pipeline A.
In the second raw material storage tank group 8, 95% industrial pure ethanol and raney nickel are stored in an isolated manner, and a discharge port of the second raw material storage tank group 8 is connected to a feed port of the tower reactor 10 through a pipeline with a valve.
In the second raw material storage tank 9, 80% industrial pure hydrazine hydrate is stored, the discharge port of the second raw material storage tank 9 is connected to the feed port of the tower reactor 10 through a pipeline with a valve, and meanwhile, a rotor flow meter is installed on the pipeline between the second raw material storage tank 9 and the tower reactor 10.
The tower reactor 10 is connected with the reflux tank 14 through two pipelines with valves to form a loop structure, and meanwhile, a power pump is arranged on the pipeline flowing from the reflux tank 14 to the tower reactor 10; the discharge port of the column reactor 10 is connected to the feed port of the second solid-liquid separator 11 through a pipe with a valve.
A distillation tower 12 is arranged in the liquid phase outflow direction of the second solid-liquid separator 11, and a discharge port of the distillation tower 12 is connected with a discharge pipeline B; a washing tower is arranged in the solid phase outflow direction of the second solid-liquid separator 11, and a discharge hole of the washing tower is connected with a C discharge pipeline.
The application of a synthesis device of 2, 6-dichloro-4-aminophenol for batch synthesis of 2, 6-dichloro-4-aminophenol comprises the following steps:
s1, preparation of 2, 6-dichloro-4-nitrophenol from 2, 6-dichlorophenol:
s1-1, flowing 10Kg of 2, 6-dichlorophenol, 30L of tetrachloroethylene and 0.3L of concentrated sulfuric acid into a mixing kettle 2 from a first raw material storage tank group 1, starting a motor, and stirring until the materials are completely dissolved at the speed of 800r/min to obtain a mixture a;
s1-2, feeding the mixture a into a kettle type reactor 4, heating to 35 ℃, feeding 6Kg of nitric acid into the kettle type reactor 4 from a first raw material storage tank 3, controlling the flow rate to be 2Kg/h, always keeping stirring at 800r/min, and keeping stirring for 2h after the nitric acid is completely added to obtain a reaction liquid a;
s1-3, cooling the reaction liquid a to room temperature, and allowing the reaction liquid a to flow into a first solid-liquid separator 5 from the kettle type reactor 4 for solid-liquid separation treatment;
s1-4, after solid-liquid separation, the solid phase enters a drying tower 7, and is dried to obtain solid 2, 6-dichloro-4-nitrophenol; the liquid phase enters a standing tank 6, and after layering, tetrachloroethylene positioned at the lower layer flows out from a discharge pipeline A;
s2 preparation of 2, 6-dichloro-4-aminophenol from 2, 6-dichloro-4-nitrophenol:
s2-1, feeding 30L of ethanol and 0.5Kg of Raney nickel into the tower reactor 10 from the second raw material storage tank group 8, adding all the 2, 6-dichloro-4-nitrophenol prepared in the step S1-4, heating to 75 ℃, and mixing to obtain a mixture b;
s2-2, flowing 6Kg of hydrazine hydrate into the tower reactor 10 from the second raw material storage tank 9, controlling the flow rate to be 3Kg/h, obtaining a reaction liquid b after the addition is finished, and carrying out heat preservation and reflux on the reaction liquid b between the tower reactor 10 and the reflux tank 14 for 4 h;
s2-3, and the reaction liquid b enters a second solid-liquid separator 11 from the bottom of the tower reactor 10, and is subjected to heat filtration treatment at the temperature of 75 ℃;
s2-4, filtering, feeding the liquid phase into a distillation tower 12, distilling out ethanol, and discharging solid 2, 6-dichloro-4-aminophenol from a discharge pipeline B; the solid phase enters a purifying tower 13, and after washing, the Raney nickel flows out from a C discharge pipeline.
HPLC detection shows that the conversion rate of 2, 6-dichlorophenol reaches 99.86 percent, and the selectivity of 2, 6-dichloro-4-aminophenol reaches 97.60 percent.
Example 2:
an apparatus for synthesizing 2, 6-dichloro-4-aminophenol, similar to that of example 1.
The application of a synthesis device of 2, 6-dichloro-4-aminophenol for continuously synthesizing 2, 6-dichloro-4-aminophenol comprises the following steps:
s1, preparation of 2, 6-dichloro-4-nitrophenol from 2, 6-dichlorophenol:
s1-1, putting 2, 6-dichlorophenol into a mixing kettle 2 which is always kept running at 600r/min from a first raw material storage tank group 1 at a rate of 2Kg/h, allowing tetrachloroethylene to flow at a rate of 6L/h, and allowing concentrated sulfuric acid to flow at a rate of 0.06L/h;
s1-2, the kettle type reactor 4 is always kept at 35 ℃ and stirred at 600 r/min; the nitric acid flows into the kettle type reactor 4 from the first raw material storage tank 3 at a rate of 1.08L/h all the time; every 2h, the mixed liquor in the mixing kettle 2 flows into the kettle type reactor for 43h at a rate of 10L/h;
s1-3, enabling the mixture in the kettle-type reactor 4 to flow into a first solid-liquid separator at an interval of 5h for a period of 7.2L/h for solid-liquid separation treatment;
s1-4, after solid-liquid separation, the solid phase enters a drying tower 7, and is dried to obtain solid 2, 6-dichloro-4-nitrophenol; the liquid phase enters a standing tank 6, and after layering, tetrachloroethylene positioned at the lower layer flows out from a discharge pipeline A;
s2 preparation of 2, 6-dichloro-4-aminophenol from 2, 6-dichloro-4-nitrophenol:
s2-1, feeding ethanol at a rate of 6L/h, feeding Raney nickel at a rate of 0.1Kg/h, and feeding 2, 6-dichloro-4-nitrophenol prepared in the step S1-4 at a rate of 1.8Kg/h into a tower reactor 10 kept at 75 ℃ all the time from a second raw material tank group 8;
s2-2, feeding hydrazine hydrate into the tower reactor 10 from the second raw material storage tank 9 at a rate of 1.5Kg/h to obtain a reaction solution b, wherein the reaction solution b far away from the bottom of the tower reactor 10 is always refluxed at a temperature of 75 ℃ between the tower reactor 10 and the reflux tank 14;
s2-3, enabling the reaction liquid b positioned at the bottom of the tower reactor 10 to flow into a second solid-liquid separator 11 at a rate of 6L/h, and carrying out heat filtration treatment at a temperature of 75 ℃;
s2-4, after heat filtration treatment, the liquid phase enters a distillation tower 12, ethanol is distilled out, and solid 2, 6-dichloro-4-aminophenol flows out from a discharge pipeline B; the solid phase enters a purifying tower 13, and after washing, the Raney nickel flows out from a C discharge pipeline.
HPLC detection is carried out on a product generated after continuous and stable reaction for 12 hours, the conversion rate of 2, 6-dichlorophenol reaches 98.91 percent, and the selectivity of 2, 6-dichloro-4-aminophenol reaches 95.75 percent.
According to the test results of the examples 1-2, it can be seen that the batch synthesis or continuous synthesis of 2, 6-dichloro-4-aminophenol can be carried out by using the present invention, and the product yield and purity of the continuous synthesis are slightly lower than those of the batch synthesis, but higher than those of the product synthesized by using the conventional process. Meanwhile, part of the solvent and the catalyst selected in the invention can be recycled, such as tetrachloroethylene and Raney nickel. In conclusion, the advantages of the present invention over the prior art are apparent.
Claims (10)
1. A synthesis device of 2, 6-dichloro-4-aminophenol is characterized by comprising a first raw material storage tank group (1), a mixing kettle (2), a first raw material storage tank (3), a kettle type reactor (4), a first solid-liquid separator (5), a drying tower (7), a second raw material storage tank group (8), a second raw material storage tank (9), a tower type reactor (10), a second solid-liquid separator (11) and a distillation tower (12);
the discharge hole of the first raw material storage tank group (1) is connected with the feed inlet of the mixing kettle (2); the discharge ports of the mixing kettle (2) and the first raw material storage tank (3) are both connected with the feed port of the kettle-type reactor (4); a discharge hole of the kettle type reactor (4) is connected to a feed hole of the first solid-liquid separator (5); the solid phase outflow port of the first solid-liquid separator (5) is connected with the feed port of the tower reactor (10), and a drying tower (7) is arranged between the solid phase outflow port and the feed port; the discharge ports of the second raw material storage tank group (8) and the second raw material storage tank (9) are both connected with the feed port of the tower reactor (10); the discharge hole of the tower reactor (10) is connected to the feed hole of the second solid-liquid separator (11), and a liquid phase flow outlet of the second solid-liquid separator (11) is provided with a distillation tower (12).
2. The synthesis device of 2, 6-dichloro-4-aminophenol according to claim 1, characterized in that a reflux drum (14) is connected to said column reactor (10).
3. The apparatus for synthesizing 2, 6-dichloro-4-aminophenol according to claim 1, wherein the discharge pipes of the first raw material tank (3) and the second raw material tank (9) are provided with rotameters.
4. The apparatus for synthesizing 2, 6-dichloro-4-aminophenol according to claim 1, wherein said second solid-liquid separator (11) is a jacketed insulated solid-liquid separator.
5. The apparatus for synthesizing 2, 6-dichloro-4-aminophenol according to claim 1, wherein said first solid-liquid separator (5) is provided with a standing tank (6) in the liquid phase outflow direction.
6. The apparatus for synthesizing 2, 6-dichloro-4-aminophenol according to claim 1, wherein said second solid-liquid separator (11) is provided with a washing column in the solid phase outflow direction.
7. Use of the synthesis device according to any one of claims 1 to 6 for the synthesis of 2, 6-dichloro-4-aminophenol, characterized in that it comprises the following steps:
s1 preparation of 2, 6-dichloro-4-nitrophenol from 2, 6-dichlorophenol
S1-1, feeding the 2, 6-dichlorophenol, the tetrachloroethylene and the water absorbent stored in the first raw material storage tank group (1) into a mixing kettle (2) to be uniformly mixed, and stirring until the mixture is completely dissolved to obtain a mixture a;
s1-2, feeding the mixture a into a kettle type reactor (4), heating to a first reaction temperature, feeding nitric acid in a first raw material storage tank (3) into the kettle type reactor (4), and keeping the first reaction temperature for reaction for a period of time to obtain a reaction solution a;
s1-3, cooling, and allowing the reaction liquid a to flow into a first solid-liquid separator (5) from the kettle reactor (4) for solid-liquid separation treatment;
s1-4, after solid-liquid separation, the solid phase enters a drying tower (7), and 2, 6-dichloro-4-nitrophenol is obtained after drying;
s2 preparation of 2, 6-dichloro-4-aminophenol from 2, 6-dichloro-4-nitrophenol
S2-1, ethanol and catalyst in the second raw material storage tank group (8) and 2, 6-dichloro-4-nitrophenol prepared by S1 enter a tower reactor (10) together, and are heated to a second reaction temperature to be mixed, so that a mixture b is obtained;
s2-2, feeding hydrazine hydrate in a second raw material storage tank (9) into a tower reactor (10), and reacting with the mixture b for a period of time at a second reaction temperature to obtain a reaction liquid b;
s2-3, feeding the reaction liquid b into a second solid-liquid separator (11), keeping the second reaction temperature, and carrying out heat filtration treatment;
s2-4, filtering, feeding the liquid phase into a distillation tower (12), and distilling off ethanol to obtain 2, 6-dichloro-4-aminophenol.
8. The method for synthesizing 2, 6-dichloro-4-aminophenol according to claim 7, wherein the molar ratio of the 2, 6-dichlorophenol to the nitric acid in step S1 is 1 (1.2-1.6).
9. The method for synthesizing 2, 6-dichloro-4-aminophenol according to claim 7, wherein the molar ratio of 2, 6-dichloro-4-nitrophenol to hydrazine hydrate in step S2 is 1 (1.8-2.2).
10. The method for synthesizing 2, 6-dichloro-4-aminophenol according to claim 7, wherein the first reaction temperature in step S1 is 34-36 ℃; the second reaction temperature in the step S2 is 72 to 76 ℃.
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| CN115141109A (en) * | 2022-07-29 | 2022-10-04 | 浙江乾精新材料科技有限责任公司 | Synthetic method of hexaflumuron key intermediate 2,6-dichloro-4-aminophenol |
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