CN117602645A - Production process and system of food-grade potassium hydroxide - Google Patents

Production process and system of food-grade potassium hydroxide Download PDF

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Publication number
CN117602645A
CN117602645A CN202311653668.1A CN202311653668A CN117602645A CN 117602645 A CN117602645 A CN 117602645A CN 202311653668 A CN202311653668 A CN 202311653668A CN 117602645 A CN117602645 A CN 117602645A
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effect
potassium hydroxide
effect evaporator
sugar
evaporator
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CN202311653668.1A
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CN117602645B (en
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唐永兴
肖道兵
曹进
周金龙
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Jiangsu Aoxie Chemical Co ltd
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Jiangsu Aoxie Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D1/00Oxides or hydroxides of sodium, potassium or alkali metals in general
    • C01D1/04Hydroxides
    • C01D1/28Purification; Separation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/26Multiple-effect evaporating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D5/00Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • B01D5/006Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The application relates to a production process and a production system of food-grade potassium hydroxide, wherein soft white sugar solution is added in the process of producing 48% potassium hydroxide products by a three-effect countercurrent falling film evaporation system, so that the soft white sugar and chlorate can rapidly complete reaction at 155-165 ℃ to reduce the chlorate content in the 48% potassium hydroxide solution.

Description

Production process and system of food-grade potassium hydroxide
Technical Field
The application relates to the technical field of chemical production, in particular to a production process and a production system of food-grade potassium hydroxide.
Background
The formula milk powder is daily consumable for infants, the chlorate content of the potassium citrate used in the milk powder additive is too high, and the children intelligence is influenced, so that the chlorate content needs to be strictly controlled in the production process of the potassium citrate, and a 48% potassium hydroxide solution product is used as a production raw material of the food additive potassium citrate, and the chlorate content in the potassium hydroxide solution is strictly required, namely, the chlorate content in the 48% potassium hydroxide solution needs to be less than 10ppm. Potassium hydroxide is obtained by electrolyzing potassium chloride by an ion-exchange membrane method, and is obtained by electrolyzing saturated potassium chloride solution by an ion-exchange membrane method, chlorine gas is generated in an anode chamber, and hydrogen gas and 30% potassium hydroxide are generated in a cathode chamber. Meanwhile, a certain amount of side reaction exists in the cathode chamber and the anode chamber, chlorine reacts with cathode product potassium hydroxide to generate a small amount of potassium chlorate, and 30% potassium hydroxide generated by electrolysis is evaporated and concentrated to 48% potassium hydroxide product for sale. The potassium chlorate is further enriched in the evaporation concentration process of the potassium hydroxide solution, and the potassium chlorate content in the 48% potassium hydroxide solution is about 30-40ppm, so that the requirement of the production raw material of the food additive potassium citrate (48% potassium hydroxide) on the chlorate content being lower than 10ppm can not be met.
Disclosure of Invention
The purpose of the application is to overcome the defects of the prior art and provide a production process and a system of food-grade potassium hydroxide, wherein a soft white sugar solution is added in the process of producing 48% potassium hydroxide products by a three-effect countercurrent falling film evaporation device, so that the soft white sugar and chlorate can rapidly complete reaction at the temperature of 155-165 ℃ to reduce the chlorate content in the 48% potassium hydroxide solution.
According to the production process of the food-grade potassium hydroxide provided by the application, the production process specifically comprises the following steps:
the ratio of the sugar solution is as follows: cleaning a first sugar storage tank and a second sugar storage tank, respectively adding pure water and steam condensate into the first sugar storage tank and the second sugar storage tank, starting a stirrer to stir at the same time, and controlling the water temperature in the first sugar storage tank and the water temperature in the second sugar storage tank to be 50-55 ℃; adding edible soft white sugar with concentration of 10% -11%, stirring, and standing for 6-8 hr;
chlorate removal: the method comprises the steps of enabling potassium hydroxide solution with concentration of 28% -30% from an inlet at the top end of a three-effect evaporator to enter the three-effect evaporator, evaporating and concentrating the potassium hydroxide solution through the three-effect evaporator, enabling a purge valve on an inlet pipeline of the two-effect pump to be opened after entering the two-effect evaporator, starting a sugar solution metering pump, replacing a sugar solution pipeline from an outlet of the sugar solution metering pump to an inlet of the two-effect pump, closing the sugar solution metering pump after the pipeline is completely replaced, closing the purge valve, opening a sugar solution charging valve at the inlet of the two-effect pump, starting the sugar solution metering pump again, adding the sugar solution, enabling the potassium hydroxide solution to flow out of the two-effect evaporator and uniformly mix with the sugar solution through the two-effect pump and the one-effect heat exchanger, and then sending the potassium hydroxide solution into the top of the one-effect evaporator through the pipeline, and evaporating and concentrating the uniform mixed solution into potassium hydroxide solution with concentration of 50% in the one-effect evaporator;
and (3) precise filtration: conveying 50% potassium hydroxide solution evaporated and concentrated by a first-effect evaporator to a first alkali distribution tank and a second alkali distribution tank through a first-effect pump, a first-effect heat exchanger A, a second-effect heat exchanger A and a 50% potassium hydroxide solution cooler, adding pure water into the first alkali distribution tank and the second alkali distribution tank for accurate blending, blending 50% potassium hydroxide into 48% potassium hydroxide solution with qualified concentration, conveying the qualified potassium hydroxide solution into a filtering device through an alkali distribution pump, and obtaining a transparent 48% potassium hydroxide solution product after two-stage filtering;
the chlorate content in the prepared 48% potassium hydroxide solution product is less than 10ppm.
Preferably, in the chlorate removing step, the pressure of the solution in the first-effect evaporator is 150KPa, the pressure of the solution in the second-effect evaporator is-30 KPa, and the pressure of the solution in the third-effect evaporator is-90 KPa; the first-effect evaporator tube Cheng Caizhi and the second-effect evaporator tube Cheng Caizhi are nickel N6, the third-effect evaporator tube Cheng Caizhi is stainless steel 316L, and the shell side materials of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are carbon steel Q345R.
Preferably, in the chlorate removal step, the temperature of the three-effect evaporator is 70-80 ℃ and the temperature of the two-effect evaporator is 105-115 ℃; the temperature of the one-effect evaporator is 155-165 ℃.
Preferably, the two stage filtration cartridges are 2 microns and 1 micron, respectively.
Preferably, in the chlorate removal step, the uniform mixed solution enters a feed liquid distributor at the top of the one-effect evaporator through a pipeline with the length of 30 meters, and naturally flows down in a film shape along a vertical heat exchange pipe in the evaporator, so that the potassium hydroxide solution is boiled, and the chlorate and the sugar solution react more fully.
The application also comprises a production system of food-grade potassium hydroxide, which comprises a triple-effect evaporation system and a sugar adding system, wherein the triple-effect evaporation system comprises a first-effect evaporator, a second-effect evaporator, a triple-effect evaporator, a first-effect condensate recoverer, a second-effect condensate recoverer, a third-effect condensate recoverer, a surface condenser, a first vacuum pump, a second vacuum pump, a separating tank, a first-effect heat exchanger, a second-effect heat exchanger, a 50% potassium hydroxide solution cooler, a first-effect pump, a second-effect pump, a triple-effect pump and a flow regulating valve; the heat source inlet of the first-effect evaporator is externally connected with steam, the secondary steam of the first-effect evaporator is communicated with the second-effect evaporator, the secondary steam of the second-effect evaporator is communicated with the third-effect evaporator, the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are arranged in series, the third-effect evaporator is sequentially connected with the third-effect pump, the second-effect heat exchanger, the second-effect evaporator, the second-effect pump, the first-effect heat exchanger and the first-effect evaporator through pipelines, the outlet of the first-effect evaporator is provided with the first-effect pump, and the 50% potassium hydroxide solution cooler is arranged on the pipeline of the 50% potassium hydroxide solution outlet of the first-effect evaporator; the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are respectively provided with a first-effect condensate recoverer, a second-effect condensate recoverer and a third-effect condensate recoverer below, the third-effect evaporator is connected with the surface condenser through pipelines, the surface condenser is respectively connected with the first vacuum pump and the second vacuum pump through pipelines, the first vacuum pump and the second vacuum pump are connected with the separation tank through pipelines, and the flow regulating valve is arranged on an inlet pipeline of 28% -30% potassium hydroxide solution of the third-effect evaporator;
the sugar adding system comprises a first sugar storage tank, a second sugar storage tank, a first metering pump, a second metering pump, a clean discharging valve, a charging valve, a pulse damper, a pure water inlet valve I and a steam condensate water inlet valve, wherein the pulse damper is arranged on one side of the first metering pump and one side of the second metering pump, the charging valve and the clean discharging valve are sequentially arranged between pipelines of the second-effect pump and the sugar solution metering pump, the pure water inlet valve I and the steam condensate water inlet valve are arranged above the first sugar storage tank and the second sugar storage tank, and the sugar adding system is arranged between pipelines of the second-effect evaporator and the first-effect evaporator.
Preferably, a flowmeter and a check valve are also arranged between the pipelines of the two-way pump and the sugar solution metering pump.
Preferably, the first-effect heat exchanger comprises a first-effect heat exchanger A and a first-effect heat exchanger B, the second-effect heat exchanger comprises a second-effect heat exchanger A and a second-effect heat exchanger B, and the first-effect heat exchanger A and the first-effect heat exchanger B, the second-effect heat exchanger A and the second-effect heat exchanger B are all arranged in parallel; the first-effect heat exchanger and the second-effect heat exchanger are both plate heat exchangers.
Preferably, the 50% potassium hydroxide solution cooler comprises a 50% potassium hydroxide solution cooler A and a 50% potassium hydroxide solution cooler B, and the 50% potassium hydroxide solution cooler A and the 50% potassium hydroxide solution cooler B are arranged in parallel.
Preferably, the number of heat exchange tubes in the one-effect evaporator is 80, the tube wall thickness is 1.65mm, the diameter of the heat exchange tubes is 50mm, and the length of the heat exchange tubes is 7326mm.
Compared with the prior art, the application has the beneficial effects that:
firstly, soft sugar solution is added in the process of producing 48% potassium hydroxide products by a three-effect countercurrent falling film evaporation device, and the soft sugar solution can react sugar with chlorate at a lower temperature (155 ℃ -165 ℃), so that the chlorate content in 48% potassium hydroxide products is reduced.
Secondly, arranging a sugar adding system between pipelines of the two-effect evaporator and the one-effect evaporator, adding a soft white sugar solution with certain concentration and flow rate, so that the soft white sugar solution and the potassium hydroxide solution are uniformly mixed and have enough reaction time; a drain valve is also arranged in the sugar adding system, so that the sugar solution in the sugar adding system pipeline can be replaced, and the purity of the sugar solution is improved, thereby improving the quality of 48% potassium hydroxide solution products.
Thirdly, the sugar solution passes through the two-effect pump and the plate heat exchanger and then enters the inlet of the one-effect evaporator instead of directly entering the inlet of the one-effect evaporator from the sugar adding system, so that the inlet pressure of the two-effect pump is low, a common sugar solution metering pump can be selected, the equipment and the running cost are reduced, and the sugar and potassium hydroxide solution can be more uniformly mixed through the rotation of the impeller of the two-effect pump and the plate heat exchanger.
Fourthly, the material liquid distribution pipe at the top of the first-effect evaporator is improved, uniform mixed liquid enters the material liquid distributor at the top of the first-effect evaporator through a pipeline with the length of about 30 meters, the vertical heat exchange pipes in the evaporator naturally flow down in a film shape, 1.0MPa steam from the outside enters from the lower part of the shell side of the first-effect evaporator, the heat of the steam is transferred to potassium hydroxide solution on the inner wall of the heat exchange pipes through the outer walls of the 80 heat exchange pipes, the potassium hydroxide solution flows in a thin liquid film shape on the inner wall of the heat exchange pipes, and boils in the downward flowing process, so that chlorate and sugar react more fully.
Fifthly, the temperature of the potassium hydroxide solution rises and the reaction is aggravated in the downward flowing process by improving the pipe wall thickness, the pipe diameter and the number of the heat exchange pipes in the first-effect evaporator.
In the sixth chlorate removal step, because the viscosity of the sugar solution is higher, a pulse damper is arranged at one side of the sugar solution metering pump, so that the flow of the sugar solution is stable, and the quality of 48% potassium hydroxide solution products is improved.
Seventh, by providing a filter device, excess sugar in 48% potassium hydroxide was removed by two-stage filtration.
Drawings
Fig. 1 is an overall schematic diagram of a food-grade potassium hydroxide production system as set forth in the present application.
Illustration of: 1. a first effect evaporator; 2. a two-effect evaporator; 3. a triple effect evaporator; 4. a surface condenser; 5. a separation tank; 6. an alkali preparing tank I; 7. an alkali distribution tank II; 8. a filtering device; 9. a first sugar tank; 10. a second sugar tank; 11. a first-effect condensate recoverer; 12. a two-effect condensate recoverer; 13. a three-effect condensate recoverer; 14. a first-effect heat exchanger A; 15. a first-effect heat exchanger B; 16. a two-effect heat exchanger A; 17. a two-effect heat exchanger B; 18. a 50% potassium hydroxide solution cooler a; 19. a 50% potassium hydroxide solution cooler B; 20. a first-effect pump; 21. a two-effect pump; 22. a three-way pump; 23. a first metering pump; 24. a second metering pump; 25. a first vacuum pump; 26. a second vacuum pump; 27. an alkali preparing pump; 28. a flow meter; 29. a check valve; 30. a flow regulating valve; 31. a charging valve; 32. a purge valve; 33. a first metering pump outlet valve; 34. a first metering pump inlet valve; 35. a second metering pump outlet valve; 36. a second metering pump inlet valve; 37. a first sugar tank outlet valve; 38. a second outlet valve of the sugar tank; 39. a liquid inlet valve I; 40. a liquid inlet valve II; 41. a steam condensate inlet valve; 42. a pure water inlet valve I; 43. a first alkali distribution groove feeding valve; 44. a first alkali distribution groove and a second feeding valve; 45. an outlet valve of the alkali distribution tank I; 46. a second alkali distribution groove feeding valve II; 47. a first feed valve of the alkali distribution tank II; 48. an outlet valve of the alkali distribution tank II; 49. a steam condensate water switching valve; 50. a pulse damper; 51. a pure water inlet valve II; 52. and a pure water inlet valve III.
Detailed Description
In order to make the above objects, features and advantages of the present application more comprehensible, a detailed description of the embodiments accompanied with figures and examples is provided below.
In the description of the present application, it should be understood that, if there are terms such as "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc., these terms refer to the orientation or positional relationship based on the drawings, which are merely for convenience of description and simplification of description, and do not indicate or imply that the apparatus or element referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
In this application, unless explicitly stated and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly. For example, the two parts can be fixedly connected, detachably connected or integrated; the connection can be mechanical connection or electric signal connection; either directly or indirectly, through intermediaries, or both, may be in communication with each other or in interaction with each other, unless expressly defined otherwise. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.
It will be understood that if an element is referred to as being "fixed" or "disposed" on another element, it can be directly on the other element or intervening elements may also be present. If an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein, if any, are for descriptive purposes only and do not represent a unique embodiment.
Referring to fig. 1, fig. 1 shows a schematic diagram of a production system of food-grade potassium hydroxide in an embodiment of the present application. The food-grade potassium hydroxide production system provided by the embodiment of the application comprises a triple-effect evaporation system and a sugar adding system, wherein the triple-effect evaporation system comprises a first-effect evaporator 1, a second-effect evaporator 2, a triple-effect evaporator 3, a first-effect condensate recoverer 11, a second-effect condensate recoverer 12, a triple-effect condensate recoverer 13, a surface condenser 4, a first vacuum pump 25, a second vacuum pump 26, a separation tank 5, a first-effect heat exchanger, a second-effect heat exchanger, a 50% potassium hydroxide solution cooler, a first-effect pump 20, a second-effect pump 21, a third-effect pump 22 and a flow regulating valve 30; the heat source inlet of the first-effect evaporator 1 is externally connected with steam, the secondary steam of the first-effect evaporator 1 is communicated with the second-effect evaporator 2, the secondary steam of the second-effect evaporator 2 is communicated with the third-effect evaporator 3, the first-effect evaporator 1, the second-effect evaporator 2 and the third-effect evaporator 3 are arranged in series, the third-effect evaporator 3 is sequentially connected with the third-effect pump 22, the second-effect heat exchanger, the second-effect evaporator 2, the second-effect pump 21, the first-effect heat exchanger and the first-effect evaporator 1 through pipelines, the outlet of the first-effect evaporator 1 is provided with the first-effect pump 20, and the 50% potassium hydroxide solution cooler is arranged on the pipeline of the 50% potassium hydroxide solution outlet of the first-effect evaporator; the lower parts of the first-effect evaporator 1, the second-effect evaporator 2 and the third-effect evaporator 3 are respectively provided with a first-effect condensate recoverer 11, a second-effect condensate recoverer 12 and a third-effect condensate recoverer 13, the third-effect evaporator 3 is connected with the surface condenser 4 through pipelines, the surface condenser 4 is respectively connected with the first vacuum pump 25 and the second vacuum pump 26 through pipelines, the first vacuum pump 25 and the second vacuum pump 26 are connected with the separation tank 5 through pipelines, and the flow regulating valve 30 is arranged on an inlet pipeline of 28% -30% potassium hydroxide solution of the third-effect evaporator.
The sugar adding system comprises a first sugar storage tank 9, a second sugar storage tank 10, a first metering pump 23, a second metering pump 24, a drain valve 32, a charging valve 31, a pulse damper 50, a pure water inlet valve I42 and a steam condensate inlet valve 41, wherein the pulse damper 50 is arranged on one side of the first metering pump 23 and one side of the second metering pump 24, the charging valve 31 and the drain valve 32 are sequentially arranged between pipelines of the second metering pump 21 and the sugar solution metering pump, the pure water inlet valve I42 and the steam condensate inlet valve 41 are arranged above the first sugar storage tank 9 and the second sugar storage tank 10, and the sugar adding system is arranged between pipelines of the second-effect evaporator 2 and the first-effect evaporator 1.
In one embodiment, further, a flow meter 28 and a check valve 29 are provided between the piping of the two-way pump 21 and the sugar solution metering pumps 23,24.
In one embodiment, further, the first-effect heat exchanger comprises a first-effect heat exchanger A14 and a first-effect heat exchanger B15, the second-effect heat exchanger comprises a second-effect heat exchanger A16 and a second-effect heat exchanger B17, and the first-effect heat exchanger A14 and the first-effect heat exchanger B15, the second-effect heat exchanger A16 and the second-effect heat exchanger B17 are all arranged in parallel; the first-effect heat exchanger and the second-effect heat exchanger are both plate heat exchangers, and the first-effect heat exchanger adopts the plate heat exchangers, so that the sugar solution and the potassium hydroxide solution can be mixed more uniformly, and the reaction is more complete.
In one embodiment, further, the 50% potassium hydroxide solution cooler comprises a 50% potassium hydroxide solution cooler a18 and a 50% potassium hydroxide solution cooler B19, the 50% potassium hydroxide solution cooler a18 and the 50% potassium hydroxide solution cooler B19 being disposed in parallel.
In one embodiment, further, the number of heat exchange tubes in the first-effect evaporator 1 is 80, the tube wall thickness is 1.65mm, the diameter of the heat exchange tube is 50mm, and the length of the heat exchange tube is 7326mm. By the design, under the condition of ensuring heat exchange efficiency, the service life of the one-effect evaporator is prolonged, the sugar solution and chlorate in the potassium hydroxide solution can have sufficient reaction time, and the reaction can be more complete.
In one embodiment, further, according to actual requirements, in order to improve production efficiency, two sets of three-effect evaporation systems are arranged, and each set of three-effect evaporation system corresponds to two alkali distribution tanks.
In one embodiment, further, a first metering pump outlet valve 33 is disposed on one side of the first metering pump 23, a first metering pump inlet valve 34 is disposed on the other side, a second metering pump outlet valve 35 is disposed on one side of the second metering pump 24, a second metering pump inlet valve 36 is disposed on the other side, and the knob of the first metering pump 23 or the second metering pump 24 is adjusted according to the flow rate displayed by the flow meter 28 so as to achieve the required flow rate, wherein the first metering pump 23 and the second metering pump 24 are both diaphragm pumps.
In one embodiment, further, a first sugar tank outlet valve 37 is arranged on an outlet pipeline of the first sugar tank 9, a second sugar tank outlet valve 38 is arranged on an outlet pipeline of the second sugar tank 10, a first liquid inlet valve 39 and a second liquid inlet valve 40 are further arranged above the first sugar tank 9 and the second sugar tank 10, condensed water of the first effect evaporator 1 passes through the first effect condensate recoverer 11, the first effect heat exchanger B15 and the second effect heat exchanger B17, a steam condensed water switch valve 49 is arranged on a pipeline at the downstream of the second effect heat exchanger B17, and then the two branches are separated, one branch flows out of the boundary, the other branch provides steam condensed water for the sugar adding system through the steam condensed water inlet valve 41, the first liquid inlet valve 39 and the second liquid inlet valve 40 are respectively arranged on branches at the downstream of the steam condensed water inlet valve 41, and finally the steam condensed water flows into the first sugar tank 9 through the first liquid inlet valve 39 and flows into the second sugar tank 10 through the second liquid inlet valve 40.
Condensed water generated by the first-effect evaporator passes through the first-effect condensed water recoverer, the first-effect heat exchanger B and the second-effect heat exchanger B to form steam condensed water output at about 90 ℃; the 50% potassium hydroxide solution generated by the first-effect evaporator is output to a first alkali distribution tank 6 and a second alkali distribution tank 7 through pipelines after being cooled to below 50 ℃ through a first-effect pump, a first-effect heat exchanger A, a second-effect heat exchanger B and a 50% potassium hydroxide solution cooler, a first alkali distribution tank feeding valve 43 is arranged on a feeding pipeline of the first alkali distribution tank 6, a second alkali distribution tank feeding valve 47 is arranged on a feeding pipeline of the second alkali distribution tank 7, pipelines for connecting the two alkali distribution tanks are arranged above the first alkali distribution tank 6 and the second alkali distribution tank 7, a first alkali distribution tank feeding valve 44 and a second alkali distribution tank feeding valve 46 are arranged on the pipelines, pipelines for connecting the two alkali distribution tanks are also arranged at the lower ends of the first alkali distribution tank 6 and the second alkali distribution tank 7 close to the tank bottom, and an outlet valve 45, a second alkali distribution tank outlet valve 48 and an alkali distribution pump 27 are arranged on the pipelines; the upper parts of the first alkali distribution tank 6 and the second alkali distribution tank 7 are respectively provided with a pure water inlet valve II 51 and a pure water inlet valve III 52, and the addition of pure water from outside the boundary is controlled through the pure water inlet valve II 51 and the pure water inlet valve III 52 so as to accurately adjust the concentration of the potassium hydroxide solution.
The flow regulating valve 30 is used for regulating the flow of the potassium hydroxide solution with the concentration of 28-30% in the electrolysis process. The chlorate content in the 48% potassium hydroxide solution product prepared by the production system is less than 10ppm.
The embodiment of the application also provides a production process of food-grade potassium hydroxide, which comprises the following specific steps:
the ratio of the sugar solution is as follows: cleaning a first sugar storage tank 9 and a second sugar storage tank 10, respectively adding pure water and steam condensate into the first sugar storage tank 9 and the second sugar storage tank 10, simultaneously starting a stirrer to stir, and controlling the water temperature in the first sugar storage tank 9 and the second sugar storage tank 10 to be 50-55 ℃; then adding edible soft white sugar with the concentration of 10-11%, stirring uniformly, and standing for 6-8 hours.
Chlorate removal: the potassium hydroxide solution with the concentration of 28% -30% from the electrolysis process enters from an inlet at the top end of the three-effect evaporator 3, after the three-effect evaporator 3 is evaporated and concentrated, the potassium hydroxide solution passes through the three-effect pump 22 and the two-effect heat exchanger, enters the two-effect evaporator 2, a purge valve 32 on an inlet pipeline of the two-effect pump 21 is opened, sugar solution metering pumps 23 and 24 are started, sugar solution pipelines from the outlet of the sugar solution metering pumps to the inlet of the two-effect pump are replaced, after the pipelines are replaced completely, sugar solution metering pumps 23 and 24 are closed, the purge valve 32 is closed, a sugar solution charging valve 31 at the inlet of the two-effect pump is opened, sugar solution metering pumps 23 and 24 are started again, sugar solution is charged, the potassium hydroxide solution flows out of the two-effect evaporator 2 and is evenly mixed with the sugar solution through the two-effect pump 21 and the one-effect heat exchanger 14 and 15, the uniform mixed solution is fed into the top of the one-effect evaporator 1 through the pipelines, and the even mixed solution is evaporated and concentrated into the potassium hydroxide solution with the concentration of 50% in the one-effect evaporator 1.
And (3) precise filtration: the potassium hydroxide solution with the concentration of 50% evaporated and concentrated by the first-effect evaporator 1 is conveyed to the first alkali distribution tank 6 and the second alkali distribution tank 7 through the first-effect pump 20, the first-effect heat exchanger A14, the second-effect heat exchanger A16 and the 50% potassium hydroxide solution coolers 18 and 19, pure water is added into the first alkali distribution tank 6 and the second alkali distribution tank 7 for accurate blending, 50% potassium hydroxide is blended into 48% potassium hydroxide solution with the concentration qualified, the qualified potassium hydroxide solution is conveyed into the filtering device 8 through the alkali distribution pump 27, and a transparent potassium hydroxide solution product with the concentration of 48% is obtained after two-stage filtering.
Wherein, the concentration of the potassium hydroxide solution after evaporation concentration in the three-effect evaporator 3 is about 32%, the concentration of the potassium hydroxide solution after evaporation concentration in the two-effect evaporator 2 is about 40%, and the potassium hydroxide solution with the concentration of about 40% enters the one-effect evaporator 1 through the two-effect pump 21 and the one-effect heat exchanger; the outlet of the first-effect evaporator 1 is provided with a concentration detector, and when the concentration of the potassium hydroxide solution at the outlet of the first-effect evaporator reaches 50% on the concentration detector, a purge valve 32 on an inlet pipeline of the second-effect pump 21 is opened, and sugar solution metering pumps 23 and 24 are started. The sugar solution reacts with chlorate in the one-effect evaporator 1 to produce potassium chloride, carbon dioxide and water, and part of the carbon dioxide is dissolved in the potassium hydroxide solution to produce potassium carbonate. The 50% potassium hydroxide solution produced by the one-effect evaporator is conveyed to the 50% potassium hydroxide solution coolers 18,19, cooled to below 50 ℃ and then conveyed through the pipelines. The chlorate content in the prepared 48% potassium hydroxide solution product is less than 10ppm.
In one embodiment, in the chlorate removing step, the pressure of the solution in the first-effect evaporator 1 is 150KPa, the pressure of the solution in the second-effect evaporator 2 is-30 KPa, and the pressure of the solution in the third-effect evaporator 3 is-90 KPa; the first-effect evaporator tube Cheng Caizhi and the second-effect evaporator tube Cheng Caizhi are nickel N6, the third-effect evaporator tube Cheng Caizhi is stainless steel 316L, and the shell side materials of the first-effect evaporator, the second-effect evaporator and the third-effect evaporator are carbon steel Q345R.
In one embodiment, further, in the chlorate removing step, the temperature of the triple effect evaporator 3 is 70-80 ℃ and the temperature of the double effect evaporator 2 is 105-115 ℃; the temperature of the one-effect evaporator 1 is 155-165 ℃.
In one embodiment, further, a special set of filter devices 8 is provided, as the excess sugar solution would reduce the transparency of the 48% potassium hydroxide solution product, and the filter devices 8 employ two stages of filtration, PP pleated filter elements, with two stages of filtration having 2 microns and 1 micron filter elements, respectively.
In one embodiment, in the chlorate removing step, the uniform mixed solution enters the material liquid distributor at the top of the first-effect evaporator through a pipeline with the length of 30 meters, and naturally flows down in a film shape along the vertical heat exchange pipe in the evaporator, 1.0MPa steam from the outside enters from the lower part of the shell side of the first-effect evaporator, the thin liquid film in the heating pipe enables the potassium hydroxide solution to boil, and the chlorate and the sugar solution react more fully. This application carries out structural improvement to feed liquid distributor, and this feed liquid distributor includes tube sheet and head, is connected with a plurality of vertical interval arrangement's heat exchange tube entry section on the tube sheet, and heat exchange tube entry section up end stretches out the tube sheet upper surface, and the head is the open shell structure of lower extreme, and head confined up end is provided with the inlet pipe, and open lower terminal surface is connected at tube sheet upper surface and is formed cloth membrane cavity, and heat exchange tube top entry section is the cross opening.
In the prior art, the chlorate content is reduced by adding white granulated sugar, glucose and the like, and the application carries out related experimental study on the white granulated sugar and the glucose, and compares and analyzes the content of 48% potassium hydroxide chlorate obtained by the white granulated sugar and the glucose adopted in the application with the content of 48% potassium hydroxide chlorate obtained by the white granulated sugar and the glucose adopted in the prior art, and the detailed table is as follows:
because the experiment is carried out by using an open container, 48% potassium hydroxide solution is difficult to reach boiling temperature under certain conditions, the higher the temperature is, the higher the pressure is, and the normal pressure is, so that the temperature is difficult to reach 155-165 ℃ of a one-effect evaporator (the temperature in the one-effect evaporator is 155-165 ℃ because the gas phase pressure of potassium hydroxide solution in the one-effect evaporator is 0.15 MPa) when the experiment is carried out by using the open container, the higher the temperature is in a certain range from the aspect of the reaction principle, the higher the reaction is, the more complete the reaction is, and therefore, the highest temperature 152 ℃ adopted in the experiment is slightly lower than 155 ℃, thereby playing the role of guiding innovative production. As can be seen from the above table, the effect of using soft sugar in the present application is significantly better than that of white granulated sugar and glucose.
The following table shows experimental data of the present application on a triple effect countercurrent falling film evaporation device, specifically as follows:
as can be seen from the table, when the flow rate of the sugar solution in item 1 is relatively low, the chlorate content in the produced potassium hydroxide solution is 11ppm, which is not satisfactory, and when the actual feeding amount of the sugar solution is 4-6 times of the theoretical value, the reaction can be completed, and the chlorate content in the produced potassium hydroxide solution is less than 10ppm, which is satisfactory.
The 48% potassium hydroxide solution product of the present application has the following indexes:
sequence number Content Index (I) Unit (B)
1 KOH concentration ≤48
2 KClO in KOH 3 Content of <10 ppm
3 Cl in KOH - Content of <20 ppm
As can be seen from the above table, the process of the present application employs the addition of soft white sugar solution between the two-effect evaporator and the one-effect evaporator piping, and produces a 48% potassium hydroxide solution product having a desired chlorate content of less than 10ppm at a relatively low temperature.
The above examples merely represent a few embodiments of the present application, which are described in more detail and are not to be construed as limiting the scope of the invention. It should be noted that it would be apparent to those skilled in the art that various modifications and improvements could be made without departing from the spirit of the present application, which would be within the scope of the present application. Accordingly, the scope of protection of the present application is to be determined by the claims appended hereto.

Claims (10)

1. The production process of the food-grade potassium hydroxide is characterized by comprising the following specific steps of:
the ratio of the sugar solution is as follows: cleaning a first sugar storage tank (9) and a second sugar storage tank (10), respectively adding pure water and steam condensate into the first sugar storage tank (9) and the second sugar storage tank (10), and simultaneously starting a stirrer to stir, and controlling the water temperature in the first sugar storage tank (9) and the water temperature in the second sugar storage tank (10) to be 50-55 ℃; adding edible soft white sugar with concentration of 10% -11%, stirring, and standing for 6-8 hr;
chlorate removal: the potassium hydroxide solution with the concentration of 28% -30% from the electrolysis process enters from an inlet at the top end of a three-effect evaporator (3), after the three-effect evaporator (3) is subjected to evaporation concentration, the potassium hydroxide solution enters a two-effect evaporator (2) through a three-effect pump (22) and two-effect heat exchangers (16, 17), a discharging valve (32) on an inlet pipeline of the two-effect pump (21) is opened, a sugar solution metering pump (23, 24) is started, a sugar solution pipeline from an outlet of the sugar solution metering pump to an inlet of the two-effect pump is replaced, after the pipeline is replaced completely, the sugar solution metering pump (23, 24) is closed, the discharging valve (32) is closed, a sugar solution charging valve (31) at the inlet of the two-effect pump is opened, the sugar solution metering pump (23, 24) is started again, the sugar solution is charged, the potassium hydroxide solution flows out from the two-effect evaporator (2) and is uniformly mixed with the sugar solution through the two-effect pump (21) and the one-effect heat exchanger (14, 15), the uniform mixed solution is fed into the top of the one-effect evaporator (1) through the pipeline, and the uniform mixed solution is evaporated and concentrated into 50% potassium hydroxide solution in the one-effect evaporator (1);
and (3) precise filtration: conveying 50% potassium hydroxide solution evaporated and concentrated by a first-effect evaporator (1) to a first alkali distribution tank (6) and a second alkali distribution tank (7) through a first-effect pump (20), a first-effect heat exchanger A (14), a second-effect heat exchanger A (16) and 50% potassium hydroxide solution coolers (18 and 19), adding pure water into the first alkali distribution tank (6) and the second alkali distribution tank (7) for accurate blending, blending 50% potassium hydroxide into 48% potassium hydroxide solution with qualified concentration, conveying the qualified potassium hydroxide solution with the qualified concentration into a filtering device (8) through an alkali distribution pump (27), and obtaining a transparent 48% potassium hydroxide solution product after two-stage filtering;
the chlorate content in the prepared 48% potassium hydroxide solution product is less than 10ppm.
2. A process for producing food grade potassium hydroxide according to claim 1, wherein: in the chlorate removal step, the pressure of the solution in the first-effect evaporator (1) is 150KPa, the pressure of the solution in the second-effect evaporator (2) is-30 KPa, and the pressure of the solution in the third-effect evaporator (3) is-90 KPa; the first-effect evaporator tube Cheng Caizhi and the second-effect evaporator tube Cheng Caizhi are made of nickel N6, the tube side material of the third-effect evaporator tube (3) is made of stainless steel 316L, and the shell side materials of the first-effect evaporator tube (1), the second-effect evaporator tube (2) and the third-effect evaporator tube (3) are all made of carbon steel Q345R.
3. A process for producing food grade potassium hydroxide according to claim 1, wherein: in the chlorate removal step, the temperature of the three-effect evaporator (3) is 70-80 ℃, and the temperature of the two-effect evaporator (2) is 105-115 ℃; the temperature of the one-effect evaporator (1) is 155-165 ℃.
4. A process for producing food grade potassium hydroxide according to claim 1, wherein: in the precise filtering step, the filter cores of the two-stage filtration are respectively 2 microns and 1 micron.
5. A process for producing food grade potassium hydroxide according to claim 1, wherein: in the chlorate removal step, uniform mixed solution enters a feed liquid distributor at the top of the one-effect evaporator through a pipeline with the length of 30 meters, and naturally flows down in a film shape along a vertical heat exchange pipe in the evaporator, so that potassium hydroxide solution is boiled, and chlorate and sugar solution react more fully.
6. A system for producing food grade potassium hydroxide, characterized by: the system comprises a three-effect evaporation system and a sugar adding system, wherein the three-effect evaporation system comprises a first-effect evaporator (1), a second-effect evaporator (2), a three-effect evaporator (3), a first-effect condensate recoverer (11), a second-effect condensate recoverer (12), a three-effect condensate recoverer (13), a surface condenser (4), a first vacuum pump (25), a second vacuum pump (26), a separation tank (5), first-effect heat exchangers (14 and 15), second-effect heat exchangers (16 and 17), 50% potassium hydroxide solution coolers (18 and 19), a first-effect pump (20), a second-effect pump (21), a third-effect pump (22) and a flow regulating valve (30); the heat source inlet of the first-effect evaporator (1) is externally connected with steam, the secondary steam of the first-effect evaporator (1) is communicated with the second-effect evaporator (2), the secondary steam of the second-effect evaporator (2) is communicated with the third-effect evaporator (3), the first-effect evaporator (1), the second-effect evaporator (2) and the third-effect evaporator (3) are arranged in series, the third-effect evaporator (3) is sequentially connected with a third-effect pump (22), second-effect heat exchangers (16, 17), the second-effect evaporator (2), the second-effect pump (21), first-effect heat exchangers (14, 15) and the first-effect evaporator (1) through pipelines, an outlet of the first-effect evaporator (1) is provided with a first-effect pump (20), and 50% potassium hydroxide solution coolers (18, 19) are arranged on pipelines of a 50% potassium hydroxide solution outlet of the first-effect evaporator; the device comprises a first-effect evaporator (1), a second-effect evaporator (2) and a third-effect evaporator (3), wherein a first-effect condensate recoverer (11), a second-effect condensate recoverer (12) and a third-effect condensate recoverer (13) are respectively arranged below the first-effect evaporator, the second-effect evaporator and the third-effect evaporator (3), the third-effect evaporator (3) is connected with a surface condenser (4) through pipelines, the surface condenser (4) is respectively connected with a first vacuum pump (25) and a second vacuum pump (26) through pipelines, the first vacuum pump (25) and the second vacuum pump (26) are connected with a separation tank (5) through pipelines, and a flow regulating valve (30) is arranged on an inlet pipeline of 28% -30% potassium hydroxide solution of the third-effect evaporator;
the sugar adding system comprises a first sugar storage tank (9), a second sugar storage tank (10), a first metering pump (23), a second metering pump (24), a clean discharging valve (32), a feeding valve (31), a pulse damper (50), a pure water inlet valve I (42) and a steam condensate inlet valve (41), wherein the pulse damper (50) is arranged on one side of the first metering pump (23) and one side of the second metering pump (24), the feeding valve (31) and the clean discharging valve (32) are sequentially arranged between pipelines of a second pump (21) and sugar solution metering pumps (23, 24), the pure water inlet valve I (42) and the steam condensate inlet valve (41) are arranged above the first sugar storage tank (9) and the second sugar storage tank (10), and the sugar adding system is arranged between pipelines of a second evaporator (2) and a first evaporator (1).
7. A system for producing food grade potassium hydroxide according to claim 6, wherein: a flowmeter (28) and a check valve (29) are also arranged between the pipelines of the two-way pump (21) and the sugar solution metering pumps (23, 24).
8. A system for producing food grade potassium hydroxide according to claim 6, wherein: the first-effect heat exchanger comprises a first-effect heat exchanger A (14) and a first-effect heat exchanger B (15), the second-effect heat exchanger comprises a second-effect heat exchanger A (16) and a second-effect heat exchanger B (17), and the first-effect heat exchanger A (14) and the first-effect heat exchanger B (15), the second-effect heat exchanger A (16) and the second-effect heat exchanger B (17) are all arranged in parallel; the first-effect heat exchanger and the second-effect heat exchanger are both plate heat exchangers.
9. A system for producing food grade potassium hydroxide according to claim 6, wherein: the 50% potassium hydroxide solution cooler comprises a 50% potassium hydroxide solution cooler A (18) and a 50% potassium hydroxide solution cooler B (19), wherein the 50% potassium hydroxide solution cooler A (18) and the 50% potassium hydroxide solution cooler B (19) are arranged in parallel.
10. A system for producing food grade potassium hydroxide according to claim 6, wherein: the number of heat exchange tubes in the first-effect evaporator (1) is 80, the tube wall thickness is 1.65mm, the diameter of the heat exchange tubes is 50mm, and the length of the heat exchange tubes is 7326mm.
CN202311653668.1A 2023-12-05 2023-12-05 Production process and system of food-grade potassium hydroxide Active CN117602645B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1402202A (en) * 1972-01-17 1975-08-06 Hooker Chemicals Plastics Corp Removal of sodium chlorate from caustic soda solution
WO2015062393A1 (en) * 2013-10-28 2015-05-07 南通醋酸纤维有限公司 Solid-liquid separation process with multi-effect evaporation in combination with stirring evaporation
CN109264745A (en) * 2018-12-07 2019-01-25 青海盐湖工业股份有限公司 A kind of hydroxide flake potassium production method
CN209259708U (en) * 2018-12-07 2019-08-16 青海盐湖工业股份有限公司 A kind of hydroxide flake potassium production system
CN112481646A (en) * 2020-10-27 2021-03-12 江苏奥喜埃化工有限公司 Chlorate device is removed to potassium chloride salt water

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1402202A (en) * 1972-01-17 1975-08-06 Hooker Chemicals Plastics Corp Removal of sodium chlorate from caustic soda solution
WO2015062393A1 (en) * 2013-10-28 2015-05-07 南通醋酸纤维有限公司 Solid-liquid separation process with multi-effect evaporation in combination with stirring evaporation
CN109264745A (en) * 2018-12-07 2019-01-25 青海盐湖工业股份有限公司 A kind of hydroxide flake potassium production method
CN209259708U (en) * 2018-12-07 2019-08-16 青海盐湖工业股份有限公司 A kind of hydroxide flake potassium production system
CN112481646A (en) * 2020-10-27 2021-03-12 江苏奥喜埃化工有限公司 Chlorate device is removed to potassium chloride salt water

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