CN105837431B - A kind of method that sodium acetate is detached in sodium acetate and sodium sulphate mixed system - Google Patents
A kind of method that sodium acetate is detached in sodium acetate and sodium sulphate mixed system Download PDFInfo
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- CN105837431B CN105837431B CN201610203630.8A CN201610203630A CN105837431B CN 105837431 B CN105837431 B CN 105837431B CN 201610203630 A CN201610203630 A CN 201610203630A CN 105837431 B CN105837431 B CN 105837431B
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- sodium acetate
- sodium
- acetate
- calcium
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
Abstract
The present invention provides a kind of methods that sodium acetate is detached in sodium acetate and sodium sulphate mixed system, belong to sodium acetate separation and recovery field.The separation method is to form calcium sulfate precipitation by the way that calcium acetate is added in mixed solution, and sodium sulphate is precipitated after appropriate water removal, realizes that the desulfurization of mixed solution, crystallization obtain sodium acetate.Prepare through mixed liquor, prepared by calcium acetate, precipitate desulfurization and sodium acetate crystallisation step.The method that sodium acetate is detached in sodium acetate and sodium sulphate mixed system provided by the invention, precipitating reagent component is simple, and manufacturing cost is low, a sulfate ion part in the mixed solution Precipitation in the form of calcium sulfate, a part is crystallized with sulfuric acid na form after appropriate water removal and is precipitated, and desulfurization effect is good, and sodium acetate can pass through crystallization recycling, cycle is in industrial production, this method technical process is simple, and operability is good, at low cost, it consumes energy small, is suitable for the industrial production and liquid waste processing of related field.
Description
Technical field
The present invention relates to sodium acetates to separate and recover field, particularly relates to the vinegar in a kind of sodium sulphate and sodium acetate mixed system
The method of sour sodium separation.
Background technology
Sodium acetate molecular formula is CH3COONa or NaAc, also referred to as anhydrous sodium acetate, can be used as in the industrial production lead,
The stabilizer of the metallic elements such as zinc, aluminium, iron, cobalt, nickel, the esterifying agent of organic synthesis, it is also possible to make buffer, pH adjusting agent,
Chemical Manufacture and some Applications in Food Industry are extensive, therefore often will produce the largely industrial wastes containing sodium acetate.One
In a little processing procedures, sulfate ion is existed simultaneously in waste liquid, this kind of waste liquid containing sodium acetate can pass through desulfurization process, crystallization
Realize the recycling of sodium acetate.Realize that the solidification removing of sulfate radical is a kind of commonplace does currently with precipitating ion
Method, the precipitating reagent probed into out have barium chloride, nitric hydrate aluminium and calcium hydroxide and some compounding ingredients precipitating reagents, not
Desulfurization process suitable for the industrial wastes containing a large amount of sodium acetates.It is simple in order to explore a kind of ingredient, at low cost, desulfurization effect
Well, suitable for the desulfurization precipitating reagent of sodium acetate and sodium sulphate mixed system, we have probed into using calcium ion as precipitating ion
The desulfurization of sodium sulphate and sodium acetate mixed solution is realized by removing water in right amount, and is crystallized and obtained the side of the higher sodium acetate of purity
Method has obtained ideal effect.
Invention content
The present invention solves sodium acetate and sodium sulphate mixed solution desulfurization effect is poor, and efficiency is low, precipitating reagent complicated components, at
This high technical problem, therefore a kind of method that sodium acetate is detached in sodium acetate and sodium sulphate mixed solution is provided, using calcium from
Son makes calcium sulfate and sodium sulphate Precipitation realize taking off for sodium acetate and sodium sulphate system as precipitating ion by evaporation water loss
The recycling of sulphur and sodium acetate, method is simple, at low cost, and desulfurization effect is good, and the sodium acetate rate of recovery is high.
To achieve the above object, the technical scheme is that：In a kind of sodium acetate and sodium sulphate mixed system point
Method from sodium acetate, which is characterized in that calcium acetate is added in mixed solution and forms calcium sulfate precipitation, is precipitated after appropriate water removal
Sodium sulphate realizes that the desulfurization of mixed solution, crystallization obtain sodium acetate, specifically comprise the following steps：
(1) mixed solution prepares：The mixed solution of sodium sulphate and sodium acetate is taken, wherein solution sulfur acid na concn is 0.18
~0.34mol/L, sodium acetate concentration are 3.65~4.95mol/L；
(2) prepared by calcium acetate：Calcium oxide and water are mixed, the mixed system of paste liquid or solid-liquid is obtained, stirs
Lower addition acetic acid is mixed, reaction to solution is clarified, spare；
(3) desulfurization is precipitated：Step (2) acquired solution is added in sodium acetate and sodium sulphate mixed system obtained by step (1),
Being carried out at the same time heating stirring makes solution be uniformly mixed, and system becomes cloudy, that is, has calcium sulfate precipitation generation, continuous heating stirring to make to mix
Close solution dehydration, with the evaporation of moisture, precipitation increases, and solid sodium sulfate is precipitated together, heat preservation be filtered to remove sulfur acid calcium and
The precipitation of sodium sulphate, sulfate radical removal rate are 90.0%~95.0%；
(4) sodium acetate crystallizes：Filtrate obtained by step (3) is transferred in clean container, is stored at room temperature, it is cooled to 10~
It is kept for 2~6 hours under this temperature range after 20 DEG C, keeps sodium acetate crystallization complete, after the completion of crystallization, room temperature filtering obtains band
There is the acetic acid sodium crystal containing absorption water and the crystallization water of impurity, the rate of recovery of sodium acetate is 60~95% after water removal, and purity is
85.0~95.0%.
Sodium sulfate concentration is one kind in 0.23mol/L, 0.26mol/L, 0.28mol/L, acetic acid in the step (1)
One kind in a concentration of 4.40mol/L, 4.70mol/L, 4.80mol/L of sodium.
The molar ratio of Calcium Oxide Dosage and sodium sulphate in former mixed solution is (2~3) in the step (2):1, it is added
The amount of water and the mass ratio of calcium oxide are (6~8)：1, the molar ratio that acetic acid amount and calcium oxide is added is (1.7~3.0):1, it stirs
It is 50~300rpm to mix speed.
The appropriate removal process of the instant liquid system of evaporation water loss process in the step (3), dehydration percentage are 28%
~42%, dehydration percentage is that evaporation water loss quality accounts for percentage of the total solution containing water quality, non-to account for the hundred of solution gross mass
Point ratio, the heating temperature of step (3) is all 60~100 DEG C, and mixing speed is all 50~300rpm, heat preservation filtration temperature is 50~
100 DEG C, heat preservation is filtered into heat preservation decompression and filters or keep the temperature press filtration, and heat preservation decompression, which filters, selects Buchner funnel to operate, and keeps the temperature press filtration
Select filter press operation.
Room temperature is filtered into room temperature decompression suction filtration or room temperature press filtration in the step (4), and room temperature decompression, which filters, selects Bu Shi
Funnel operates, and filter press operation is selected in room temperature press filtration.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
(1) present invention makes sulfate ion with sulfuric acid by the way that calcium acetate is added in mixed solution and is removed water in right amount
The form Precipitation of calcium and sodium sulphate, realizes the desulfurization of mixed solution, then it is crystallized obtain sodium acetate, calcium acetate by acetic acid and
Calcium oxide is obtained by the reaction, low production cost, reduces processing cost, and precipitating reagent component is simple, and desulfurization effect is good.
(2) vapor being evaporated in the present invention can carry out condensing recovery by cooling device, and recycling is used for other
In step, recycling for resource is realized, reduce the cost of industrial water.
(3) sodium acetate content is 85.0~95.0% in the impure acetic acid sodium crystal crystallized in the present invention, full
Purity requirement in sufficient industrial production can be directly recycled in production, reduce production cost.
(4) present invention process flow is simple, has operability, can be handled using simple process equipment, at
This is cheap, and can realize recycling for water and sodium acetate, saves energy consumption.
Description of the drawings
Fig. 1 is the schematic diagram of the method for separation sodium acetate in sodium acetate provided by the invention and sodium sulphate mixed system.
Specific implementation mode
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
A kind of method that sodium acetate is detached in sodium acetate and sodium sulphate mixed system, specific embodiment are as follows：
Embodiment 1
(1) take 74mL sodium sulphate and sodium acetate mixed solution spare, wherein sodium sulfate concentration is 0.19mol/L, sodium acetate
A concentration of 3.65mol/L.(2) it weighs 1.60g calcium oxide to mix with 10mL water, is added with stirring 2.80mL acetic acid reactions to solution
Clarification.(3) step (2) acquired solution is added in the solution of step (1), 100 DEG C of heating stirrings, evaporation removes 21g water, that is, loses
Water percentage is 29%.80 DEG C of heat preservations filter, and obtain the filter cake of sulfur acid calcium and sodium sulphate.(4) filtrate obtained suction filtration is fast
Speed is transferred in open-top receptacle, stands kept for 3 hours after being cooled to 10 DEG C at room temperature, room temperature filters, and it is brilliant to obtain transparent sodium acetate
Body.The sodium acetate rate of recovery is 60%, and sulfate radical removal rate is 90.2%.
Embodiment 2
(1) take 82mL sodium sulphate and sodium acetate mixed solution spare, wherein sodium sulfate concentration is 0.26mol/L, sodium acetate
A concentration of 4.70mol/L.(2) it weighs 3.00g calcium oxide to mix with 21mL water, is added with stirring 9.20mL acetic acid reactions to solution
Clarification.(3) step (2) acquired solution is added in the solution of step (1), 60 DEG C of heating stirrings, evaporation removes 34g water, that is, loses
Water percentage is 40%.50 DEG C of heat preservations filter, and obtain the filter cake of sulfur acid calcium and sodium sulphate.(4) filtrate obtained suction filtration is fast
Speed is transferred in open-top receptacle, stands kept for 5 hours after being cooled to 15 DEG C at room temperature, room temperature filters, and it is brilliant to obtain transparent sodium acetate
Body.The sodium acetate rate of recovery is 95%, and sulfate radical removal rate is 93.1%.
Embodiment 3
(1) take 82mL sodium sulphate and sodium acetate mixed solution spare, wherein sodium sulfate concentration is 0.34mol/L, sodium acetate
A concentration of 4.95mol/L.(2) it weighs 3.19g calcium oxide to mix with 20mL water, is added with stirring 7.60mL acetic acid reactions to solution
Clarification.(3) step (2) acquired solution is added in the solution of step (1), 85 DEG C of heating stirrings, evaporation removes 29g water, that is, loses
Water percentage is 34%.95 DEG C of heat preservations filter, and obtain the filter cake of sulfur acid calcium and sodium sulphate.(4) filtrate obtained suction filtration is fast
Speed is transferred in open-top receptacle, stands kept for 2 hours after being cooled to 20 DEG C at room temperature, room temperature filters, and it is brilliant to obtain transparent sodium acetate
Body.The sodium acetate rate of recovery is 73%, and sulfate radical removal rate is 94.7%.
Embodiment 4
(1) take 82mL sodium sulphate and sodium acetate mixed solution spare, wherein sodium sulfate concentration is 0.23mol/L, sodium acetate
A concentration of 4.40mol/L.(2) it weighs 2.85g calcium oxide to mix with 22mL water, is added with stirring 7.90mL acetic acid reactions to solution
Clarification.(3) step (2) acquired solution is added in the solution of step (1), 90 DEG C of heating stirrings, evaporation removes 30g water, that is, loses
Water percentage is 32%.60 DEG C of heat preservations filter, and obtain the filter cake of sulfur acid calcium and sodium sulphate.(4) filtrate obtained suction filtration is fast
Speed is transferred in open-top receptacle, stands kept for 6 hours after being cooled to 15 DEG C at room temperature, room temperature filters, and it is brilliant to obtain transparent sodium acetate
Body.The sodium acetate rate of recovery is 84%, and sulfate radical removal rate is 91.6%.
Embodiment 5
(1) take 82mL sodium sulphate and sodium acetate mixed solution spare, wherein sodium sulfate concentration is 0.28mol/L, sodium acetate
A concentration of 4.80mol/L.(2) it weighs 3.86g calcium oxide to mix with 30mL water, is added with stirring 7.92mL acetic acid reactions to solution
Clarification.(3) step (2) acquired solution is added in the solution of step (1), 80 DEG C of heating stirrings, evaporation removes 36g water, that is, loses
Water percentage is 35%.75 DEG C of heat preservations filter, and obtain the filter cake of sulfur acid calcium and sodium sulphate.(4) filtrate obtained suction filtration is fast
Speed is transferred in open-top receptacle, stands kept for 4 hours after being cooled to 18 DEG C at room temperature, room temperature filters, and it is brilliant to obtain transparent sodium acetate
Body.The sodium acetate rate of recovery is 87%, and sulfate radical removal rate is 92.2%.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (1)
1. a kind of method for detaching sodium acetate in sodium acetate and sodium sulphate mixed system, which is characterized in that add in mixed solution
Enter calcium acetate and form calcium sulfate precipitation, sodium sulphate is precipitated after appropriate water removal, realizes that the desulfurization of mixed solution, crystallization obtain acetic acid
Sodium specifically comprises the following steps：
(1) mixed solution prepares：Take the mixed solution of sodium sulphate and sodium acetate, wherein solution sulfur acid na concn be 0.18~
0.34mol/L, sodium acetate concentration are 3.65~4.95mol/L；
(2) prepared by calcium acetate：Calcium oxide and water are mixed, the mixed system of paste liquid or solid-liquid is obtained, under stirring
Acetic acid is added, reaction to solution is clarified, spare；
(3) desulfurization is precipitated：Step (2) acquired solution is added in sodium acetate and sodium sulphate mixed system obtained by step (1), simultaneously
Carrying out heating stirring makes solution be uniformly mixed, and system becomes cloudy, that is, has calcium sulfate precipitation generation, continuous heating stirring to keep mixing molten
Liquid dehydration, with the evaporation of moisture, precipitation increases, and solid sodium sulfate is precipitated together, and heat preservation is filtered to remove sulfur acid calcium and sulfuric acid
The precipitation of sodium, sulfate radical removal rate are 90.0%~95.0%；
(4) sodium acetate crystallizes：Filtrate obtained by step (3) is transferred in clean container, is stored at room temperature, is cooled to 10~20 DEG C
It is kept for 2~6 hours under this temperature range afterwards, keeps sodium acetate crystallization complete, after the completion of crystallization, room temperature filtering is obtained containing absorption
The acetic acid sodium crystal of water and the crystallization water, the rate of recovery of sodium acetate is 60~95% after water removal, and purity is 85.0~95.0%；
In the step (1), one kind in sodium sulfate concentration 0.23mol/L, 0.26mol/L, 0.28mol/L, sodium acetate
A concentration of 4.40mol/L, 4.70mol/L, 4.80mol/L in one kind；
The molar ratio of Calcium Oxide Dosage and sodium sulphate in former mixed solution is (2~3) in the step (2):1, water is added
The mass ratio of amount and calcium oxide is (6~8)：1, the molar ratio that acetic acid amount and calcium oxide is added is (1.7~3.0):1, stirring speed
Degree is 50~300rpm；
The appropriate removal process of the instant liquid system of evaporation water loss process in the step (3), dehydration percentage are that evaporation is lost
Water quality accounts for percentage of the total solution containing water quality, the non-percentage for accounting for solution gross mass, and dehydration percentage is 28%~42%,
The heating temperature of step (3) is 60~100 DEG C, and mixing speed is 50~300rpm, and heat preservation filtration temperature is 50~100
DEG C, heat preservation is filtered into heat preservation decompression and filters or keep the temperature press filtration, and heat preservation decompression, which filters, selects Buchner funnel to operate, and heat preservation press filtration is selected
Filter press operates；
Room temperature is filtered into room temperature decompression suction filtration or room temperature press filtration in the step (4), and room temperature decompression, which filters, selects Buchner funnel
Filter press operation is selected in operation, room temperature press filtration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610203630.8A CN105837431B (en) | 2016-04-01 | 2016-04-01 | A kind of method that sodium acetate is detached in sodium acetate and sodium sulphate mixed system |
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| CN113292416A (en) * | 2021-06-04 | 2021-08-24 | 枣庄市泰瑞精细化工有限公司 | Production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid |
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