CN111423322A - Sodium acetate preparation method and energy-saving preparation system thereof - Google Patents
Sodium acetate preparation method and energy-saving preparation system thereof Download PDFInfo
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- CN111423322A CN111423322A CN202010398411.6A CN202010398411A CN111423322A CN 111423322 A CN111423322 A CN 111423322A CN 202010398411 A CN202010398411 A CN 202010398411A CN 111423322 A CN111423322 A CN 111423322A
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Abstract
The invention discloses a sodium acetate preparation method and an energy-saving preparation system thereof, wherein the sodium acetate preparation method 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 system 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
Technical Field
The invention relates to the technical field of sodium acetate production, in particular to a sodium acetate preparation method and an energy-saving preparation system thereof.
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 sodium acetate preparation method and an energy-saving preparation system thereof, which utilize acetic acid wastewater to prepare industrial sodium acetate so as to achieve the purpose of saving 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.
Preferably, in step S2, the temperature of the neutralization reaction is 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 1250kg/m3。
The invention also discloses an energy-saving preparation system 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 water 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; a cooling pool and a cooling device are arranged between the concentration reaction kettle and the crystallizing tank, the cooling pool is used for naturally cooling the liquefied water coming out of the coiled pipe of the concentration reaction kettle, the temperature of the liquefied water is reduced, the cooling device cools the liquefied water in the cooling pool to form crystallization cooling water, and the cooling crystal water in the cooling device can be used for cooling crystallization 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 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.
The cooling method of the cooling device comprises the following steps:
a1: respectively freezing and cooling 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: the ice slush was mixed with the cooling water in a1 to form crystallized cooling water.
Specifically, the cooling device comprises 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 ℃, part of 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 and the water in the cooling chamber enter the mixing chamber to form the crystallization cooling water.
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.
The invention has the beneficial effects that:
1. 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 device in the sodium acetate preparation system can cool the neutralization reaction and the crystallization process through the ice-water mixture, ice 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 device has great superiority particularly in accurately controlling the reaction temperature.
4. The freezing chamber of the cooling device in the sodium acetate preparation system can realize freezing and automatic crushing of ice cakes, the cooling device can realize continuous cooling, and the cooling efficiency is high.
Drawings
FIG. 1 is a flow chart of the preparation method of sodium acetate;
FIG. 2 is a schematic structural diagram of the sodium acetate energy-saving preparation system;
FIG. 3 is a schematic structural diagram of a neutralization reaction kettle of the energy-saving sodium acetate preparation system;
FIG. 4 is a flow chart of the cooling method of the cooling device of the sodium acetate energy-saving preparation system;
FIG. 5 is a schematic structural diagram of a cooling device of the sodium acetate energy-saving preparation system;
FIG. 6 is a schematic structural diagram of a freezing box of the energy-saving sodium acetate preparation system;
fig. 7 is a schematic structural diagram of a freezing chamber of the energy-saving sodium acetate preparation system.
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 device; 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; 841. a box body; 842. a partition plate; 843. a silicone membrane; 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. 2, 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. 3, 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; a cooling pool 6 and a cooling device 8 are arranged between the concentration reaction kettle 3 and the crystallizing tank 4, the cooling pool 6 is used for naturally cooling the liquefied water coming out of the coil pipe of the concentration reaction kettle 3, the temperature of the liquefied water is reduced, the cooling device 8 cools the liquefied water in the cooling pool 6 to form crystal cooling water, and the cooled crystal water in the cooling device 8 can be used for cooling 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. 4, the cooling method of the cooling device 8 includes the steps of:
a1: respectively freezing and cooling 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: the ice slush was mixed with the cooling water in a1 to form crystallized cooling water.
In particular, with reference to fig. 5, the cooling device 8 comprises a cooling chamber, a freezing chamber 81 and a mixing chamber, the material inside the cooling chamber, the freezing chamber 81 and the mixing chamber being transportable by means of 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 to form the crystallization cooling water.
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 the mixing chamber.
Referring to fig. 6, 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.
In the ice sand got into the mixing chamber through ice sand discharging pipe 83, mixed liquid was formed after ice sand and cooling water mixed, and the ice heat absorption that mixed liquid produced in the cooling process changed into water, and the cooling effect is strong, can accelerate cooling efficiency when needing, in particular in the aspect of accurately controlling reaction temperature, has great superiority. And the cooling device can continuously and automatically work under the control of the controller, and the controller controls a transportation pump body, a crushing motor, a turnover motor and a cylinder in the cooling device to realize automatic cooling.
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, 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 crystal3The content of COONa is 58.6%, the content of free alkali is 0.021%, the content of water-insoluble substances is 0.025%, and the sodium acetate meets the industrial sodium acetate standard of sodium acetate trihydrate execution Standard (Q/NH 18-1999).
Example 3
Referring to fig. 1, 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 55 ℃. 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 7.6, 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 43 ℃;
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 60.1%, the content of free alkali is 0.023%, the content of water-insoluble substances is 0.022%, and the sodium acetate meets the industrial sodium acetate standard of sodium acetate trihydrate execution standard (Q/NH 18-1999).
Example 4
Referring to fig. 1, 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 62 ℃. 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 5.5% more than that of the caustic soda.
S3: when the pH value of the reaction liquid of the neutralization reaction is 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 with density of 1250kg/m3；
S5: crystallizing the concentrated mother liquor at 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.
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 61.2%, the content of free alkali is 0.023%, the content of water-insoluble substances is 0.024%, and the industrial sodium acetate standard of sodium acetate trihydrate execution standard (Q/NH18-1999) is met.
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 (10)
1. 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: 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;
s5: crystallizing the concentrated mother liquor;
s6: separating the crystals and the mother liquor by a centrifuge, collecting and packaging the crystals, and recrystallizing the mother liquor again.
2. The method for preparing sodium acetate according to claim 1, characterized in that in the neutralization reaction of step S2, caustic soda is added dropwise into the acetic acid wastewater, and after the addition of caustic soda is completed, the mass of acetic acid in the acetic acid wastewater is kept 4% -8% more than that of caustic soda.
3. The sodium acetate preparation method and energy-saving preparation system thereof according to claim 2, wherein in the step S4, the density of the concentrated mother liquor is 1250kg/m3。
4. The energy-saving preparation system for preparing the sodium acetate according to claim 1 or 3, which 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 the communication pipelines among the components are provided with delivery pumps, and the liquid discharge port of the separator (5) is communicated with the feed port of the crystallization tank (4) through a return pipe.
5. The energy-saving sodium acetate preparation system according to claim 4, wherein the neutralization reaction kettle (1) comprises a shell (11), 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 the 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 inlet (111), a caustic soda inlet (112) and an exhaust gas extraction port (114) are arranged on the upper part of the shell (11), and a discharge port (113) is arranged at the bottom of the shell (11); a temperature measuring instrument (14) is arranged on the shell (11).
6. The energy-saving sodium acetate preparation system according to claim 5, wherein 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 device (8) are arranged between the concentration reaction kettle (3) and the crystallizing tank (4).
7. The energy-saving sodium acetate preparation system according to claim 6, wherein the cooling device (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), the upper part of the freezing chamber (81) is provided with the reversible freezing box (84), 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 bottom of the crushing box (85) is provided with the frozen sand discharging pipe (83) inclined on the net.
8. The energy-saving sodium acetate preparation system of claim 7, 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).
9. The energy-saving sodium acetate preparation system according to claim 8, wherein the box (841) is rotatably connected with the freezing chamber (81), a push plate (87) and a cylinder (88) for pushing the push plate (87) downwards are arranged above the freezing chamber (81), and when the box (841) is turned over by 180 degrees, the press plate (845) corresponds to the push plate (87).
10. The energy-saving sodium acetate preparation system according to claim 9, wherein the cooling method of the cooling device (8) comprises the following steps:
a1: respectively freezing and cooling 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: the ice slush was mixed with the cooling water in a1 to form crystallized cooling water.
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