CN111777494B - Leaching and separating method for solid mixture of sodium phenolate and sodium hydroxide - Google Patents
Leaching and separating method for solid mixture of sodium phenolate and sodium hydroxide Download PDFInfo
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- CN111777494B CN111777494B CN202010666785.1A CN202010666785A CN111777494B CN 111777494 B CN111777494 B CN 111777494B CN 202010666785 A CN202010666785 A CN 202010666785A CN 111777494 B CN111777494 B CN 111777494B
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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
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
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- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
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- C01D1/34—Purification; Separation with selective solvents
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- C07C37/64—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring
- C07C37/66—Preparation of O-metal compounds with O-metal group bound to a carbon atom belonging to a six-membered aromatic ring by conversion of hydroxy groups to O-metal groups
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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
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Abstract
The invention relates to a method for leaching and separating a solid mixture of sodium phenolate and sodium hydroxide, in particular to a separation method for leaching and separating the solid mixture of the sodium phenolate and the sodium hydroxide by adopting a leaching, solid-liquid separation and evaporation desolventizing coupling technology and taking an acetone-water mixed solvent as a leaching agent. The separation method has reasonable process, simple and easy operation, low operation cost and high material utilization rate, and is a clean production method which meets the development requirement of green chemical industry.
Description
Technical Field
The invention relates to a leaching and separating method of a solid mixture of sodium phenolate and sodium hydroxide, in particular to a separating method for leaching and separating the solid mixture of the sodium phenolate and the sodium hydroxide by adopting a leaching, solid-liquid separation and evaporation desolventizing coupling technology and taking an acetone-water mixed solvent as a leaching agent.
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 the volatilization of phenol and protect phenolic hydroxyl groups from chemical reaction, sodium hydroxide is added into a phenol aqueous solution, so that phenol and sodium hydroxide react to generate sodium phenolate which is difficult to volatilize and has stable chemical properties. Meanwhile, in order to complete the reaction, an excess of sodium hydroxide is usually added, 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 technology for separating the solid mixture of sodium phenolate and sodium hydroxide is developed, the resource recycling of the sodium phenolate and the sodium hydroxide is realized, and meanwhile, no environmental pollution is generated, so that the method has wide application prospect and remarkable economic and social benefits.
Disclosure of Invention
The invention aims to solve the defects of the prior art, and provides a separation method of a solid mixture of sodium phenolate and sodium hydroxide, which is reasonable in research and development process, simple in method, low in cost, high in utilization rate of valuable components, clean and environment-friendly.
The technical scheme for realizing the purpose is as follows:
a method for leaching and separating solid mixture of sodium phenate and sodium hydroxide, in particular to a method for leaching and separating solid mixture of sodium phenate and sodium hydroxide by using an acetone-water mixed solvent as a leaching agent by adopting leaching, solid-liquid separation and evaporation desolventizing coupling technologies, wherein the leaching agent is recycled while the sodium phenate and the sodium hydroxide are obtained by separation, 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: in a leaching device, the acetone-water mixed solvent prepared in the previous step is used as a leaching agent to perform leaching operation on the sodium phenolate and sodium hydroxide solid mixture, so that the sodium phenolate in the solid-phase material is dissolved in the liquid phase, and the material after the leaching operation enters the next step;
(3) solid-liquid separation: in solid-liquid separation 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 phenolate or can be further processed to obtain a sodium hydroxide product, and the liquid-phase material enters the next step;
(4) decoloring and removing impurities: adding a decoloring and impurity-removing agent into the liquid-phase material obtained in the last step to perform decoloring and impurity-removing operation;
(5) solid-liquid separation: in solid-liquid separation equipment, performing solid-liquid separation on the material obtained in the previous step, wherein the solid-phase material is a decoloring and impurity-removing agent, and the liquid-phase material is subjected to the next step;
(6) and (3) evaporating and removing the solvent: in evaporation equipment, removing the solvent from the liquid-phase material obtained in the last step through evaporation operation, enabling the gas-phase material to enter the eighth step, and enabling the evaporation concentrate to enter the next step;
(7) and (3) drying: drying the evaporation concentrate obtained in the last step in drying equipment to obtain sodium phenolate;
(8) gas phase condensation: the gas phase material obtained in the sixth step is condensed into liquid state by a condenser, and the material can be used as a raw material for preparing the leaching agent in the first step.
Further, in the preparation process of the first-step leaching agent, the volume ratio of water to acetone is 1.0:100-10.0: 100.
Further 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.
In the fourth step of decolorizing and impurity removing, the adsorbent is activated carbon, diatomite or molecular sieve, or the mixture of two or three components, and the adsorbent may be powder, granule or fiber material.
Further, in the solid-liquid separation process of the third step and the fifth step, the solid-liquid separation apparatus may be any one of a filter press apparatus, a centrifugal filter apparatus, a blade type filter apparatus, a tubular filter apparatus and a vacuum filtration apparatus.
The evaporation concentration equipment adopted by the evaporation desolventizing of the sixth step can be atmospheric evaporation equipment or vacuum evaporation equipment.
Furthermore, the mass percent of the sodium phenolate in the solid mixture of the sodium phenolate and the sodium hydroxide is 20-80%.
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.
The main process equipment for realizing the invention is as follows: leaching equipment, solid-liquid separation equipment, evaporation equipment and the like.
The technical scheme has the advantages that: the method adopts the coupling technology of leaching, solid-liquid separation and evaporation desolventizing, and particularly takes an acetone-water mixed solvent containing a small amount of water as a leaching agent, so that the recycling of the leaching agent is realized while the mixture of sodium phenolate and sodium hydroxide is leached and separated. The concrete points are as follows:
(1) an acetone-water mixed solvent containing a small amount of water is used as an extracting agent. Sodium phenolate has a certain solubility in acetone and increases with increasing temperature, whereas sodium hydroxide is poorly soluble in acetone. Acetone is a suitable leaching agent in view of the selectivity of the leaching separation. However, the use of acetone as an extractant results in a leaching separation process that is of limited utility due to the limited solubility of sodium phenolate. The acetone-water mixed solvent containing a small amount of water is used as an extracting agent, so that the separation selectivity is reduced, but the solubility of the sodium phenolate 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) By adopting the evaporation desolventizing technology, the acetone-water mixed solvent obtained by condensing the gas-phase material can be used as the raw material of the leaching agent for recycling, thereby realizing the greenization and cleanness of the separation process.
The method is particularly suitable for separating and recycling the solid mixture of the sodium phenolate and the sodium hydroxide. The separation method has reasonable process, simple and easy operation, low operation cost and high material utilization rate, and is a clean production method which meets the development requirement 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 and the like.
A method for leaching and separating solid mixture of sodium phenate and sodium hydroxide, in particular to a method for leaching and separating solid mixture of sodium phenate and sodium hydroxide by using an acetone-water mixed solvent as a leaching agent by adopting leaching, solid-liquid separation and evaporation desolventizing coupling technologies, wherein the leaching agent is recycled while the sodium phenate and the sodium hydroxide are obtained by separation, and the method 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 operation on a sodium phenate and sodium hydroxide solid mixture, the ratio of the mass of the sodium phenate in the mixture to the volume of the leaching agent is 1.0kg:50L, the operation temperature is 60 ℃, the sodium phenate 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) decoloring and removing impurities: adding a decoloring and impurity-removing agent into the liquid-phase material obtained in the last step for decoloring and impurity-removing operation, wherein the adopted adsorbent is powdery diatomite;
(5) solid-liquid separation: in vacuum filtration equipment, performing solid-liquid separation on the material obtained in the previous step, wherein a solid-phase material is a decoloring and impurity-removing agent, and a liquid-phase material is subjected to the next step;
(6) and (3) evaporating and removing the solvent: in evaporation equipment, removing the solvent from the liquid-phase material obtained in the last step through evaporation operation, enabling the gas-phase material to enter the eighth step, and enabling the evaporation concentrate to enter the next step;
(7) and (3) drying: drying the evaporation concentrate obtained in the last step in drying equipment to obtain sodium phenolate;
(8) gas phase condensation: the gas phase material obtained in the sixth step is condensed into liquid state by a condenser, and the material can be used as a raw material for preparing the leaching agent in the first step.
Example two
The main process equipment is leaching equipment, solid-liquid separation equipment, evaporation equipment and the like.
A method for leaching and separating solid mixture of sodium phenate and sodium hydroxide, in particular to a method for leaching and separating solid mixture of sodium phenate and sodium hydroxide by using an acetone-water mixed solvent as a leaching agent by adopting leaching, solid-liquid separation and evaporation desolventizing coupling technologies, wherein the leaching agent is recycled while the sodium phenate and the sodium hydroxide are obtained by separation, and the method 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 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 56 ℃, 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) decoloring and removing impurities: adding a decoloring and impurity-removing agent into the liquid-phase material obtained in the last step for decoloring and impurity-removing operation, wherein the adopted adsorbent is granular activated carbon;
(5) solid-liquid separation: in a pipeline type solid-liquid separation device, performing solid-liquid separation on the material obtained in the previous step, wherein the solid-phase material is a decoloring and impurity-removing agent, and the liquid-phase material is subjected to the next step;
(6) and (3) evaporating and removing the solvent: in evaporation equipment, removing the solvent from the liquid-phase material obtained in the last step through evaporation operation, enabling the gas-phase material to enter the eighth step, and enabling the evaporation concentrate to enter the next step;
(7) and (3) drying: drying the evaporation concentrate obtained in the last step in drying equipment to obtain sodium phenolate;
(8) gas phase condensation: the gas phase material obtained in the sixth step is condensed into liquid state by a condenser, and the material can be used as a raw material for preparing the leaching agent in the first step.
EXAMPLE III
The main process equipment is leaching equipment, solid-liquid separation equipment, evaporation equipment and the like.
A method for leaching and separating solid mixture of sodium phenate and sodium hydroxide, in particular to a method for leaching and separating solid mixture of sodium phenate and sodium hydroxide by using an acetone-water mixed solvent as a leaching agent by adopting leaching, solid-liquid separation and evaporation desolventizing coupling technologies, wherein the leaching agent is recycled while the sodium phenate and the sodium hydroxide are obtained by separation, and the method 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 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 after 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) decoloring and removing impurities: adding a decoloring and impurity-removing agent into the liquid-phase material obtained in the last step for decoloring and impurity-removing operation, wherein the adopted adsorbent is a molecular sieve;
(5) solid-liquid separation: in a pipeline type solid-liquid separation device, performing solid-liquid separation on the material obtained in the previous step, wherein the solid-phase material is a decoloring and impurity-removing agent, and the liquid-phase material is subjected to the next step;
(6) and (3) evaporating and removing the solvent: in evaporation equipment, removing the solvent from the liquid-phase material obtained in the last step through evaporation operation, enabling the gas-phase material to enter the eighth step, and enabling the evaporation concentrate to enter the next step;
(7) and (3) drying: drying the evaporation concentrate obtained in the last step in drying equipment to obtain sodium phenolate;
(8) gas phase condensation: the gas phase material obtained in the sixth step is condensed into liquid state by a condenser, and the material can be used as a raw material for preparing the leaching agent in the first step.
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 (7)
1. A method for leaching and separating solid mixture of sodium phenate and sodium hydroxide adopts leaching, solid-liquid separation and evaporation desolventizing coupling technologies, uses an acetone-water mixed solvent as a leaching agent to leach and separate the solid mixture of the sodium phenate and the sodium hydroxide, and obtains the sodium phenate and the sodium hydroxide by separation and simultaneously recycles the leaching agent, 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: in a leaching device, the acetone-water mixed solvent prepared in the previous step is used as a leaching agent to perform leaching operation on the sodium phenolate and sodium hydroxide solid mixture, so that the sodium phenolate in the solid-phase material is dissolved in the liquid phase, and the material after the leaching operation enters the next step;
(3) solid-liquid separation: in solid-liquid separation 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 phenolate or can be further processed to obtain a sodium hydroxide product, and the liquid-phase material enters the next step;
(4) decoloring and removing impurities: adding a decoloring and impurity-removing agent into the liquid-phase material obtained in the last step to perform decoloring and impurity-removing operation;
(5) solid-liquid separation: in solid-liquid separation equipment, performing solid-liquid separation on the material obtained in the previous step, wherein the solid-phase material is a decoloring and impurity-removing agent, and the liquid-phase material is subjected to the next step;
(6) and (3) evaporating and removing the solvent: in evaporation equipment, removing the solvent from the liquid-phase material obtained in the last step through evaporation operation, enabling the gas-phase material to enter the eighth step, and enabling the evaporation concentrate to enter the next step;
(7) and (3) drying: drying the evaporation concentrate obtained in the last step in drying equipment to obtain sodium phenolate;
(8) gas phase condensation: the gas phase material obtained in the sixth step is condensed into liquid state by a condenser, and the material can be used as a raw material for preparing the leaching agent in the first step.
2. The process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, 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 process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, 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 process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, characterized in that: in the fourth step of decolorizing and impurity removing, the adsorbent is activated carbon, diatomite or molecular sieve, or the mixture of two or three components, and the adsorbent is powdered, granular or fibrous material.
5. The process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, characterized in that: in the third and fifth solid-liquid separation processes, the solid-liquid separation equipment is any one of pressure filtration equipment, centrifugal filtration equipment, blade type filtration equipment, pipeline type filtration equipment and vacuum filtration equipment.
6. The process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, characterized in that: and the evaporation equipment adopted by the sixth step of evaporation and desolventization is normal-pressure evaporation equipment or vacuum evaporation equipment.
7. The process according to claim 1 for the leaching separation of a solid mixture of sodium phenate and sodium hydroxide, characterized in that: the mass percent of the sodium phenolate in the solid mixture of the sodium phenolate and the sodium hydroxide is 20-80%.
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