CN111777495B - Method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene - Google Patents
Method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene Download PDFInfo
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- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
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- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/01—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis
- C07C37/055—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis the substituted group being bound to oxygen, e.g. ether group
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- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
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- C07—ORGANIC CHEMISTRY
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- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
Abstract
The invention relates to a method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol by toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining the phenol. The separation method of the invention fully utilizes the characteristics of the separated material system and the characteristics of the separation process, not only has simple and easy separation operation, low operation cost and high material utilization rate, but also is clean and environment-friendly, and is a clean production method which meets the development requirements of green chemical industry.
Description
Technical Field
The invention relates to a method for separating a solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining the phenol, and belongs to the technical field of chemical separation.
Background
The solid mixture of sodium phenolate and sodium hydroxide is obtained by reacting phenol with sodium hydroxide to produce sodium phenolate, evaporating and drying the sodium phenolate. In general, when phenol-containing materials are subjected to evaporation dehydration treatment, in order to reduce phenol volatilization and protect phenolic hydroxyl groups from chemical reaction, sodium hydroxide is added into a phenol aqueous solution to react phenol with the sodium hydroxide to generate sodium phenolate which is difficult to volatilize and has stable chemical properties. Also, in order to complete the reaction, the sodium hydroxide is usually in excess, so that a solid mixture of sodium phenolate and sodium hydroxide is formed after the evaporation dehydration and drying treatment.
At present, the method for processing solid mixture of sodium phenolate and sodium hydroxide is to add sulfuric acid or hydrochloric acid into the material to react with sodium hydroxide in the mixture to generate sodium salt (sodium sulfate, sodium chloride); meanwhile, sodium phenolate reacts with acid to generate free phenol, and the phenol is recovered by utilizing the characteristic of easy volatilization of the free phenol. The method mainly has the following problems:
(1) sulfuric acid or hydrochloric acid is added as a neutralizer in the separation process, so that acid is consumed;
(2) the added sulfuric acid or hydrochloric acid reacts with sodium hydroxide, and the sodium hydroxide in the material is also consumed;
(3) the treatment method has the outstanding problems that the added acid reacts with sodium hydroxide to generate sodium salt, the sodium salt has low utilization value, is difficult to recycle, can only be used as waste to carry out solid waste treatment, and the treatment difficulty of the solid waste is relatively high.
Therefore, the process for separating the sodium phenolate and the sodium hydroxide is reasonable in research and development process, simple in method, low in cost and high in utilization rate of valuable components, so that phenol and other materials can be recycled and recycled, and the process has industrial application value and remarkable economic and social benefits.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides a method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol by toluene, which has the advantages of reasonable research and development process, simple method, low cost, high utilization rate of valuable components, cleanness and environmental protection. The recycling of the sodium hydroxide, the leaching agent and the extracting agent is realized while the phenol is obtained by separation.
The technical scheme for realizing the purpose is as follows:
a method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining phenol, and is characterized by comprising the following steps:
(1) preparing a leaching agent: mixing acetone and water to prepare an acetone-water mixed solvent, and taking the acetone-water mixed solvent as an extracting agent to enter the next step;
(2) leaching sodium phenolate: leaching and separating the solid mixture of sodium phenolate and sodium hydroxide in a leaching device by using the leaching agent prepared in the previous step to dissolve the sodium phenolate in the solid material into a liquid phase, and feeding the material subjected to the leaching operation to the next step;
(3) solid-liquid separation: carrying out solid-liquid separation on the material obtained in the last step in solid-liquid separation equipment, wherein the solid phase is a crude sodium hydroxide product, the material can be directly used as a reactant in the process of converting phenol into sodium phenate, and can also be further processed to obtain a sodium hydroxide product, and the liquid phase material enters the next step;
(4) and (3) evaporating and removing the solvent: removing the solvent from the liquid-phase material obtained in the last step through evaporation operation in evaporation equipment, allowing the gas-phase material to enter the next step, and allowing the evaporation concentrate to enter the sixth step;
(5) gas phase condensation: condensing the gas-phase material obtained in the last step into liquid by a condenser, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(6) and (3) sulfuric acid neutralization: in a neutralization device, neutralizing the sodium phenolate subjected to the solvent removal by evaporation in the fourth step with sulfuric acid to generate phenol and sodium sulfate, and feeding the materials to the next step;
(7) and (3) extracting phenol: adding an extracting agent toluene into the material obtained in the last step in an extraction device for extraction operation, extracting phenol into an extraction phase, allowing the extraction phase material to enter the tenth step, and allowing the extraction raffinate phase material to enter the next step;
(8) evaporation and dehydration: evaporating and dehydrating the raffinate phase material obtained in the last step in evaporation equipment to obtain a sodium sulfate crude product, further recrystallizing and refining to obtain sodium sulfate, and feeding the evaporated gas phase material to the next step;
(9) gas phase condensation: condensing the gas-phase material obtained in the last step by a condenser to obtain water, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(10) and (3) rectifying and separating an extract phase: and (3) rectifying the extract phase material in the seventh step in a rectifying tower, wherein a toluene-water azeotrope is at the top of the tower, toluene is at the lateral line of the tower, phenol is at the bottom of the tower, the toluene-water azeotrope can be divided into toluene and water after condensation and layering, the separated toluene can be directly used as an extracting agent in the extraction operation in the seventh step, and the separated water can be used for preparing a leaching agent, so that the toluene and water can be recycled while sodium phenolate is obtained.
Furthermore, the volume ratio of water to acetone in the preparation process of the primary leaching agent is 1.0:100-10.0: 100.
Further, in the second leaching process, the ratio of the mass of the sodium phenate to the volume of the leaching agent in the mixture of the sodium phenate and the sodium hydroxide is 1.0kg:5.0L-1.0kg: 50L.
Further, in the third step of solid-liquid separation, the solid-liquid separation apparatus may be any one of a filter press apparatus, a centrifugal filter apparatus, a blade type filter apparatus, a pipeline type filter apparatus and a vacuum filtration apparatus.
Further, the evaporation apparatus of the fourth step and the eighth step may be an atmospheric evaporation apparatus or a vacuum evaporation apparatus.
Further, during the sixth step of sulfuric acid neutralization operation, the pH of the solution is neutralized to 5 to 6.
Further, the seventh extraction equipment is ultrasonic enhanced extraction equipment, the ultrasonic generator is any one of a probe type ultrasonic generator, an immersion type ultrasonic generator and a tank type ultrasonic generator, and the extraction operation process conditions are as follows: the volume ratio of the extracting agent to the material neutralized by sulfuric acid is 1.0L:1.0-1.0L:6.0L, the operation temperature is 10-60 ℃, and the ultrasonic action intensity is 0.2W/cm2-20.0W/cm2The ultrasonic frequency is 19kHz-80 kHz.
Further, the tenth step of the rectification separation process is continuous operation, the adopted rectification tower is a rectification tower with three discharge ports of the tower top, the tower bottom and the lateral line, reflux is arranged at the tower top, and gas phase discharge is carried out at the lateral line.
The main principle and characteristics of the application of the invention are as follows:
(1) utilizes the solubility difference of sodium phenolate and sodium hydroxide in acetone and water
Sodium phenolate and sodium hydroxide are both readily soluble in water, but sodium hydroxide is poorly soluble in acetone, whereas sodium phenolate has some solubility in acetone. The solubility of sodium phenolate in acetone increased with increasing temperature, and was about 22.0g/100ml under reflux conditions.
(2) Utilizes the solubility difference of sodium phenolate and sodium hydroxide in the acetone-water mixed solvent
In order to improve the solubility of sodium phenolate in the leaching agent, an acetone-water mixed solvent is innovatively developed as the leaching agent, namely a small amount of water is added into acetone, and the acetone-water mixed solvent can greatly improve the solubility of the sodium phenolate.
(3) Separating solid mixture of sodium phenolate and sodium hydroxide by leaching method
The acetone-water mixed solvent is used as a leaching agent, and sodium phenolate in the mixture is leached into a liquid phase through leaching operation, so that the separation of the sodium phenolate and the sodium hydroxide is realized.
(4) Separating leaching agent by evaporation
Because the sodium phenolate is not easy to generate chemical change after being heated and the sodium phenolate is not easy to volatilize as salt, the leaching agent can be separated by adopting an evaporation method to realize the separation of the sodium phenolate and the leaching agent. Sodium phenolate can be obtained through evaporation and drying treatment, and the leaching agent separated through evaporation can be recycled as a leaching agent raw material after being condensed by a condenser.
(5) Utilizes the characteristic that phenol is easily dissolved in toluene and water are not mutually soluble
The phenol is easily dissolved in toluene, and can be extracted from the water phase to the toluene phase by an extraction method; meanwhile, toluene and water are immiscible and layered at room temperature, and the toluene and the water can be separated by a phase separation method, so that phenol and a sodium sulfate aqueous solution can be separated by an extraction separation method using toluene as an extracting agent.
(6) Separating and recovering phenol by adopting rectification method
By utilizing the characteristic that the boiling point of phenol is higher than that of toluene, water and a toluene-water azeotrope, when a continuous rectifying tower with side line discharging is adopted for separation, the toluene-water azeotrope is at the top of the tower, the toluene is at the side line, and the phenol is at the bottom of the tower, so that the separation and recovery of the phenol are realized.
The main process equipment for realizing the invention is as follows: leaching equipment, solid-liquid separation equipment, evaporation equipment, extraction equipment, rectification equipment and the like.
The technical scheme has the advantages that: by adopting a leaching-extraction-rectification coupling technology, particularly taking an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent, the recycling of sodium hydroxide, the leaching agent and the extracting agent is realized while phenol is separated and recovered. The concrete points are as follows:
(1) an acetone-water mixed solvent containing a small amount of water is used as an extracting agent. The acetone-water mixed solvent containing a small amount of water is used as the leaching agent, so that the solubility of the sodium phenolate in the leaching agent is obviously increased, and the separation process still has higher selectivity. The sodium phenolate with the required purity can be obtained by adjusting the water content in the leaching agent, the solid-liquid ratio of the leaching operation, the leaching separation times and the like. The use of an acetone-water mixed solvent containing a small amount of water as the leaching agent not only makes the separation of the solid mixture of sodium phenate and sodium hydroxide technically feasible, but also makes the separation process economically advantageous.
(2) The separation process thoroughly overcomes the defects of the process for neutralizing and separating the sodium phenolate and the sodium hydroxide by adding acid, does not need to consume acid, does not lose the sodium hydroxide in materials, and does not generate sodium salt solid waste.
(3) The evaporation desolventizing technology is adopted, the operation is simple, the recovered solvent can be recycled as the raw material of the leaching agent, the resources are saved, and the waste discharge is greatly reduced.
(4) Toluene is used as an extracting agent to extract phenol, an oil phase and a water phase are separated by a phase separation method, the extracting agent toluene and water can be recycled, the separation operation is simple and easy to implement, and the energy consumption of the process is low.
(5) The continuous rectifying tower with the lateral line discharging function is adopted to separate and recycle phenol, and the toluene-water azeotrope, the toluene and the phenol can be respectively obtained at the tower top, the lateral line and the tower kettle, so that the separation of the phenol, the toluene and the water is realized, and the treatment efficiency and the energy utilization rate of the rectifying tower are obviously improved due to the adoption of the lateral line discharging and continuous operation.
The method of the invention is particularly suitable for separating and recovering phenol from a solid mixture of sodium phenolate and sodium hydroxide. The method makes full use of the characteristics of the separated material system and the characteristics of the separation process, not only has simple and easy separation operation and low operation cost, but also has high utilization rate of valuable components, and is a clean production method which meets the development requirements of green chemical industry.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
Example one
The main process equipment is leaching equipment, solid-liquid separation equipment, evaporation equipment, extraction equipment, rectification equipment and the like.
A method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining phenol, and is characterized by comprising the following steps:
(1) preparing a leaching agent: mixing acetone and water, wherein the volume ratio of water to acetone in the prepared leaching agent is 10.0:100, and the solvent serving as the leaching agent enters the next step;
(2) leaching sodium phenolate: in a leaching device, the acetone-water mixed solvent prepared in the previous step is used as a leaching agent to perform leaching separation operation on a sodium phenolate and sodium hydroxide solid mixture, the ratio of the mass of the sodium phenolate in the mixture to the volume of the leaching agent is 1.0kg:5.0L, the operation temperature is 40 ℃, the sodium phenolate in a solid-phase material is dissolved in a liquid phase, and the material subjected to the leaching operation enters the next step;
(3) solid-liquid separation: in vacuum filtration equipment, performing solid-liquid separation on the material obtained in the last step to obtain a solid-phase material which is a sodium hydroxide crude product, wherein the material can be directly used as a reactant in the process of converting phenol into sodium phenate, and can also be further processed to obtain a sodium hydroxide product, and the liquid-phase material enters the next step;
(4) and (3) evaporating and removing the solvent: removing the solvent from the liquid-phase material obtained in the last step through evaporation operation in evaporation equipment, allowing the gas-phase material to enter the next step, and allowing the evaporation concentrate to enter the sixth step;
(5) gas phase condensation: condensing the gas-phase material obtained in the last step into liquid by a condenser, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(6) and (3) sulfuric acid neutralization: fourthly, neutralizing the evaporated concentrate subjected to solvent removal by evaporation with sulfuric acid in a neutralization device until the pH value of the solution is 6.0, reacting the sulfuric acid with sodium phenolate to generate phenol and sodium sulfate, and enabling the material to enter the next step;
(7) and (3) extracting phenol: extracting in an immersed ultrasonic extraction device at 60 deg.C with the volume ratio of the extractant to the material neutralized with sulfuric acid of 1.0L:6.0L and ultrasonic action intensity of 20W/cm2Extracting phenol and dissolving the phenol into the extract liquor at the ultrasonic frequency of 19kHz, wherein the extract phase material enters the tenth step, and the raffinate phase material enters the next step;
(8) evaporation and dehydration: evaporating and dehydrating the raffinate phase material obtained in the last step in evaporation equipment to obtain a sodium sulfate crude product, further recrystallizing and refining to obtain sodium sulfate, and feeding the evaporated gas phase material to the next step;
(9) gas phase condensation: condensing the gas-phase material obtained in the last step by a condenser to obtain water, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(10) and (3) rectifying and separating an extract phase: and (3) rectifying the extract phase material in the seventh step in a rectifying tower, wherein a toluene-water azeotrope is at the top of the tower, toluene is at the lateral line of the tower, phenol is at the bottom of the tower, the toluene-water azeotrope can be divided into toluene and water after condensation and layering, the separated toluene can be directly used as an extracting agent in the extraction operation in the seventh step, and the separated water can be used for preparing a leaching agent, so that the toluene and water can be recycled while sodium phenolate is obtained.
Example two
The main process equipment is leaching equipment, solid-liquid separation equipment, evaporation equipment, extraction equipment, rectification equipment and the like.
A method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining phenol, and is characterized by comprising the following steps:
(1) preparing a leaching agent: mixing acetone and water, wherein the volume ratio of water to acetone in the prepared leaching agent is 1.0:100, and the solvent is used as the leaching agent to enter the next step;
(2) leaching sodium phenolate: in a leaching device, the acetone-water mixed solvent prepared in the previous step is used as a leaching agent to perform leaching separation operation on a sodium phenolate and sodium hydroxide solid mixture, the ratio of the mass of the sodium phenolate in the mixture to the volume of the leaching agent is 1.0kg:50L, the operation temperature is 60 ℃, the sodium phenolate in a solid-phase material is dissolved in a liquid phase, and the material subjected to the leaching operation enters the next step;
(3) solid-liquid separation: performing solid-liquid separation on the material obtained in the last step in a filter-press type solid-liquid separation device to obtain a solid-phase material which is a sodium hydroxide crude product, wherein the solid-phase material can be directly used as a reactant in the process of converting phenol into sodium phenolate or can be further processed to obtain a sodium hydroxide product, and the liquid-phase material is subjected to the next step;
(4) and (3) evaporating and removing the solvent: removing the solvent from the liquid-phase material obtained in the last step through evaporation operation in evaporation equipment, allowing the gas-phase material to enter the next step, and allowing the evaporation concentrate to enter the sixth step;
(5) gas phase condensation: condensing the gas-phase material obtained in the last step into liquid by a condenser, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(6) and (3) sulfuric acid neutralization: fourthly, neutralizing the evaporated concentrate subjected to solvent removal by evaporation with sulfuric acid in a neutralization device until the pH value of the solution is 5.0, reacting the sulfuric acid with sodium phenolate to generate phenol and sodium sulfate, and enabling the material to enter the next step;
(7) and (3) extracting phenol: extracting in immersed ultrasonic extractor with extractantThe volume ratio of the material neutralized by sulfuric acid in the last step is 1.0L to 1.0L, the operation temperature is 40 ℃, and the ultrasonic action intensity is 2.0W/cm2Extracting phenol and dissolving the phenol into the extract liquor at the ultrasonic frequency of 80kHz, wherein the extract phase material enters the tenth step, and the extract raffinate phase material enters the next step;
(8) evaporation and dehydration: evaporating and dehydrating the raffinate phase material obtained in the last step in evaporation equipment to obtain a sodium sulfate crude product, further recrystallizing and refining to obtain sodium sulfate, and feeding the evaporated gas phase material to the next step;
(9) gas phase condensation: condensing the gas-phase material obtained in the last step by a condenser to obtain water, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(10) and (3) rectifying and separating an extract phase: and (3) rectifying the extract phase material in the seventh step in a rectifying tower, wherein a toluene-water azeotrope is at the top of the tower, toluene is at the lateral line of the tower, phenol is at the bottom of the tower, the toluene-water azeotrope can be divided into toluene and water after condensation and layering, the separated toluene can be directly used as an extracting agent in the extraction operation in the seventh step, and the separated water can be used for preparing a leaching agent, so that the toluene and water can be recycled while sodium phenolate is obtained.
EXAMPLE III
The main process equipment is leaching equipment, solid-liquid separation equipment, evaporation equipment, extraction equipment, rectification equipment and the like.
A method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene, in particular to a method for separating and recovering phenol by adopting an acetone-water mixed solvent as a leaching agent and toluene as an extracting agent and adopting a leaching-extraction-rectification coupling technology, which realizes the recycling of the sodium hydroxide, the leaching agent and the extracting agent while separating and obtaining phenol, and is characterized by comprising the following steps:
(1) preparing a leaching agent: mixing acetone and water, wherein the volume ratio of water to acetone in the prepared leaching agent is 5.0:100, and the solvent serving as the leaching agent enters the next step;
(2) leaching sodium phenolate: in a leaching device, the acetone-water mixed solvent prepared in the previous step is used as a leaching agent to perform leaching separation operation on a sodium phenolate and sodium hydroxide solid mixture, the ratio of the mass of the sodium phenolate in the mixture to the volume of the leaching agent is 1.0kg:20L, the operation temperature is 50 ℃, the sodium phenolate in a solid-phase material is dissolved in a liquid phase, and the material subjected to the leaching operation enters the next step;
(3) solid-liquid separation: in blade type filtering equipment, performing solid-liquid separation on the material obtained in the last step to obtain a solid phase material which is a sodium hydroxide crude product, wherein the solid phase material can be directly used as a reactant in the process of converting phenol into sodium phenate, and can also be further processed to obtain a sodium hydroxide product, and the liquid phase material enters the next step;
(4) and (3) evaporating and removing the solvent: removing the solvent from the liquid-phase material obtained in the last step through evaporation operation in evaporation equipment, allowing the gas-phase material to enter the next step, and allowing the evaporation concentrate to enter the sixth step;
(5) gas phase condensation: condensing the gas-phase material obtained in the last step into liquid by a condenser, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(6) and (3) sulfuric acid neutralization: fourthly, neutralizing the evaporated concentrate subjected to solvent removal by evaporation with sulfuric acid in a neutralization device until the pH value of the solution is 5.4, reacting the sulfuric acid with sodium phenolate to generate phenol and sodium sulfate, and enabling the material to enter the next step;
(7) and (3) extracting phenol: extracting in an immersed ultrasonic extraction device at 30 deg.C with the volume ratio of the extractant to the material neutralized with sulfuric acid of 1.0L:2.0L and ultrasonic action intensity of 10W/cm2Extracting phenol and dissolving into the extract liquor at the ultrasonic frequency of 24kHz, wherein the extract phase material enters the tenth step, and the raffinate phase material enters the next step;
(8) evaporation and dehydration: evaporating and dehydrating the raffinate phase material obtained in the last step in evaporation equipment to obtain a sodium sulfate crude product, further recrystallizing and refining to obtain sodium sulfate, and feeding the evaporated gas phase material to the next step;
(9) gas phase condensation: condensing the gas-phase material obtained in the last step by a condenser to obtain water, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(10) and (3) rectifying and separating an extract phase: and (3) rectifying the extract phase material in the seventh step in a rectifying tower, wherein a toluene-water azeotrope is at the top of the tower, toluene is at the lateral line of the tower, phenol is at the bottom of the tower, the toluene-water azeotrope can be divided into toluene and water after condensation and layering, the separated toluene can be directly used as an extracting agent in the extraction operation in the seventh step, and the separated water can be used for preparing a leaching agent, so that the toluene and water can be recycled while sodium phenolate is obtained.
Besides the above examples, the present invention has many embodiments, and all the technical solutions using equivalent or equivalent substitution are within the protection scope of the present invention.
Claims (8)
1. A method for separating solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene is characterized in that an acetone-water mixed solvent is used as a leaching agent, the toluene is used as an extracting agent, the phenol is separated and recovered by adopting a leaching-extraction-rectification coupling technology, and the recycling of the sodium hydroxide, the leaching agent and the extracting agent is realized while the phenol is separated and obtained, and the method is characterized by comprising the following steps:
(1) preparing a leaching agent: mixing acetone and water to prepare an acetone-water mixed solvent, and taking the acetone-water mixed solvent as an extracting agent to enter the next step;
(2) leaching sodium phenolate: leaching and separating the solid mixture of sodium phenolate and sodium hydroxide in a leaching device by using the leaching agent prepared in the previous step to dissolve the sodium phenolate in the solid material into a liquid phase, and feeding the material subjected to the leaching operation to the next step;
(3) solid-liquid separation: carrying out solid-liquid separation on the material obtained in the last step in solid-liquid separation equipment, wherein the solid phase is a crude sodium hydroxide product, the material can be directly used as a reactant in the process of converting phenol into sodium phenate, and can also be further processed to obtain a sodium hydroxide product, and the liquid phase material enters the next step;
(4) and (3) evaporating and removing the solvent: removing the solvent from the liquid-phase material obtained in the last step through evaporation operation in evaporation equipment, allowing the gas-phase material to enter the next step, and allowing the evaporation concentrate to enter the sixth step;
(5) gas phase condensation: condensing the gas-phase material obtained in the last step into liquid by a condenser, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(6) and (3) sulfuric acid neutralization: in a neutralization device, neutralizing the sodium phenolate subjected to the solvent removal by evaporation in the fourth step with sulfuric acid to generate phenol and sodium sulfate, and feeding the materials to the next step;
(7) and (3) extracting phenol: adding an extracting agent toluene into the material obtained in the last step in an extraction device for extraction operation, extracting phenol into an extraction phase, allowing the extraction phase material to enter the tenth step, and allowing the extraction raffinate phase material to enter the next step;
(8) evaporation and dehydration: evaporating and dehydrating the raffinate phase material obtained in the last step in evaporation equipment to obtain a sodium sulfate crude product, further recrystallizing and refining to obtain sodium sulfate, and feeding the evaporated gas phase material to the next step;
(9) gas phase condensation: condensing the gas-phase material obtained in the last step by a condenser to obtain water, wherein the material can be used as a raw material for preparing the leaching agent in the first step;
(10) and (3) rectifying and separating an extract phase: and (3) rectifying the extract phase material in the seventh step in a rectifying tower, wherein a toluene-water azeotrope is at the top of the tower, toluene is at the lateral line of the tower, phenol is at the bottom of the tower, the toluene-water azeotrope can be divided into toluene and water after condensation and layering, the separated toluene can be directly used as an extracting agent in the extraction operation in the seventh step, and the separated water can be used for preparing a leaching agent, so that the toluene and water can be recycled while sodium phenolate is obtained.
2. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: in the first-step leaching agent preparation process, the volume ratio of water to acetone is 1.0:100-10.0: 100.
3. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: in the second leaching process, the ratio of the mass of the sodium phenate in the mixture of the sodium phenate and the sodium hydroxide to the volume of the leaching agent is 1.0kg:5.0L-1.0kg: 50L.
4. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: in the third step of solid-liquid separation, the solid-liquid separation equipment is any one of filter pressing equipment, centrifugal filter equipment, blade type filter equipment, pipeline type filter equipment and vacuum filtration equipment.
5. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: the evaporation equipment in the fourth step and the eighth step is normal pressure evaporation equipment or vacuum evaporation equipment.
6. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: during the sixth sulfuric acid neutralization step, the solution is neutralized to a pH of 5-6.
7. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: the seventh step of toluene extraction equipment is ultrasonic enhanced extraction equipment, the ultrasonic generating device is any one of a probe type ultrasonic generator, an immersed type ultrasonic generator and a groove type ultrasonic generator, and the process conditions of the extraction operation are as follows: the volume ratio of the extracting agent to the material neutralized by sulfuric acid is 1.0L:1.0-1.0L:6.0L, the operation temperature is 10-60 ℃, and the ultrasonic action intensity is 0.2W/cm2-20.0W/cm2The ultrasonic frequency is 19kHz-80 kHz.
8. The method for separating the solid mixture of sodium phenolate and sodium hydroxide and extracting, separating and recovering phenol from toluene according to claim 1, characterized in that: the tenth step of the rectification separation process is continuous operation, the adopted rectification tower is a rectification tower with three discharge ports of the tower top, the tower bottom and the lateral line, the tower top is provided with reflux, and the lateral line is gas phase discharge.
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