CN114835576A - Preparation method of 2-hydroxy-3-naphthoic acid - Google Patents
Preparation method of 2-hydroxy-3-naphthoic acid Download PDFInfo
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Abstract
The invention discloses a preparation method of 2-hydroxy-3-naphthoic acid, which comprises the following steps of S101, putting 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate when the temperature in the pot is raised to be more than 120 ℃, and obtaining liquid 2-naphthol; s102, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to the temperature of 120-naphthol sodium salt solution for reaction at 150 ℃ to obtain a 2-naphthol sodium salt solution, and after the reaction is finished, vacuumizing the pot to a negative pressure and then continuously heating for primary dehydration; s103, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into an autoclave, performing second dehydration and drying, and performing carbonization-distillation-carbonization circulation to finish carbonization. The synthesis efficiency of the 2-hydroxy-3-naphthoic acid in the production and preparation process is improved, and the waste of raw materials and the production power consumption are reduced, so that the production cost is reduced.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a preparation method of 2-hydroxy-3-naphthoic acid.
Background
2-hydroxy-3-naphthoic acid is also called 2, 3 acid, is mainly used for preparing naphthol AS and other various intermediate of naphthol, and is also an intermediate for preparing medicines and organic pigments. In the prior art, the preparation process is relatively extensive, so that the synthesis efficiency of the 2-hydroxy-3-naphthoic acid in the production and preparation process is low, the purity of the product is influenced, raw material waste is caused, and meanwhile, the power consumption of production is high, and the control of the product cost is not facilitated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the preparation method of the 2-hydroxy-3-naphthoic acid, which improves the synthesis efficiency of the 2-hydroxy-3-naphthoic acid in the production and preparation process, ensures the product purity, and is beneficial to reducing the raw material waste and the production power consumption, thereby reducing the production cost.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a method for preparing 2-hydroxy-3-naphthoic acid comprises the following steps:
s101, putting 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate after the temperature in the pot is raised to be higher than 120 ℃, and obtaining liquid 2-naphthol;
s102, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to 120-naphthol and 150 ℃ for reaction to obtain a 2-naphthol sodium salt solution, and after the reaction is finished, vacuumizing the pot to negative pressure and then continuously heating for primary dehydration;
s103, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into an autoclave, performing carbonization-distillation-carbonization circulation after performing second dehydration and drying, discharging residual pressure in the autoclave after the carbonization is finished, adding hot water, stirring for dissolving, and continuously adding water until the autoclave is filled;
s104, pressing reactants dissolved in the high-pressure kettle into a resin barrel with a preset aqueous solution by using gas, then pumping into a neutralization barrel, controlling the temperature to be 50-65 ℃, adding dilute sulfuric acid to reduce the pH value to 4.5-6.8, then performing filter pressing, controlling the filter pressing pressure to be 0.1-0.4Mpa, returning a 2-naphthol filter cake obtained after filter pressing to the step S101, and heating the filtrate;
s105, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-5 ℃ under the stirring condition, adding sodium hydrosulfite, adding dilute sulfuric acid until the pH value is 2.1-2.7, and standing for more than 10 min;
s106, separating the upper wastewater of the acid precipitation barrel, and injecting the residual materials into an automatic centrifuge to obtain a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s107, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is more than or equal to 140 ℃, and the temperature of a mixing chamber is not less than 70 ℃ to obtain the product.
Further, in the step S101, the dehydration temperature is 130-155 ℃.
Further, in step S102, the dehydration temperature is less than or equal to 172 ℃ during the first dehydration.
Further, in step S102, the molar ratio of 2-naphthol to sodium hydroxide is within 1 ± 0.05.
Further, in step S103, the second dehydration specifically includes: gradually raising the temperature of the autoclave, and gradually opening a dehydration valve when the pressure in the autoclave reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the material is increased to 240 ℃, the pressure of the autoclave is quickly discharged, and when the pressure is reduced to 0.05MPa, the dehydration valve is closed.
Further, in step S103, the drying specifically includes: the material is dried for 30min at the temperature of 220 ℃ and 235 ℃ and the vacuum degree of-0.098 MPa.
Further, in step S103, the carbonization-distillation-carbonization cycle specifically includes: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is up to 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min;and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa.
Further, in step S104, the gas is CO 2 。
Further, in the steps S104 and S105, the concentration of the dilute sulfuric acid is 20% by volume.
Further, in the step S106, the operation program of the automatic centrifuge is set to feed 480S, wash 180S, dewater 240S, and discharge 120S.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, through a series of optimization on the production process and the raw material addition proportion, the synthesis efficiency of the 2-hydroxy-3-naphthoic acid in the production and preparation process is improved, the product purity is ensured, and simultaneously, the waste of raw materials and the production power consumption are reduced, so that the production cost is reduced.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
The invention discloses a preparation method of 2-hydroxy-3-naphthoic acid, which comprises the following steps:
s101, putting 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate after the temperature in the pot is raised to be higher than 120 ℃, and obtaining liquid 2-naphthol;
s102, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to 120-naphthol and 150 ℃ for reaction to obtain a 2-naphthol sodium salt solution, and after the reaction is finished, vacuumizing the pot to negative pressure and then continuously heating for primary dehydration;
s103, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into an autoclave, performing carbonization-distillation-carbonization circulation after performing second dehydration and drying, discharging residual pressure in the autoclave after the carbonization is finished, adding hot water, stirring for dissolving, and continuously adding water until the autoclave is filled;
s104, pressing reactants dissolved in the high-pressure kettle into a resin barrel with a preset aqueous solution by using gas, then pumping into a neutralization barrel, controlling the temperature to be 50-65 ℃, adding dilute sulfuric acid to reduce the pH value to 4.5-6.8, then performing filter pressing, controlling the filter pressing pressure to be 0.1-0.4Mpa, returning a 2-naphthol filter cake obtained after filter pressing to the step S101, and heating the filtrate;
s105, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-5 ℃ under the stirring condition, adding sodium hydrosulfite, adding dilute sulfuric acid until the pH value is 2.1-2.7, and standing for more than 10 min;
s106, separating the upper wastewater of the acid precipitation barrel, and injecting the residual materials into an automatic centrifuge to obtain a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s107, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is more than or equal to 140 ℃, and the temperature of a mixing chamber is not less than 70 ℃ to obtain the product.
Further, in the step S101, the dehydration temperature is 130-155 ℃. In step S102, the dehydration temperature is less than or equal to 172 ℃ during the first dehydration, and the molar ratio of the 2-naphthol to the sodium hydroxide is within 1 +/-0.05. In step S103, the second dehydration specifically includes: gradually raising the temperature of the autoclave, and gradually opening a dehydration valve when the pressure in the autoclave reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the materials rises to 240 ℃, quickly discharging pressure to the high-pressure kettle, and when the pressure is reduced to 0.05MPa, closing a dehydration valve; the drying specifically comprises the following steps: drying the materials for 30min at the temperature of 220 plus 235 ℃ and the vacuum degree of minus 0.098 MPa; the carbonization-distillation-carbonization cycle specifically comprises the following steps: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: to autoclaveIntroducing CO into the reactor 2 To make CO in the kettle 2 The pressure is up to 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min; and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa. In the step S104, the gas is CO 2 . In the steps S104 and S105, the concentration of the dilute sulfuric acid is 20% by volume. In the step S106, the operation program of the automatic centrifuge is set to feed 480S, wash 180S, dewater 240S, and discharge 120S.
Example 1
Preparation of 2-hydroxy-3-naphthoic acid S-1
S101, putting 500kg of 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate when the temperature in the pot is raised to be more than 120 ℃, wherein the dehydration temperature is 135 ℃, and obtaining liquid 2-naphthol;
s102, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to 120 ℃ for reaction to obtain a 2-naphthol sodium salt solution, vacuumizing the pot to negative pressure after the reaction is finished, continuing to heat for first dehydration, wherein the dehydration temperature is 150 ℃ during the first dehydration, and the molar ratio of the 2-naphthol to the sodium hydroxide is 0.95.
S103, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into a high-pressure kettle, and performing second dehydration: gradually raising the temperature of the autoclave, and gradually opening a dehydration valve when the pressure in the autoclave reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the materials rises to 240 ℃, quickly discharging pressure to the high-pressure kettle, and when the pressure is reduced to 0.05MPa, closing a dehydration valve; keeping the material temperature at 220 ℃ and 235 ℃ and the vacuum degree at-0.098 MPa, and drying for 30 min; carrying out carbonization-distillation-carbonization circulation, wherein the carbonization-distillation-carbonization circulation specifically comprises the following steps: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is up to 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min; and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa; after carbonization is finished, discharging the residual pressure in the kettle, adding hot water, starting stirring for dissolving, and continuously adding water until the autoclave is filled;
s104, utilizing CO to react the reactants dissolved in the autoclave 2 Pressing gas into a resin barrel with a preset aqueous solution, pumping the gas into a neutralization barrel, controlling the temperature at 50-55 ℃, adding dilute sulfuric acid with the volume fraction of 20%, reducing the pH value to 4.5-5.2, performing filter pressing, controlling the filter pressing pressure at 0.1-0.3Mpa, returning the 2-naphthol filter cake obtained after filter pressing to the step S101, and heating the filtrate;
s105, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-2 ℃ under the stirring condition, adding sodium hydrosulfite, adding 20 volume percent dilute sulfuric acid until the pH value is 2.1-2.5, and standing for more than 10 min;
s106, separating the upper wastewater of the acid precipitation barrel, and injecting the residual materials into an automatic centrifuge, wherein the working procedures of the automatic centrifuge are 480S of feeding, 180S of washing, 240S of dehydration and 120S of discharging, so as to obtain a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s107, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is 145 ℃, the temperature of a mixing chamber is 75 ℃, and obtaining the 2-hydroxy-3-naphthoic acid S-1, and detecting the yield and the purity of the 2-hydroxy-3-naphthoic acid S-1.
Example 2
Preparation of 2-hydroxy-3-naphthoic acid S-2
S201, putting 500kg of 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate when the temperature in the pot is raised to be more than 120 ℃, wherein the dehydration temperature is 145 ℃, and obtaining liquid 2-naphthol;
s202, adding 50% by mass of sodium hydroxide solution into a salt forming pot, adding liquid 2-naphthol under stirring, heating to 135 ℃ for reaction to obtain 2-naphthol sodium salt solution, vacuumizing the pot to negative pressure after the reaction is finished, continuing heating for first dehydration, wherein the dehydration temperature in the first dehydration is 170 ℃, and the molar ratio of 2-naphthol to sodium hydroxide is 1.
S203, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into a high-pressure kettle, and performing second dehydration: gradually raising the temperature of the autoclave, and gradually opening a dehydration valve when the pressure in the autoclave reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the materials rises to 240 ℃, quickly discharging pressure to the high-pressure kettle, and when the pressure is reduced to 0.05MPa, closing a dehydration valve; keeping the material temperature at 220 ℃ and 235 ℃ and the vacuum degree at-0.098 MPa, and drying for 30 min; carrying out carbonization-distillation-carbonization circulation, wherein the carbonization-distillation-carbonization circulation specifically comprises the following steps: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Maintaining the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 When the pressure reaches 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min; and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa; after carbonization is finished, discharging the residual pressure in the kettle, adding hot water, starting stirring for dissolving, and continuously adding water until the autoclave is filled;
s204, utilizing CO to react the reactants dissolved in the autoclave 2 Pressing gas into a resin barrel with a preset aqueous solution, then pumping the gas into a neutralization barrel, controlling the temperature at 55-60 ℃, adding 20% dilute sulfuric acid by volume fraction, reducing the pH value to 5.5-6.8, then performing filter pressing, controlling the filter pressing pressure at 0.2-0.4Mpa, returning the 2-naphthol filter cake obtained after filter pressing to the step S201, and heating the filtrate;
s205, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-5 ℃ under the stirring condition, adding sodium hydrosulfite, adding 20 volume percent dilute sulfuric acid until the pH value is 2.3-2.5, and standing for more than 10 min;
s206, separating the upper wastewater of the acid precipitation barrel, injecting the residual materials into an automatic centrifuge, wherein the working procedures of the automatic centrifuge are 480S of feeding, 180S of washing, 240S of dehydration and 120S of discharging, and obtaining a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s207, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is 150 ℃, the temperature of a mixing chamber is 80 ℃, and detecting the yield and the purity of the 2-hydroxy-3-naphthoic acid S-2.
Example 3
Preparation of 2-hydroxy-3-naphthoic acid S-3
S301, putting 500kg of 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate when the temperature in the pot is raised to be more than 120 ℃, and obtaining liquid 2-naphthol, wherein the dehydration temperature is 150 ℃;
s302, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to 145 ℃ for reaction to obtain a 2-naphthol sodium salt solution, vacuumizing the pot to negative pressure after the reaction is finished, continuing to heat for first dehydration, wherein the dehydration temperature in the first dehydration is 165 ℃, and the molar ratio of 2-naphthol to sodium hydroxide is 1.05.
S303, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into a high-pressure kettle, and performing second dehydration: for high pressure kettleGradually raising the temperature, and gradually opening a dehydration valve when the pressure in the kettle reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the materials rises to 240 ℃, quickly discharging pressure to the high-pressure kettle, and when the pressure is reduced to 0.05MPa, closing a dehydration valve; keeping the material temperature at 220 ℃ and 235 ℃ and the vacuum degree at-0.098 MPa, and drying for 30 min; carrying out carbonization-distillation-carbonization circulation, wherein the carbonization-distillation-carbonization circulation specifically comprises the following steps: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is up to 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min; and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa; after carbonization is finished, discharging the residual pressure in the kettle, adding hot water, starting stirring for dissolving, and continuously adding water until the autoclave is filled;
s304, utilizing CO to react the reactants dissolved in the autoclave 2 Pressing gas into a resin barrel with a preset aqueous solution, pumping the gas into a neutralization barrel, controlling the temperature to be 50-55 ℃, adding dilute sulfuric acid with the volume fraction of 20% to reduce the pH value to 4.8-6.2, then performing filter pressing, controlling the filter pressing pressure to be 0.2-0.3Mpa, returning a 2-naphthol filter cake obtained after filter pressing to the step S101, and heating the filtrate;
s305, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-3 ℃ under the stirring condition, adding sodium hydrosulfite, adding 20 volume percent dilute sulfuric acid until the pH value is 2.4-2.5, and standing for more than 10 min;
s306, separating the upper wastewater of the acid precipitation barrel, injecting the residual materials into an automatic centrifuge, wherein the working procedures of the automatic centrifuge are 480S of feeding, 180S of washing, 240S of dehydration and 120S of discharging, and obtaining a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s307, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is 155 ℃, the temperature of a mixing chamber is not lower than 85 ℃, obtaining 2-hydroxy-3-naphthoic acid S-3, and detecting the yield and the purity of the 2-hydroxy-3-naphthoic acid S-3.
Comparative example 1
The conventional production method is adopted, 500kg of 2-naphthol is added to prepare the 2-hydroxy-3-naphthoic acid, and the weighing and the purity detection are carried out.
By combining the data of examples 1-3 and comparative example 1, the data are shown in Table 1
TABLE 1 yield and purity of 2-hydroxy-3-naphthoic acid
| Item | Conventional production | Example 1 | Example 2 | Example 3 |
| Yield (kg) | 506.26 | 543.56 | 546.27 | 544.45 |
| Purity (%) | 96.68 | 99.21 | 99.35 | 99.29 |
By comparing the yield and the purity of the 2-hydroxy-3-naphthoic acid prepared in the above examples 1 to 3 with those of the 2-hydroxy-3-naphthoic acid prepared in the comparative example 1, the synthesis efficiency of the 2-hydroxy-3-naphthoic acid in the production and preparation process is greatly improved by a series of optimization on the production process and the raw material addition ratio, the yield is improved by more than 5%, the purity is also greatly improved, and the waste of the raw materials and the production power consumption are favorably reduced, so that the production cost is reduced.
Various other modifications and changes may be made by those skilled in the art based on the above-described technical solutions and concepts, and all such modifications and changes should fall within the scope of the claims of the present invention.
Claims (10)
1. A method for preparing 2-hydroxy-3-naphthoic acid comprises the following steps:
s101, putting 2-naphthol into a melting pot, starting heating, starting stirring to dehydrate after the temperature in the pot is raised to be higher than 120 ℃, and obtaining liquid 2-naphthol;
s102, adding a sodium hydroxide solution with the mass fraction of 50% into a salt forming pot, adding liquid 2-naphthol under the stirring condition, heating to 120-naphthol and 150 ℃ for reaction to obtain a 2-naphthol sodium salt solution, and after the reaction is finished, vacuumizing the pot to negative pressure and then continuously heating for primary dehydration;
s103, pressing the 2-naphthol sodium salt solution subjected to the first dehydration treatment into an autoclave, performing carbonization-distillation-carbonization circulation after performing second dehydration and drying, discharging residual pressure in the autoclave after the carbonization is finished, adding hot water, stirring for dissolving, and continuously adding water until the autoclave is filled;
s104, pressing reactants dissolved in the high-pressure kettle into a resin barrel with a preset aqueous solution by using gas, then pumping into a neutralization barrel, controlling the temperature to be 50-65 ℃, adding dilute sulfuric acid to reduce the pH value to 4.5-6.8, then performing filter pressing, controlling the filter pressing pressure to be 0.1-0.4Mpa, returning a 2-naphthol filter cake obtained after filter pressing to the step S101, and heating the filtrate;
s105, injecting the heated filtrate into an acid precipitation barrel, heating to 98 +/-5 ℃ under the stirring condition, adding sodium hydrosulfite, adding dilute sulfuric acid until the pH value is 2.1-2.7, and standing for more than 10 min;
s106, separating the upper wastewater of the acid precipitation barrel, and injecting the residual materials into an automatic centrifuge to obtain a dehydrated wet 2-hydroxy-3-naphthoic acid product;
s107, adding the dehydrated wet 2-hydroxy-3-naphthoic acid into a feeder for drying, wherein the inlet temperature of a heater is more than or equal to 140 ℃, and the temperature of a mixing chamber is not less than 70 ℃ to obtain the product.
2. The method according to claim 1, wherein the dehydration temperature in step S101 is 130-155 ℃.
3. The method of producing 2-hydroxy-3-naphthoic acid according to claim 1, wherein in the step S102, a dehydration temperature at the first dehydration is 172 ℃ or lower.
4. The process for producing 2-hydroxy-3-naphthoic acid according to claim 1, wherein: the molar ratio of the 2-naphthol to the sodium hydroxide in the step S102 is within 1 +/-0.05.
5. The method of claim 1, wherein in step S103, the second dehydration is specifically: gradually raising the temperature of the autoclave, and gradually opening a dehydration valve when the pressure in the autoclave reaches 0.17 MPa; when the pressure is increased to 0.26MPa, normal dehydration is started, and the pressure is controlled to be 0.26 +/-0.02 MPa; when the temperature of the material is increased to 240 ℃, the pressure of the autoclave is quickly discharged, and when the pressure is reduced to 0.05MPa, the dehydration valve is closed.
6. The method of producing 2-hydroxy-3-naphthoic acid as claimed in claim 1, wherein the drying in step S103 is specifically: the material is dried for 30min at the temperature of 220 ℃ and 235 ℃ and the vacuum degree of-0.098 MPa.
7. The method of producing 2-hydroxy-3-naphthoic acid according to claim 1, wherein in the step S103, the carbonization-distillation-carbonization cycle specifically comprises: and (3) trial carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 15 min; starting stirring, and adding CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; distillation I: discharging CO in the kettle 2 Vacuumizing under pressure to-0.098 MPa, and distilling for 60 min; carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 10 min; starting stirring, introducing CO 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 70 min; and (2) distilling: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (2) carbonizing: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is up to 0.7MPa, the stirring is started, and CO is introduced 2 Make CO in the kettle 2 Keeping the pressure at 0.4-0.7MPa for 20 min; and (3) distillation: discharging CO in the kettle 2 Vacuumizing under pressure until the vacuum degree is-0.096 MPa, and distilling; and (3) carbonization: introducing CO into the autoclave 2 To make CO in the kettle 2 The pressure is 0.7 MPa.
8. The method of claim 1, wherein in step S104, the gas is CO 2 。
9. The method of producing 2-hydroxy-3-naphthoic acid according to claim 1, wherein said steps S104 and S105 are performed by using dilute sulfuric acid having a concentration of 20% by volume.
10. The method of claim 1, wherein in step S106, the automatic centrifuge is programmed to feed 480S, wash 180S, dewater 240S, and discharge 120S.
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