CN111574357B - Method and device for preparing sodium acetate by using acetic acid wastewater - Google Patents

Method and device for preparing sodium acetate by using acetic acid wastewater Download PDF

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Publication number
CN111574357B
CN111574357B CN202010487426.XA CN202010487426A CN111574357B CN 111574357 B CN111574357 B CN 111574357B CN 202010487426 A CN202010487426 A CN 202010487426A CN 111574357 B CN111574357 B CN 111574357B
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acetic acid
box
acid wastewater
sodium acetate
freezing
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CN111574357A (en
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蒋其明
钱春龙
李爱红
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Jiangsu Aolikai Food Technology Co.,Ltd.
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Wuxi Yangshan Biochemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/22Evaporating by bringing a thin layer of the liquid into contact with a heated surface
    • B01D1/222In rotating vessels; vessels with movable parts
    • B01D1/223In rotating vessels; vessels with movable parts containing a rotor
    • B01D1/225In rotating vessels; vessels with movable parts containing a rotor with blades or scrapers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • B01D9/0013Crystallisation cooling by heat exchange by indirect heat exchange
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01FMIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80Mixing plants; Combinations of mixers
    • B01F33/83Mixing plants specially adapted for mixing in combination with disintegrating operations
    • B01F33/831Devices with consecutive working receptacles, e.g. with two intermeshing tools in one of the receptacles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053Details of the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0086Processes carried out with a view to control or to change the pH-value; Applications of buffer salts; Neutralisation reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives
    • C07C51/43Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00092Tubes

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
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  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a method and a device for preparing sodium acetate by using acetic acid wastewater, wherein the method for preparing sodium acetate by using acetic acid wastewater comprises the following steps: filtering acetic acid wastewater; neutralizing the filtered acetic acid wastewater with caustic soda; filtering the product after the neutralization reaction to obtain a filtrate; evaporating and concentrating the filtrate to obtain concentrated mother liquor; the concentrated mother liquor is crystallized, and the crystals and the mother liquor are separated by a centrifugal machine to obtain sodium acetate crystals; the sodium acetate preparation device comprehensively utilizes the heat release and heat absorption processes in all the working procedures to preheat and pre-cool water, thereby being beneficial to the comprehensive utilization of energy and saving the preparation energy.

Description

Method and device for preparing sodium acetate by using acetic acid wastewater
Technical Field
The invention relates to the technical field of sodium acetate production, in particular to a method and a device for preparing sodium acetate by using acetic acid wastewater.
Background
In the production of glacial acetic acid, a certain amount of acetic acid wastewater can be generated in the acetic acid refining link due to rectification and concentration. The substances contained in the acetic acid wastewater mainly comprise acetic acid, formic acid, acetaldehyde, miscellaneous lipid and other substances, generally, the total acid content in the acetic acid wastewater is about 33 percent (wherein the acetic acid content is about 30 percent, and the formic acid content is about 3 percent), and the content of the acetaldehyde, miscellaneous lipid and other organic impurities is less than 66 percent. In most glacial acetic acid production devices, acetic acid wastewater is directly discharged as one of three industrial wastes. Thereby causing the reduction of the pH value of the wastewater in the main drainage ditch and causing environmental pollution.
Sodium acetate is industrially useful for measuring lead, zinc, aluminum, iron, cobalt, antimony, nickel, tin. The compound is used as an esterification agent for organic synthesis, and is used in the aspects of photographic medicines, printing and dyeing mordants, buffering agents, chemical reagents, meat preservation, pigments, tanning and the like.
The sodium acetate laboratory is usually prepared by the following method: adding proper amount of sodium carbonate or caustic soda into 15-40% dilute acetic acid to produce neutralization, and evaporating the reacted solution to concentrate and crystallize sodium acetate. In industrial production, sodium acetate is also generally produced by using this principle, but the raw material of acetic acid needs to be purchased.
Disclosure of Invention
The invention provides a method and a device for preparing sodium acetate by using acetic acid wastewater, which aim to save acetic acid raw materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of sodium acetate is characterized by comprising the following steps:
s1: filtering the acetic acid wastewater to remove impurities in the acetic acid wastewater;
s2: neutralizing the filtered acetic acid wastewater with caustic soda, wherein the temperature of the neutralization reaction is controlled to be between 55 and 65 ℃;
s3: when the pH value of the reaction liquid of the neutralization reaction is 7.5-8, filtering the product after the neutralization reaction, and removing filter residues to obtain a filtrate;
s4: evaporating and concentrating the filtrate to obtain concentrated mother liquor;
s5: crystallizing the concentrated mother liquor at 40-50 deg.c;
s6: separating the crystals and the mother liquor by a centrifuge, collecting and packaging the crystals, and recrystallizing the mother liquor again.
In the invention, the flaky caustic soda and the acetic acid wastewater are selected for neutralization reaction, and the concentration of sodium acetate in the reaction solution can be improved because of little moisture brought by the caustic soda, thereby greatly reducing the steam consumption of evaporation concentration in the subsequent process.
In step S2, the temperature of the neutralization reaction was 60 ℃. The reaction of acetic acid and caustic soda is acid-base neutralization reaction, and a large amount of heat is released, so that the temperature of reaction liquid is increased, the reaction is more violent when the temperature is high, and simultaneously, volatile materials in acetic acid wastewater begin to volatilize due to the temperature increase, and certain irritant gas is generated. The reaction temperature is controlled below 60 ℃, so that the generation of irritant gas can be effectively avoided, and a small amount of irritant gas generated is pumped to the waste gas absorption tower by using the vacuum pump to be absorbed.
The miscellaneous fat in the acetic acid wastewater also has the following side reaction in the presence of caustic soda: RCOOR '+ NaOH → RCOONa + R' OH, preferably, in the neutralization reaction in the step S2, caustic soda is slowly dripped into acetic acid wastewater, so that the caustic soda with relatively high cost can be fully reacted, and the caustic soda generated by side reaction due to excessive caustic soda can be avoided; after the dropwise addition is finished, the mass of acetic acid in the acetic acid wastewater is kept 4% -8% more than that of caustic soda, preferably, the mass of acetic acid in the acetic acid wastewater is 5% excessive, and the occurrence of side reactions is reduced.
The concentration of the concentrated mother liquor is low, although the crystallized crystal particles are large and the product purity is high, the crystallization speed is low, the yield is low and the production efficiency is low; and the concentration of the concentrated mother liquor is too high, and impurities can be separated out along with crystallization when the crystallized sodium acetate is separated out, so that the product quality is influenced. Preferably, in the step S4, the density of the concentrated mother liquor is 1250 kg/m.
In the step S4, the steam used for evaporation and concentration is generated by heating the neutralization reaction cooling water, the self-steam liquefied water, and the crystallization cooling water, so that comprehensive utilization of heat can be achieved.
The invention also discloses a preparation device for preparing the sodium acetate, which comprises a cloth bag filter, a neutralization reaction kettle, a filter, a concentration reaction kettle, a crystallization tank and a separator which are sequentially communicated, wherein the communication pipelines among the components are respectively provided with a delivery pump, namely acetic acid wastewater is filtered by the cloth bag filter and then enters the neutralization reaction kettle, caustic soda is dripped into the neutralization reaction kettle for neutralization reaction, reaction liquid after reaction enters the concentration reaction kettle after impurities are filtered by the filter, concentrated mother liquor after concentration enters the crystallization tank for crystallization, mixed liquor after crystallization enters the separator, the separator separates crystals from the mother liquor, a liquid discharge port of the pump is communicated with a feed port of the crystallization tank through a return pipe, and the separated mother liquor can be crystallized again.
Preferably, the neutralization reaction kettle comprises a shell, wherein a coiled pipe and an anchor stirring rod which are fixed on the inner wall of the shell are arranged inside the shell, the coiled pipe is used for introducing cooling water and cooling the neutralization reaction, and a water inlet and a water outlet of the coiled pipe extend to the outside of the shell. The stirring rod is used for stirring, the inclined plate is arranged above the anchor part of the stirring rod and used for promoting the upwelling of the reaction liquid and facilitating the uniform reaction of the reaction liquid.
The upper part of the shell is provided with an acetic acid wastewater feeding hole, a caustic soda feeding hole and a waste gas extraction hole, and the bottom of the shell is provided with a discharge hole; the shell is provided with a temperature measuring instrument for measuring the temperature in the reaction kettle.
Further, the structures of the concentration reaction kettle and the crystallization tank are the same as those of the neutralization reaction kettle. The coil pipes are also arranged in the concentration reaction kettle and the crystallization tank, and the coil pipes in the concentration reaction kettle are used for introducing high-temperature steam and heating the concentrated reaction solution; the coil pipe in the crystallizing tank is used for introducing crystallization cooling gas for concentrating the crystallization of the mother liquor.
A steam generator is arranged between the coiled pipes in the neutralization reaction kettle and the concentration reaction kettle and is used for heating cooling water from the coiled pipes in the neutralization reaction kettle to form steam; set up cooling tank and cooling structure between concentrated reation kettle and the crystallizer, the cooling tank is used for the liquefied water that natural cooling goes out from concentrated reation kettle coiled pipe, reduces the temperature of liquefied water, and the liquefied water in the cooling tank is followed in the cooling structure cooling, makes it form crystallization cooling gas, and the crystallization cooling gas in the cooling structure can be used to the cooling of crystallization cooling and neutralization reaction. Wherein the liquefied water from the coiled pipe of the concentration reaction kettle and the cooling water from the crystallization tank can enter a steam generator through a pipeline for evaporation concentration.
The cooling water from the coiled pipe of the neutralization reaction kettle and the crystallization tank is preheated due to heat absorption, the liquefied water from the coiled pipe of the concentration reaction kettle has the temperature, and the three parts are used as the liquid to be heated of the steam generator, so that the heating burden of the steam generator is reduced. The device comprehensively utilizes the heat release and heat absorption processes in each procedure to preheat and pre-cool water, thereby being beneficial to the comprehensive utilization of energy and saving the energy.
The cooling method of the cooling structure comprises the following steps:
a1: respectively freezing the liquefied water from the coiled pipe of the concentration reaction kettle by using a refrigerating piece;
a2: crushing ice blocks formed by freezing to form ice slush;
a3: and mixing the air of the ice sand box to form mixed air with ice sand.
Specifically, the cooling structure includes a cooling chamber, a freezing chamber, and a mixing chamber. The cooling chamber is used for cooling the liquefied water from the coiled pipe of the concentration reaction kettle to 5-10 ℃, the water in the cooling chamber is introduced into the freezing chamber and is frozen and crushed to form the ice sand, and the ice sand enters the air in the mixing chamber box to form mixed air with the ice sand, namely crystallized cooling gas.
It is specific, the freezer is inside to be set up inlet tube, the husky discharging pipe of ice, freezes box, crushing box, and the freezer outside sets up freezing subassembly, makes the temperature of freezer below 0 ℃, the upper portion of freezer sets up the box that freezes that can overturn, the top of freezing the box sets up the inlet tube, the below of freezing the box sets up crushing box, smashes the inside crushing blade that sets up of box, the bottom of smashing the box sets up the husky discharging pipe of online slope.
The water that the inlet tube came in gets into freezing the box and freezes, and the ice-cube after freezing falls into crushing box through freezing 180 upsets of box, smashes the ice-cube of box inside crushing blade, forms the ice-slush, and the ice-slush can go out from the ice-slush discharging pipe and get into the mixing chamber.
The freezing box comprises a box body and a pressing plate below the box body, wherein a spring is arranged between the pressing plate and the box body; the box body is internally provided with a partition plate which divides the box body into a plurality of freezing units, the upper end of the partition plate is lower than the upper end of the box body, the freezing units are communicated with one another, ice water can conveniently enter each freezing unit, each freezing unit is provided with a flexible silica gel film at the bottom, the pressing plate is provided with a convex block corresponding to the silica gel film at one side close to the box body, the pressing plate is pressed in the direction close to the box body, and the convex block can abut against the silica gel film to push the ice blocks of the box body, so.
Further, box body and freezer swivelling joint, the top of freezer sets up the push pedal and is used for down promoting the cylinder of push pedal, and after the box body carried out 180 upsets, the clamp plate was corresponding with the push pedal, and the cylinder promoted the push pedal and presses the clamp plate, makes the lug push away the ice-cube to crushing box in, smashes the blade and smashes the ice-cube, forms the ice-slush.
Furthermore, the inside fan, dispersion box, guide tube, cooling thing discharging pipe that sets up of mixing chamber, the mixing chamber is located freezing room one side, and the inside temperature of mixing chamber is crossed the refrigeration subassembly and is kept below 0 ℃ all, is used for cooling air and keeps the sand ice not to melt. The air outlet fixed connection of fan disperses the upper end of box and communicates with the inside of dispersion box, the air outlet of fan is connected to the one end of guiding tube, and the other end of guiding tube is connected the lower extreme of fixed connection dispersion box and communicates with the inside of dispersion box, the dispersion box passes through the ice sand discharging pipe and smashes the box intercommunication, dispersion box one end sets up the cooling thing discharging pipe. The fan blows air into the dispersing box, the pump body is arranged above the ice sand discharging pipe and guides the ice sand in the crushing box into the dispersing box, the air and the ice sand in the dispersing box are mixed to form mixed air with the ice sand, and the guide pipe enables the upper end and the lower end of the dispersing box to enter the air so as to accelerate the dispersion of the ice sand in the air. The cooling medium outlet pipe guides the mixed air with the ice slush into the coil of the crystallization tank.
Preferably, the inner wall of the dispersing box is provided with a spiral convex plate to accelerate the mixing of the sand ice and the air in the dispersing box.
1. The invention has the beneficial effects that: the sodium acetate is prepared by using the acetic acid wastewater, the raw material is low in cost of raw materials, the process flow is simple, so that the product cost is low, the discharge of the acetic acid wastewater is reduced, and the sodium acetate has good economic value and social value.
2. The heat release and heat absorption processes in all the procedures are comprehensively utilized in the sodium acetate preparation system, water is preheated and precooled, comprehensive utilization of energy is facilitated, and energy is saved.
3. The cooling structure in the sodium acetate preparation system can cool the neutralization reaction and the crystallization process through the ice-water mixture, ice sand generated in the cooling process absorbs heat to form water, the cooling effect is strong, the cooling efficiency can be accelerated when needed, and the cooling structure has great superiority in the aspect of accurately controlling the reaction temperature.
4. The freezing chamber of the cooling structure in the sodium acetate preparation system can realize freezing and automatic crushing of ice blocks and automatic mixing of air and sand ice, the cooling structure can realize continuous cooling, and the cooling efficiency is high.
Drawings
FIG. 1 is a process diagram of the method for preparing sodium acetate from acetic acid wastewater;
FIG. 2 is a flow chart of the method for preparing sodium acetate by using acetic acid wastewater;
FIG. 3 is a schematic structural diagram of the apparatus for preparing sodium acetate from acetic acid wastewater;
FIG. 4 is a schematic structural diagram of a neutralization reaction kettle of the sodium acetate preparation device;
FIG. 5 is a flow chart of the cooling method of the cooling structure of the apparatus for preparing sodium acetate;
FIG. 6 is a schematic structural diagram of the cooling structure of the apparatus for preparing sodium acetate;
FIG. 7 is a schematic diagram of the structure of the freezing chamber of the apparatus for preparing sodium acetate;
FIG. 8 is a schematic view of the structure of the dispersing box part of the apparatus for preparing sodium acetate.
In the figure: 1. a neutralization reaction kettle; 2. a filter; 3. concentrating the reaction kettle; 4. a crystallization tank; 5. a separator; 6. a cooling pool; 7. a steam generator; 8. a cooling structure; 11. a housing; 12. a stirring rod; 13. a serpentine tube; 14. a temperature measuring instrument; 121. a sloping plate; 131. a water inlet; 132. a water outlet; 111. an acetic acid wastewater inlet; 112. a caustic soda feed port; 113. a discharge port; 114. an exhaust gas extraction port; 81. a freezing chamber; 82. a water inlet pipe; 83. a smoothie discharging pipe; 84. a freezing box; 85. a crushing box; 86. a crushing blade; 87. pushing the plate; 88. a cylinder; 89. a mixing chamber; 810. a fan; 811. a dispersion box; 812. a guide tube; 813. a cooling material discharge pipe; 814. a spiral convex plate; 841. a box body; 842. a partition plate; 843. silica gel; 844. a freezing unit; 845. pressing a plate; 846. a spring; 847. and (4) a bump.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
Referring to fig. 3, an energy-saving preparation system for preparing sodium acetate comprises a cloth bag filter, a neutralization reaction kettle 1, a filter 2, a concentration reaction kettle 3, a crystallizing tank 4 and a separator 5 which are sequentially communicated, wherein a communicating pipeline between the components is provided with a delivery pump, namely acetic acid wastewater is filtered by the cloth bag filter and then enters the neutralization reaction kettle 1, caustic soda is dripped into the neutralization reaction kettle 1 for neutralization reaction, a reaction solution after reaction enters the concentration reaction kettle 3 after impurities are filtered by the filter 2, a concentrated mother solution after concentration enters the crystallizing tank 4 for crystallization, a mixed solution after crystallization is introduced into the separator 5, the separator 5 separates crystals from the mother solution, a liquid discharge port of the separator 5 is communicated with a feed port of the crystallizing tank 4 through a return pipe, and the separated mother solution can be crystallized again.
Further, referring to fig. 4, the neutralization reactor 1 includes a housing 11, a coil 13 and an anchor stirring rod 12 fixed to an inner wall of the housing 11 are disposed inside the housing 11, the coil 13 is used for introducing cooling water for cooling the neutralization reaction, and a water inlet 131 and a water outlet 132 of the coil 13 extend to the outside of the housing 11. The stirring rod 12 is used for stirring, and the inclined plate 121 is arranged above the anchor part of the stirring rod 12 and used for promoting the upwelling of the reaction liquid and facilitating the uniform reaction of the reaction liquid.
The upper part of the shell 11 is provided with an acetic acid wastewater inlet 111, a caustic soda inlet 112 and a waste gas extraction port 114, and the bottom of the shell 11 is provided with a discharge port 113; the shell 11 is provided with a temperature measuring instrument 14 for measuring the temperature in the reaction kettle, and the shell 11 is provided with a pH value measurer for measuring the temperature of the reaction liquid in the reaction kettle.
Further, the structures of the concentration reaction kettle 3 and the crystallization tank 4 are the same as the structure of the neutralization reaction kettle 1. The inner parts of the concentration reaction kettle 3 and the crystallization tank 4 are also provided with coiled pipes, and the coiled pipes in the concentration reaction kettle 3 are used for introducing high-temperature steam and heating concentrated reaction liquid; the coil pipe in the crystallizing tank 4 is used for introducing crystallization cooling water for concentrating the crystallization of the mother liquor.
A steam generator 7 is arranged between the coiled pipes in the neutralization reaction kettle 1 and the concentration reaction kettle 3, and the steam generator 7 is used for heating the cooling water from the coiled pipes in the neutralization reaction kettle 1 to form steam; set up cooling tank 6 and cooling structure 8 between concentrated reation kettle 3 and crystallizer 4, cooling tank 6 is used for the natural cooling to reduce the temperature of liquefied water from the liquefied water that concentrated reation kettle 3 coiled pipe came out, and cooling structure 8 cools off the liquefied water from cooling tank 6, makes it form crystallization cooling water, and the cooling crystal water in the cooling structure 8 can be used to the cooling of crystallization cooling and neutralization reaction. Wherein the liquefied water from the coil of the concentration reaction kettle 3 and the cooling water from the crystallization tank 4 can enter the steam generator 7 through a pipeline for evaporation concentration.
The cooling water from the coiled pipes of the neutralization reaction kettle 1 and the crystallization tank 4 is preheated due to heat absorption, the liquefied water from the coiled pipes of the concentration reaction kettle 3 has the temperature, and the three are used as the liquid to be heated of the steam generator 7, so that the heating burden of the steam generator 7 is reduced. The system comprehensively utilizes the heat release and heat absorption processes in each procedure to preheat and pre-cool water, thereby being beneficial to the comprehensive utilization of energy and saving the energy.
Referring to fig. 5, the cooling method of the cooling structure 8 includes the steps of:
a1: respectively freezing the liquefied water from the coiled pipe of the concentration reaction kettle by using a refrigerating piece;
a2: crushing ice blocks formed by freezing to form ice slush;
a3: and mixing the air of the ice sand box to form mixed air with ice sand.
Specifically, referring to fig. 6, the cooling structure 8 includes a cooling chamber (not shown), a freezing chamber 81 and a mixing chamber 89, and the materials inside the cooling chamber, the freezing chamber 81 and the mixing chamber 89 can be transported by a pump body. The cooling chamber is used for cooling the liquefied water from the coiled pipe of the concentration reaction kettle 3 to 5-10 ℃, part of the water in the cooling chamber is introduced into the freezing chamber 81 and is frozen and crushed to form the ice sand, and the ice sand and the water in the cooling chamber enter the mixing chamber 89 to form the crystallized cooling gas.
Specifically, referring to fig. 6, a water inlet pipe 82, a frozen sand discharging pipe 83, a frozen box 84 and a crushing box 85 are arranged inside the freezing chamber 81, a freezing component is arranged outside the freezing chamber 81, the freezing component can use a refrigerating component of a refrigerator refrigerating system, so that the temperature of the freezing chamber 81 is kept below 0 ℃, the reversible frozen box 84 is arranged on the upper portion of the freezing chamber 81, the water inlet pipe 82 is arranged above the frozen box 84, the crushing box 85 is arranged below the frozen box 84, a crushing blade 86 is arranged inside the crushing box 85, a rotating motor for driving the crushing blade 86 to rotate is arranged at the bottom of the freezing chamber 81, and the ice sand discharging pipe 83 inclined on the net is arranged at the bottom of the crushing box 85.
The water that the inlet tube 82 came in gets into the box 84 that freezes, and the ice-cube after freezing falls into crushing box 85 through the 180 upset of freezing box 84, smashes the blade 86 inside crushing box 85 and smashes the ice-cube, forms the ice-slush, and the ice-slush can go out from ice-slush discharging pipe 83 and get into mixing chamber 89.
Referring to fig. 7, the freezing box 84 includes a box body 841 and a pressing plate 845 under the box body 841, the pressing plate 845 being provided with a spring 846 near the box body 841; the box body 841 is internally provided with a partition plate 842 to divide the box body 841 into a plurality of freezing units 844, the upper end of the partition plate 842 is lower than the upper end of the box body 841, the freezing units 844 are communicated with each other, ice water conveniently enters each freezing unit 844, the bottom of each freezing unit 844 is provided with a flexible silica gel film 843, one side of the pressing plate 845, which is close to the box body 841, is provided with a bump 847 corresponding to the silica gel film 843, the pressing plate 845 is pressed in the direction close to the box body 841, and the bump 847 can prop against the silica gel film 843 to push ice cubes of the box body 841, so.
Further, box 841 and freezer 81 are through round pin axle swivelling joint, and the one end of round pin axle sets up the upset motor of drive freezer 81 upset, the top of freezer 81 sets up push pedal 87 and is used for down promoting push pedal 87's cylinder 88, and after box 841 carried out 180 upsets, clamp plate 845 was corresponding with push pedal 87, and cylinder 88 promoted push pedal 87 and pressed clamp plate 845, made during lug 847 pushed the ice-cube to smash box 85, smashes blade 86 smashed the ice-cube, formed the ice-cube.
The ice-sand enters into the mixing chamber 89 through the ice-sand discharging pipe 83, referring to fig. 8, a fan 810, a dispersing box 811, a guiding pipe 812 and a cooling material discharging pipe 813 are arranged inside the mixing chamber 89, the mixing chamber 89 is positioned at one side of the freezing chamber 81, and the temperature inside the mixing chamber 89 is kept below 0 ℃ through a refrigerating assembly for cooling air and keeping the ice-sand from melting. An air outlet of the fan 810 is fixedly connected with the upper end of the dispersing box 811 and is communicated with the inside of the dispersing box 811, one end of the guide pipe 812 is connected with the air outlet of the fan 810, the other end of the guide pipe 812 is fixedly connected with the lower end of the dispersing box 811 and is communicated with the inside of the dispersing box 811, the dispersing box 811 is communicated with the crushing box 85 through the smoothie discharging pipe 83, and one end of the dispersing box 811 is provided with a cooling material discharging pipe 813. The blower 810 blows air into the dispersing box 811, and a pump body is provided above the slush discharge pipe 83 to guide the slush in the pulverization box 85 into the dispersing box 811, and the air in the dispersing box 811 is mixed with the slush to form mixed air with the slush, wherein the guide pipe 812 allows both the upper end and the lower end of the dispersing box 811 to enter the air to accelerate the dispersion of the slush in the air. The inner wall of the dispersing box 811 is provided with a spiral convex plate 814 to accelerate the mixing of the sand ice and the air in the dispersing box 811. The coolant outlet pipe 813 introduces the mixed air with the slush into the coil of the crystallization tank 4.
The ice and the air are mixed to form mixed gas, ice generated in the cooling process of the mixed gas body fluid of the ice and the ice absorbs heat to be changed into water, the cooling effect is strong, the cooling efficiency can be accelerated when needed, and the ice and the water cooling device have great superiority particularly in accurately controlling the reaction temperature. And the cooling structure can continuously and automatically work under the control of a controller, and the controller controls a transportation pump body, a crushing motor, a turnover motor and a cylinder in the cooling structure, so that automatic cooling is realized.
The structures of the concentration reaction kettle 3 and the crystallizing tank 4 in the sodium acetate preparation system are the same as the structures of the neutralization reaction kettle 1, one neutralization reaction kettle 1 can be selected to work intermittently under the conditions of limited places and limited cost, and the neutralization reaction, concentration and crystallization processes can be completed by one kettle body through pumping in and pumping in reaction liquid for many times.
Example 2
Referring to fig. 1 and 2, a method for preparing sodium acetate is characterized by comprising the following steps:
s1: filtering acetic acid wastewater to remove impurities in the acetic acid wastewater, wherein a cloth bag filter is selected as the filter;
s2: and (3) carrying out neutralization reaction on the filtered acetic acid wastewater and caustic soda, measuring the content of acetic acid in the acetic acid wastewater, determining the quality of the caustic soda, and controlling the temperature of the neutralization reaction at 60 ℃. The specific process is that caustic soda is slowly dripped into acetic acid wastewater, so that the caustic soda with relatively high cost can be fully reacted, and the caustic soda which causes side reaction due to excessive caustic soda can be avoided; after the dropwise addition is finished, the mass of the acetic acid in the acetic acid wastewater is kept to be 5% more than that of the caustic soda.
S3: when the pH value of the reaction liquid of the neutralization reaction is 7.5, filtering the product after the neutralization reaction, and removing filter residues to obtain filtrate;
s4: evaporating and concentrating the filtrate to obtain concentrated mother liquor with density of 1250kg/m3
S5: crystallizing the concentrated mother liquor, wherein the crystallization temperature is kept at 45 ℃;
s6: separating the crystals and the mother liquor by a centrifuge, collecting and packaging the crystals, and recrystallizing the mother liquor again.
The sodium acetate crystal is obtained by the preparation of the sodium acetate preparation system. CH in the obtained sodium acetate crystal3COONa content of 58.8%, free alkali content of 0.022%, and water-insoluble content of 0.0%21% of the total amount of sodium acetate, which meets the industrial sodium acetate standard of sodium acetate trihydrate implementation Standard (Q/NH 18-1999).
Example 3
Referring to fig. 1 and 2, a method for preparing sodium acetate is characterized by comprising the following steps:
s1: filtering acetic acid wastewater to remove impurities in the acetic acid wastewater, wherein a cloth bag filter is selected as the filter;
s2: and (3) carrying out neutralization reaction on the filtered acetic acid wastewater and caustic soda, measuring the content of acetic acid in the acetic acid wastewater, determining the quality of the caustic soda, and controlling the temperature of the neutralization reaction at 52 ℃. The specific process is that caustic soda is slowly dripped into acetic acid wastewater, so that the caustic soda with relatively high cost can be fully reacted, and the caustic soda which causes side reaction due to excessive caustic soda can be avoided; after the dropwise addition is finished, the mass of the acetic acid in the acetic acid wastewater is kept 6% more than that of the caustic soda.
S3: when the pH value of the reaction liquid of the neutralization reaction is 7.5, filtering the product after the neutralization reaction, and removing filter residues to obtain filtrate;
s4: evaporating and concentrating the filtrate to obtain concentrated mother liquor with density of 1250kg/m3
S5: crystallizing the concentrated mother liquor, wherein the crystallization temperature is kept at 45 ℃;
s6: separating the crystals and the mother liquor by a centrifuge, collecting and packaging the crystals, and recrystallizing the mother liquor again.
The sodium acetate crystal is obtained by the preparation of the sodium acetate preparation system. CH in the obtained sodium acetate crystal3The content of COONa is 60.9%, the content of free alkali is 0.024%, the content of water-insoluble substances is 0.023%, and the industrial sodium acetate standard of sodium acetate trihydrate execution standard (Q/NH18-1999) is met.
Example 4
Referring to fig. 1 and 2, a method for preparing sodium acetate is characterized by comprising the following steps:
s1: filtering acetic acid wastewater to remove impurities in the acetic acid wastewater, wherein a cloth bag filter is selected as the filter;
s2: and (3) carrying out neutralization reaction on the filtered acetic acid wastewater and caustic soda, measuring the content of acetic acid in the acetic acid wastewater, determining the quality of the caustic soda, and controlling the temperature of the neutralization reaction at 61 ℃. The specific process is that caustic soda is slowly dripped into acetic acid wastewater, so that the caustic soda with relatively high cost can be fully reacted, and the caustic soda which causes side reaction due to excessive caustic soda can be avoided; after the dropwise addition is finished, the mass of the acetic acid in the acetic acid wastewater is kept to be 5.1% more than that of the caustic soda.
S3: when the pH value of the reaction liquid of the neutralization reaction is 7.9, filtering the product after the neutralization reaction, and removing filter residues to obtain filtrate;
s4: evaporating and concentrating the filtrate to obtain concentrated mother liquor with density of 1250kg/m3
S5: crystallizing the concentrated mother liquor, wherein the crystallization temperature is kept at 48 ℃;
s6: separating the crystals and the mother liquor by a centrifuge, collecting and packaging the crystals, and recrystallizing the mother liquor again.
The sodium acetate crystal is obtained by the preparation of the sodium acetate preparation system. CH in the obtained sodium acetate crystal3The content of COONa is 62.1 percent, the content of free alkali is 0.021 percent, the content of water-insoluble substances is 0.020 percent, and the sodium acetate meets the industrial sodium acetate standard of sodium acetate trihydrate execution standard (Q/NH 18-1999).
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (5)

1. A method for preparing sodium acetate by using acetic acid wastewater is characterized in that the method is realized by a device for preparing sodium acetate by using acetic acid wastewater;
the method comprises the following steps:
s1: filtering the acetic acid wastewater to remove impurities in the acetic acid wastewater;
s2: neutralizing the filtered acetic acid wastewater with caustic soda, controlling the temperature of the neutralization reaction to be 55-65 ℃, dropwise adding the caustic soda into the acetic acid wastewater, and keeping the mass of acetic acid in the acetic acid wastewater to be 4-8% more than that of the caustic soda after the dropwise adding of the caustic soda is finished;
s3: filtering the product after the neutralization reaction, and removing filter residues to obtain filtrate;
s4: evaporating and concentrating the filtrate to obtain concentrated mother liquor with concentration of 1250kg/m3
S5: crystallizing the concentrated mother liquor;
s6: separating the crystals from the mother liquor by a centrifugal machine, collecting and packaging the crystals, and recrystallizing the mother liquor again;
in the step S4, steam is used for evaporation and concentration and is generated by heating the neutralization reaction cooling water, the self steam liquefied water and the crystallization cooling water;
the device for preparing sodium acetate by using acetic acid wastewater comprises a neutralization reaction kettle (1), a filter (2), a concentration reaction kettle (3), a crystallization tank (4) and a separator (5) which are sequentially communicated, wherein conveying pumps are arranged on communication pipelines among the components, and a liquid discharge hole of the separator (5) is communicated with a feed inlet of the crystallization tank (4) through a return pipe;
the neutralization reaction kettle (1) comprises a shell (11), wherein a coiled pipe (13) and an anchor type stirring rod (12) which are fixed on the inner wall of the shell (11) are arranged inside the shell (11), an inclined plate (121) is arranged above an anchor part of the stirring rod (12), a water inlet (131) and a water outlet (132) of the coiled pipe (13) extend to the outside of the shell (11), an acetic acid wastewater feeding hole (111), a caustic soda feeding hole (112) and a waste gas extraction hole (114) are arranged at the upper part of the shell (11), and a discharging hole (113) is arranged at the bottom of the shell (11); a temperature measuring instrument (14) is arranged on the shell (11).
The structures of the concentration reaction kettle (3) and the crystallization tank (4) are the same as the structure of the neutralization reaction kettle (1);
a steam generator (7) is arranged between the coiled pipes in the neutralization reaction kettle (1) and the concentration reaction kettle (3), and a cooling pool (6) and a cooling structure (8) are arranged between the concentration reaction kettle (3) and the crystallizing tank (4);
the cooling structure (8) comprises a freezing chamber (81), a water inlet pipe (82), a frozen sand discharging pipe (83), a freezing box (84) and a crushing box (85) are arranged in the freezing chamber (81), the freezing box (84) which can be turned over is arranged at the upper part of the freezing chamber (81), the water inlet pipe (82) is arranged above the freezing box (84), the crushing box (85) is arranged below the freezing box (84), and the frozen sand discharging pipe (83) which is inclined on the net is arranged at the bottom of the crushing box (85);
cooling structure (8) still includes mixing chamber (89), mixing chamber (89) inside sets up fan (810), dispersion box (811), guide tube (812), coolant discharging pipe (813), the upper end of the air outlet fixed connection dispersion box (811) of fan (810) and with the inside intercommunication of dispersion box (811), the air outlet of fan (810) is connected to the one end of guide tube (812), the other end of guide tube (812) is connected the lower extreme of fixed connection dispersion box (811) and is communicated with the inside of dispersion box (811), dispersion box (811) are through ice sand discharging pipe (83) and are smashed box (85) and communicate, dispersion box (811) one end sets up coolant discharging pipe (813).
2. The method for preparing sodium acetate by using acetic acid wastewater as claimed in claim 1, wherein the freezing box (84) comprises a box body (841) and a pressure plate (845) below the box body (841), and a spring (846) is arranged between the pressure plate (845) and the box body (841);
box body (841) inside setting up baffle (842) and dividing into a plurality of freezing units (844) with box body (841), communicate each other between freezing unit (844), every the bottom of freezing unit (844) sets up pellosil (843), clamp plate (845) are close to box body (841) one side and set up lug (847) that correspond with pellosil (843).
3. The method for preparing sodium acetate from acetic acid wastewater as claimed in claim 2, wherein the case (841) is rotatably connected to a freezing chamber (81), a push plate (87) and a cylinder (88) for pushing the push plate (87) downward are provided above the freezing chamber (81), and the push plate (845) corresponds to the push plate (87) after the case (841) is turned over by 180 °.
4. The method for preparing sodium acetate using acetic acid wastewater as claimed in claim 3, wherein the inner wall of the dispersion box (811) is provided with a spiral convex plate (814).
5. The method for preparing sodium acetate by using acetic acid wastewater as claimed in claim 4, wherein the cooling method of the cooling structure (8) comprises the following steps:
a1: respectively freezing the liquefied water from the coiled pipe of the concentration reaction kettle by using a refrigerating piece;
a2: crushing ice blocks formed by freezing to form ice slush;
a3: and mixing the air of the ice sand box to form mixed air with ice sand.
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CN202730041U (en) * 2012-07-02 2013-02-13 徐州汉高酒业有限公司 Novel device for producing sodium acetate from grain stillage
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