CN112850653A - Method for increasing yield of sodium persulfate - Google Patents

Method for increasing yield of sodium persulfate Download PDF

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Publication number
CN112850653A
CN112850653A CN202110134792.1A CN202110134792A CN112850653A CN 112850653 A CN112850653 A CN 112850653A CN 202110134792 A CN202110134792 A CN 202110134792A CN 112850653 A CN112850653 A CN 112850653A
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container
sodium persulfate
solution
ammonium persulfate
reaction kettle
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CN202110134792.1A
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Inventor
谢益宁
郑南华
蒋彪
吴松
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Unitech Initiator Hefei Co ltd
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Unitech Initiator Hefei Co ltd
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Priority to CN202110134792.1A priority Critical patent/CN112850653A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055Peroxyhydrates; Peroxyacids or salts thereof
    • C01B15/06Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
    • C01B15/08Peroxysulfates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the technical field of sodium persulfate production, and discloses a method for improving the yield of sodium persulfate, which comprises the following steps: s1, adding ammonium persulfate into the container A, adding a proper amount of water into the container A, and fully stirring by using a stirring device to obtain an ammonium persulfate aqueous solution; s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into the container B, and adding a proper amount of sulfuric acid into the container B; when the sodium persulfate is prepared, the preparation of the sodium persulfate can be simplified, so that the preparation step of the sodium persulfate is simpler and more convenient, and the production of the sodium persulfate by a chemical enterprise is more convenient.

Description

Method for increasing yield of sodium persulfate
Technical Field
The invention relates to the technical field of sodium persulfate production, in particular to a method for increasing the yield of sodium persulfate.
Background
Sodium persulfate is also called high sodium sulfate, an inorganic matter, the outward appearance is white crystalline powder, odorless, can be dissolved in water, be used as bleaching agent, oxidizing agent, emulsion polymerization promoter, because sodium persulfate is by the large amount of needs in market, consequently, the chemical industry enterprise needs carry out the needs of a large amount of productions in order to satisfy the market to the ammonium persulfate, traditional sodium persulfate's the process of preparing is comparatively complicated, and when preparing sodium persulfate, cause the waste of a large amount of resources easily, be unfavorable for the chemical industry enterprise to spend a small amount of cost and prepare more sodium persulfate finished products.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for improving the yield of sodium persulfate, which solves the problems in the prior art.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: a method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding a proper amount of water into the container A, and fully stirring by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into the container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a proper amount of sodium hydroxide solution into the reaction kettle, and reacting at a certain temperature;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device for cooling;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a drying device for drying, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
Preferably, in the step S1, the ratio of the ammonium persulfate to the water in the container a is 1: 1, and the ammonium persulfate aqueous solution is obtained after fully stirring for 10min to 20min by using a stirring device.
Preferably, the container B in step S2 is a closed container.
Preferably, the ratio of the ammonium persulfate aqueous solution to the sodium hydroxide solution in the step S3 is 1: 2, the ammonium persulfate aqueous solution and the sodium hydroxide solution react at a temperature of 40 ℃ to 60 ℃, and a vibration device is utilized to vibrate the reaction kettle in the reaction process.
Preferably, the ratio of the ammonia gas generated in the step S3 to the sulfuric acid in the step S2 is 1: 2-4.
Preferably, the temperature of the cooling device in the step S6 is 2-5 ℃, and the cooling time of the solution is 6-10 h.
Preferably, the temperature of the drying device in the step S8 is 50-70 ℃, and the drying time is 1-2 h.
(III) advantageous effects
The invention provides a method for improving the yield of sodium persulfate, which has the following beneficial effects:
the method can simplify the preparation of sodium persulfate, so that the preparation steps of sodium persulfate are simpler and more convenient, and the production of sodium persulfate by chemical enterprises is more convenient.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding water accounting for 1: 1 of the ammonium persulfate into the container A, and fully stirring for 10min by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into a closed container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a sodium hydroxide solution which is 1: 2 of the ammonium persulfate aqueous solution into the reaction kettle, and reacting at the temperature of 40 ℃;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device at 2 ℃ for cooling for 6 h;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a 50 ℃ drying device for drying for 1h, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
The ratio of the ammonia gas generated in step S3 to the sulfuric acid in step S2 was 1: 2.
Example 2
A method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding water accounting for 1: 1 of the ammonium persulfate into the container A, and fully stirring for 13min by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into a closed container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a sodium hydroxide solution which is 1: 2 of the ammonium persulfate aqueous solution into the reaction kettle, and reacting at the temperature of 45 ℃;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device at 2 ℃ for cooling for 7 h;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a drying device at 55 ℃ for drying for 1.5h, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
The ratio of the ammonia gas generated in step S3 to the sulfuric acid in step S2 was 1: 2.5.
Example 3
A method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding water accounting for 1: 1 of the ammonium persulfate into the container A, and fully stirring for 15min by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into a closed container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a sodium hydroxide solution which is 1: 2 of the ammonium persulfate aqueous solution into the reaction kettle, and reacting at the temperature of 50 ℃;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device at 3 ℃ for cooling for 8 h;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a drying device at 60 ℃ for drying for 1.5h, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
The ratio of the ammonia gas generated in step S3 to the sulfuric acid in step S2 was 1: 3.
Example 4
A method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding water accounting for 1: 1 of the ammonium persulfate into the container A, and fully stirring for 18min by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into a closed container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, adding a sodium hydroxide solution in a ratio of 1: 2 to the ammonium persulfate aqueous solution into the reaction kettle, and reacting at the temperature of 55 ℃;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device at 4 ℃ for cooling for 9 h;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a 65 ℃ drying device for drying for 1.5h, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
The ratio of the ammonia gas generated in step S3 to the sulfuric acid in step S2 was 1: 3.
Example 5
A method for improving the yield of sodium persulfate, comprising the following steps:
s1, adding ammonium persulfate into the container A, adding water accounting for 1: 1 of the ammonium persulfate into the container A, and fully stirring for 20min by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into a closed container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a sodium hydroxide solution which is 1: 2 of the ammonium persulfate aqueous solution into the reaction kettle, and reacting at the temperature of 60 ℃;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device at 5 ℃ for cooling for 10 h;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a drying device at 70 ℃ for drying for 2h, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
The ratio of the ammonia gas generated in step S3 to the sulfuric acid in step S2 was 1: 4.
It is noted that, herein, relational terms such as first and second, and the like may be 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. Also, 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 appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A method for improving the yield of sodium persulfate, which is characterized by comprising the following steps:
s1, adding ammonium persulfate into the container A, adding a proper amount of water into the container A, and fully stirring by using a stirring device to obtain an ammonium persulfate aqueous solution;
s2, installing a pipeline with an ammonia gas sensor on the reaction kettle, extending one end of the pipeline into the container B, adding a proper amount of sulfuric acid into the container B, and connecting the container B into a preparation system of ammonium persulfate;
s3, injecting an ammonium persulfate aqueous solution into a reaction kettle, then adding a proper amount of sodium hydroxide solution into the reaction kettle, and reacting at a certain temperature;
s4, opening the reaction kettle when the ammonia gas sensor cannot monitor that ammonia gas is generated in the reaction kettle, enabling the solution in the reaction kettle to enter vacuum dehydrogenation equipment for dehydrogenation operation, and simultaneously opening the container B to enable the solution in the container B to enter a preparation system of ammonium persulfate;
s5, adding the solution subjected to vacuum dehydrogenation into a vacuum concentration device for high-speed evaporation concentration to a required concentration;
s6, putting the solution concentrated to the required concentration into a cooling device for cooling;
s7, placing the cooled solution into a centrifuge for centrifugal separation to obtain sodium persulfate crystals and liquid;
s8, putting the obtained sodium persulfate crystal into a drying device for drying, and drying to obtain a finished product of sodium persulfate;
s9, repeating the steps S5-S8 until no crystal is precipitated in the liquid in the step S7.
2. The method for increasing the production of sodium persulfate according to claim 1, wherein: and in the step S1, the ratio of the ammonium persulfate to the water in the container A is 1: 1, and the ammonium persulfate aqueous solution is obtained after fully stirring for 10-20 min by using a stirring device.
3. The method for increasing the production of sodium persulfate according to claim 1, wherein: the container B in the step S2 is a closed container.
4. The method for increasing the production of sodium persulfate according to claim 1, wherein: the ratio of the ammonium persulfate aqueous solution to the sodium hydroxide solution in the step S3 is 1: 2, the ammonium persulfate aqueous solution and the sodium hydroxide solution react at the temperature of 40-60 ℃, and a vibration device is utilized to vibrate the reaction kettle in the reaction process.
5. The method for increasing the production of sodium persulfate according to claim 1, wherein: the ratio of the ammonia gas generated in the step S3 to the sulfuric acid in the step S2 is 1: 2-4.
6. The method for increasing the production of sodium persulfate according to claim 1, wherein: the temperature of the cooling device in the step S6 is 2-5 ℃, and the cooling time of the solution is 6-10 h.
7. The method for increasing the production of sodium persulfate according to claim 1, wherein: the temperature of the drying device in the step S8 is 50-70 ℃, and the drying time is 1-2 h.
CN202110134792.1A 2021-01-29 2021-01-29 Method for increasing yield of sodium persulfate Pending CN112850653A (en)

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Application publication date: 20210528