CN114426260B - Improved process for producing sodium persulfate - Google Patents
Improved process for producing sodium persulfate Download PDFInfo
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- CN114426260B CN114426260B CN202210279815.2A CN202210279815A CN114426260B CN 114426260 B CN114426260 B CN 114426260B CN 202210279815 A CN202210279815 A CN 202210279815A CN 114426260 B CN114426260 B CN 114426260B
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
- C01B15/06—Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
- C01B15/08—Peroxysulfates
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Abstract
The invention discloses an improved process for producing sodium persulfate, which belongs to the technical field of sodium persulfate production and comprises the following steps of: adding ammonium persulfate and water into a stirring tank, stirring, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution at the same time, heating to a reaction temperature, preheating, and reacting to obtain sodium persulfate mother solution and ammonia gas; step two, the ammonia gas obtained in the step one is absorbed by the absorption liquid in the absorption tank; and thirdly, the sodium persulfate mother liquor obtained in the first step is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products. The improved process for producing sodium persulfate provided by the invention has the advantages that the steam generated by a reaction system is utilized to the maximum extent, the energy consumption is reduced, the loss of sodium persulfate in the production process is small, and the purity of the obtained sodium persulfate product is high.
Description
Technical Field
The invention belongs to the technical field of sodium persulfate production, and particularly relates to an improved process for producing sodium persulfate.
Background
Sodium persulfate is a strong oxidizing agent, and is widely used in the fields of electronics industry, petrochemical industry, textile industry, paper industry, environmental protection industry and the like because of its continuously stable oxidizing property, so that the market demand of sodium persulfate is particularly large.
The existing industrial production process route of sodium persulfate comprises the following steps: firstly, ammonium persulfate and aqueous solution of sodium hydroxide react, and then the obtained solution is subjected to deamination treatment, concentration crystallization, centrifugal separation and other procedures to obtain sodium persulfate crystals. In the production process of sodium persulfate, the mass fraction of sodium hydroxide is usually 32%. The alkali liquor with the mass fraction can cause high reaction liquid level in the kettle, higher reaction temperature and longer reaction time. However, sodium persulfate is unstable at high temperature and is decomposed, so that the purity of the subsequently obtained sodium persulfate is not high and generally does not exceed 99%. The existing sodium persulfate mother solution is generally subjected to primary crystallization separation after vacuum evaporation and then subjected to freezing crystallization separation, so that insufficient crystallization separation is easy to occur, and the loss of sodium persulfate products is caused.
Therefore, the invention provides an improved process for producing sodium persulfate, which reduces the reaction temperature of sodium persulfate and alkali liquor and shortens the reaction time by improving the mass concentration of the alkali liquor so as to improve the purity of sodium persulfate products and greatly improve the industrial production efficiency of sodium persulfate.
Disclosure of Invention
The invention aims to provide an improved process for producing sodium persulfate, which aims to solve the technical problems in the background art.
The aim of the invention can be achieved by the following technical scheme:
an improved process for producing sodium persulfate comprising the steps of:
adding ammonium persulfate and water into a stirring tank, stirring for 20-30min, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution, heating to a reaction temperature, preheating for 10min, and then reacting under (-0.08) - (-0.05 MPa) to obtain sodium persulfate mother liquor and ammonia gas, wherein the mass ratio of ammonium persulfate to sodium hydroxide is 18-22:10-15, the reaction temperature is 30-45 ℃, the reaction time is 3-6h, and the ammonium persulfate is recrystallized to remove impurities in the ammonium persulfate, and the mass fraction of the sodium hydroxide solution is 46-50%;
the ammonia gas obtained in the first step is absorbed by an absorption liquid in an absorption tank for recycling, wherein the absorption liquid is ammonium persulfate solution containing sulfuric acid;
and thirdly, the sodium persulfate mother liquor obtained in the first step is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products.
Further, in the third step, the temperature of the heat exchanger is set to 30-40 ℃.
Further, in the third step, the circulating evaporator comprises a cavity bag structure, an inner cavity is a flow channel of sodium persulfate mother liquor, an outer cavity is a steam flow channel, and when the sodium persulfate mother liquor flows through the inner cavity, the environment of the inner cavity is vacuum.
Further, in the third step, steam forms circulation in the heat exchanger and the circulation evaporator, the steam circulation returns to the circulation evaporator through the top of the crystallization separator by the steam compressor, heat in the steam is fully utilized, the heat of the steam is utilized efficiently, and energy consumption is reduced.
Further, the residual solution is returned to the sodium persulfate mother liquor, and the residual solution is circulated again under the actions of a heat exchanger, a circulating evaporator and a crystallization separator until the residual solution is distilled water.
The invention has the beneficial effects that:
1. the improved process for producing sodium persulfate provided by the invention enables the aggregate reaction and deamination to be carried out simultaneously in a reaction tank by adopting the reaction of ammonium persulfate and sodium hydroxide solution under (-0.08) - (-0.05 MPa), and the principle that the process can be carried out as follows is explained as follows: firstly, the environment of the reaction tank is a negative pressure environment, which is favorable for the ammonia to be separated from a reaction system, secondly, the mass fraction of sodium hydroxide is improved, the alkalinity of the reaction liquid is improved, the volatilization of ammonia is promoted, the production investment shows that the ammonia content in the obtained sodium persulfate mother liquor is little, and the sodium persulfate mother liquor contains a small amount of ammonia to be completely removed through the action of a vacuum pump in a circulation evaporator;
2. the invention improves the mass fraction of sodium hydroxide, has less water content and low reaction liquid level in the kettle, so that the reaction temperature is controlled to be 30-40 ℃, the decomposition of sodium persulfate is reduced, the purity of sodium persulfate products is improved, the purity of sodium persulfate products produced by the invention reaches more than 99%, the reaction time is shortened, and the production efficiency is improved;
3. according to the invention, the heat exchanger, the circulating evaporator and the crystallization separator are used together to act on the sodium persulfate mother liquor, and then the steam compressor is matched for use, so that the steam generated by the reaction system is utilized to the maximum extent, and the residual solution returns to the sodium persulfate mother liquor and passes through the heat exchanger, the circulating evaporator and the crystallization separator again, thereby reducing the loss of sodium persulfate and improving the yield of sodium persulfate products;
in summary, the improved process for producing sodium persulfate provided by the invention maximizes the utilization of the steam of the reaction system, reduces the energy consumption, has small sodium persulfate loss in the production process, and has high purity of the obtained sodium persulfate product.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of an improved process for producing sodium persulfate according to the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, an improved process flow chart for producing sodium persulfate according to the present invention comprises the following steps:
adding ammonium persulfate and water into a stirring tank, stirring, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution at the same time, heating to a reaction temperature, preheating, and reacting to obtain sodium persulfate mother solution and ammonia gas;
step two, the ammonia gas obtained in the step one is absorbed by the absorption liquid in the absorption tank;
and thirdly, the sodium persulfate mother liquor obtained in the first step is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products.
Example 1
An improved process for producing sodium persulfate comprising the steps of:
adding ammonium persulfate and water into a stirring tank, stirring for 20min, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution, heating to a reaction temperature, preheating for 10min, and then reacting at-0.08 MPa to obtain sodium persulfate mother solution and ammonia gas, wherein the mass ratio of sodium persulfate to sodium hydroxide is 18:10, the reaction temperature is 30 ℃, the reaction time is 6h, the mass ratio of ammonium persulfate to water is 1:1.5, and the mass fraction of sodium hydroxide solution is 46%;
the ammonia gas obtained in the first step is absorbed by an absorption liquid in an absorption tank, wherein the absorption liquid is ammonium persulfate solution containing sulfuric acid;
step three, the sodium persulfate mother liquor obtained in the step one is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products; the temperature of the heat exchanger is set to 30 ℃; the circulating evaporator comprises a cavity bag structure, wherein an inner cavity is a flow channel of sodium persulfate mother liquor, an outer cavity is a steam flow channel, and when the sodium persulfate mother liquor flows through the inner cavity, the environment of the inner cavity is vacuum; the steam forms circulation in the heat exchanger and the circulating evaporator, the steam circulation returns to the circulating evaporator through the top of the crystallization separator by the steam compressor, the residual solution returns to the sodium persulfate mother liquor, and the circulation is formed by the actions of the heat exchanger, the circulating evaporator and the crystallization separator again until the residual solution is distilled water.
The purity of the obtained sodium persulfate was tested to be 99.0%.
Example 2
An improved process for producing sodium persulfate comprising the steps of:
adding ammonium persulfate and water into a stirring tank, stirring for 20min, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution, heating to a reaction temperature, preheating for 10min, and then reacting at-0.06 MPa to obtain sodium persulfate mother solution and ammonia gas, wherein the mass ratio of sodium persulfate to sodium hydroxide is 20:13, the reaction temperature is 35 ℃, the reaction time is 4h, ammonium persulfate is ammonium persulfate after recrystallization treatment, the mass ratio of ammonium persulfate to water is 1:2, and the mass fraction of sodium hydroxide solution is 48%;
the ammonia gas obtained in the first step is absorbed by an absorption liquid in an absorption tank, wherein the absorption liquid is ammonium persulfate solution containing sulfuric acid;
step three, the sodium persulfate mother liquor obtained in the step one is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products; the temperature of the heat exchanger is set to 40 ℃; the circulating evaporator comprises a cavity bag structure, wherein an inner cavity is a flow channel of sodium persulfate mother liquor, an outer cavity is a steam flow channel, and when the sodium persulfate mother liquor flows through the inner cavity, the environment of the inner cavity is vacuum; the steam forms circulation in the heat exchanger and the circulating evaporator, the steam circulation returns to the circulating evaporator through the top of the crystallization separator by the steam compressor, the residual solution returns to the sodium persulfate mother liquor, and the circulation is formed by the actions of the heat exchanger, the circulating evaporator and the crystallization separator again until the residual solution is distilled water.
The purity of the obtained sodium persulfate was tested to be 99.2%.
Example 3
An improved process for producing sodium persulfate comprising the steps of:
adding ammonium persulfate and water into a stirring tank, stirring for 30min, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution, heating to a reaction temperature, preheating for 10min, and then reacting at-0.05 MPa to obtain sodium persulfate mother solution and ammonia gas, wherein the mass ratio of sodium persulfate to sodium hydroxide is 22:15, the reaction temperature is 45 ℃, the reaction time is 3h, the ammonium persulfate is ammonium persulfate after recrystallization treatment, the mass ratio of ammonium persulfate to water is 1:2.5, and the mass fraction of sodium hydroxide solution is 50%;
the ammonia gas obtained in the first step is absorbed by an absorption liquid in an absorption tank, wherein the absorption liquid is ammonium persulfate solution containing sulfuric acid;
step three, the sodium persulfate mother liquor obtained in the step one is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products; the temperature of the heat exchanger is set to 40 ℃; the circulating evaporator comprises a cavity bag structure, wherein an inner cavity is a flow channel of sodium persulfate mother liquor, an outer cavity is a steam flow channel, and when the sodium persulfate mother liquor flows through the inner cavity, the environment of the inner cavity is vacuum; the steam forms circulation in the heat exchanger and the circulating evaporator, the steam circulation returns to the circulating evaporator through the top of the crystallization separator by the steam compressor, the residual solution returns to the sodium persulfate mother liquor, and the circulation is formed by the actions of the heat exchanger, the circulating evaporator and the crystallization separator again until the residual solution is distilled water.
The purity of the obtained sodium persulfate was tested to be 99.3%.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (1)
1. An improved process for producing sodium persulfate comprising the steps of:
adding ammonium persulfate and water into a stirring tank, stirring for 20-30min, feeding the obtained mixture into a reaction tank, adding sodium hydroxide solution, heating to a reaction temperature, preheating for 10min, and reacting under negative pressure to obtain sodium persulfate mother solution and ammonia gas, wherein the mass fraction of the sodium hydroxide solution is 46-50%;
step two, the ammonia gas obtained in the step one is absorbed by the absorption liquid in the absorption tank;
step three, the sodium persulfate mother liquor obtained in the step one is subjected to the actions of a heat exchanger, a circulating evaporator and a crystallization separator to obtain wet sodium persulfate crystals and residual solution, and the wet sodium persulfate crystals are dried to obtain sodium persulfate products;
in the first step, ammonium persulfate is recrystallized to obtain ammonium persulfate; in the first step, the mass ratio of ammonium persulfate to sodium hydroxide is 18-22:10-15; the reaction temperature in the first step is 30-45 ℃; the reaction time in the first step is 3-6h; setting the temperature of the heat exchanger in the third step to be 30-40 ℃; the circulating evaporator in the third step comprises a cavity bag structure, wherein an inner cavity is a flow channel of sodium persulfate mother liquor, an outer cavity is a steam flow channel, when the sodium persulfate mother liquor flows through the inner cavity, the environment of the inner cavity is vacuum, steam in the third step forms circulation in the heat exchanger and the circulating evaporator, and the steam returns to the circulating evaporator through a steam compressor through the top of the crystallization separator; and in the third step, the residual solution is returned to the sodium persulfate mother liquor to form circulation until the residual solution is distilled water.
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Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1493723A (en) * | 1966-07-21 | 1967-09-01 | Air Liquide | Process for preparing sodium dipersulfate |
| EP0081063B1 (en) * | 1981-11-10 | 1985-07-10 | FMC Corporation | Method for producing sodium persulfate |
| TW416997B (en) * | 1998-03-30 | 2001-01-01 | Mitsubishi Gas Chemical Co | Process for producing persulfate |
| JP3832534B2 (en) * | 1998-04-07 | 2006-10-11 | 三菱瓦斯化学株式会社 | Method for producing sodium persulfate |
| JP2001003187A (en) * | 1999-06-21 | 2001-01-09 | Mitsubishi Gas Chem Co Inc | Production of sodium persulfate |
| CN100584746C (en) * | 2007-03-30 | 2010-01-27 | 西陇化工股份有限公司 | Deammonation Method in procedure for producing sodium persulfate |
| CN102320575B (en) * | 2011-08-26 | 2013-02-13 | 张小江 | Method for evaporating sodium persulfate at low temperature |
| CN108149274A (en) * | 2017-11-16 | 2018-06-12 | 铜陵泰富特种材料有限公司 | The method of novel ammonium sulfate production sodium peroxydisulfate |
| CN107720703B (en) * | 2017-11-29 | 2020-06-02 | 铜陵华兴精细化工股份有限公司 | Production process of sodium persulfate |
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