CN105601499A - Method for separating sodium acetate solution containing sodium sulfate - Google Patents
Method for separating sodium acetate solution containing sodium sulfate Download PDFInfo
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- CN105601499A CN105601499A CN201610006575.3A CN201610006575A CN105601499A CN 105601499 A CN105601499 A CN 105601499A CN 201610006575 A CN201610006575 A CN 201610006575A CN 105601499 A CN105601499 A CN 105601499A
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- sodium acetate
- sodium
- sodium sulfate
- solution
- crystallization
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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
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- 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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for separating a sodium acetate solution containing sodium sulfate and belongs to the field of sodium acetate separation and recycling. The separation method includes the steps that the solution is dehydrated through evaporation, stepped crystallization and separation of sodium sulfate and sodium acetate are achieved, and the processes of mixed solution preparation, evaporation and dehydration, sodium sulfate separation and sodium acetate crystallization are conducted. According to the method for separating the sodium acetate solution containing sodium sulfate, the separation effect is good, sulfate ions in mother liquor of sodium acetate are crystallized and precipitated in the form of sodium sulfate, the removal rate of sulfate radicals is 90.0-98.0%, and sodium acetate in the solution is crystallized and recycled and can be utilized in a circulating mode. The method is simple in technological process, high in efficiency, low in cost, small in energy consumption and suitable for industrial production and waste liquid treatment of relates fields.
Description
Technical field
The present invention relates to a kind of sodium acetate and separate recovery field, refer to especially a kind of contains sodium sulfateThe method that SAS separates.
Background technology
Sodium acetate claims again anhydrous sodium acetate, and molecular formula is CH3COONa or NaAc, extensively shouldFor Chemical Manufacture, therefore often can produce the industrial wastes containing a large amount of sodium acetates, at Hou ChuIn reason, obtain moisture sodium acetate crystal by the method for crystallization. In some production fields, uselessIn liquid, comprise sulfate radical simultaneously, need to carry out the sulfate radical processing of waste liquid, conventionally adopt and addThe method of precipitating ion generates sulfate precipitation and carrys out sulphur removal, but this method has improved liquid waste processingCost, introduced other anion, and needed complicated process equipment, flow process complexity,Energy consumption is large, in order to improve technique, exploration sodium acetate mother liquor simple, contains sodium sulfate efficientlySeparation method, we have probed into by evaporation and have made solution dehydration realize sodium sulphate and sodium acetate substepThe method of Crystallization Separation, has obtained desirable effect.
Summary of the invention
The separative efficiency of sodium acetate mother liquor that the present invention will solve contains sodium sulfate is low, and cost is high, returnsThe technical problem that yield is low, a kind of method that therefore provides SAS of contains sodium sulfate to separate,The fractional crystallization that makes solution dehydration realize sodium sulphate and sodium acetate by evaporation realizes with separatingThe separation of the sodium acetate mother liquor of contains sodium sulfate, method is simple, and cost is low, good separating effect,The rate of recovery is high.
To achieve the above object, technical scheme of the present invention is: a kind of vinegar of contains sodium sulfateThe separation method of acid sodium solution, is characterized in that, makes mixed solution dehydration realize sulphur by evaporationThe fractional crystallization of acid sodium and sodium acetate with separate, specifically comprise the steps:
(1) mixed solution is prepared: get the SAS of contains sodium sulfate, wherein solution sulfur-bearingAcid na concn is 0.17～0.35mol/L, and sodium acetate concentration is 3.33～6.38mol/L;
(2) evaporation water loss: the ready solution of step (1) is added to thermal agitation, be evaporated to moltenLiquid dehydration percentage is 41.6～54.4%, and to be wherein that evaporation water loss quality accounts for former molten for dehydration percentageIn liquid, containing the percentage of water quality, along with the evaporation of moisture, it is muddy that solution becomes gradually, has sulphurAcid sodium crystal is separated out;
(3) sodium sulphate separates: step (2) gained dirty solution is incubated to filtration while hot,To filter cake be hard blocks of solid, the filter cake obtaining is the solid filter residue containing 75～90% sodium sulphate,In solution, the clearance of sodium sulphate is 90.0～98.0%;
(4) sodium acetate crystallization: the filtrate obtaining in step (3) is transferred to rapidly cleanOpen-top receptacle, leaves standstill under room temperature, keeps 0.5～2 after being cooled to 10～20 DEG C under this temperature rangeHour, make sodium acetate perfect crystalline, after crystallization completes, normal temperature filters, obtain containing adsorbed water andThe sodium acetate crystal of the crystallization water, removes the rate of recovery of sodium acetate after adsorbed water and the crystallization water and is60～90%, purity is 99.0～99.6%.
In described step (1), sodium sulfate concentration is 0.23mol/L, 0.26mol/L, 0.28mol/LIn one, the concentration of sodium acetate is one in 4.29mol/L, 4.66mol/L, 4.80mol/LKind.
The temperature that adds thermal agitation and evaporation operation in described step (2) is 60～100 DEG C, stirsThe speed of mixing is 50～300rpm, and dehydration percentage is 48.0% or 52.0%.
In described step (3), insulation filtration temperature is 50～100 DEG C, and insulation is filtered into insulationDecompress filter or insulation press filtration, insulation decompress filter is selected Buchner funnel operation, insulation press filtration choosingOperate with filter press.
In described step (4), normal temperature is filtered into normal temperature decompress filter or normal temperature press filtration, normal temperatureDecompress filter is selected Buchner funnel operation, and filter press operation is selected in normal temperature press filtration.
The beneficial effect of technique scheme of the present invention is as follows:
(1) the present invention by evaporation dewater sodium sulfate crystal method separate remove in mixed liquorSulfate ion, method is simple, do not need the material of introducing other to react with sulfate radicalRealize sulphur removal, reduced the cost of processing mixed liquor, avoided introducing more heteroion simultaneously,Cause puzzlement to the subsequent treatment of solution.
(2) steam being evaporated in the present invention can reclaim through apparatus for supercooling condensation,In industrial production, be cycled to used in other steps, the circulation that realizes resource efficiently utilizes, and reduces workThe cost of industry water; After processing, gained liquor capacity is former mixed liquor volume 3～25%, the utmost pointLarge minimizing the discharge capacity of industrial wastewater.
(3) in the sodium acetate crystal that crystallization obtains, sodium sulphate content is 0.4～1%, and sodium acetate is pureSpend high, can direct circulation for the production of in, reduce production cost.
(4) technical process of the present invention is simple, can adopt simple process equipment to process,Processing cost is low, and can realize recycling of water and sodium acetate, saves energy consumption.
Brief description of the drawings
Fig. 1 is the separation method schematic diagram of the SAS of contains sodium sulfate of the present invention.
Detailed description of the invention
For making the technical problem to be solved in the present invention, technical scheme and advantage clearer, belowBe described in detail in connection with specific embodiment.
The method that the SAS of contains sodium sulfate separates, specific embodiment is as follows:
Embodiment 1
(1) get the sodium acetate mother liquor of 165mL contains sodium sulfate for subsequent use, wherein sodium sulfate concentration is0.26mol/L, sodium acetate concentration is 4.66mol/L. (2) 100 DEG C add thermal agitation, and evaporation is removed65g water, dehydration percentage is 52.0%. (3) 80 DEG C of insulation suction filtrations, obtain containing a large amount of sulphurThe filter cake of acid sodium. (4) filtrate suction filtration being obtained is transferred to rapidly in open-top receptacle, under room temperatureLeave standstill after being cooled to 10 DEG C and keep 2 hours, normal temperature suction filtration, obtains transparent sodium acetate crystal.The purity that mensuration is amounted to rear sodium acetate is 99.5%, and sodium sulphate clearance is 97.1%.
Embodiment 2
(1) get the sodium acetate mother liquor of 165mL contains sodium sulfate for subsequent use, wherein sodium sulfate concentration is0.17mol/L, sodium acetate concentration is 3.33mol/L. (2) 60 DEG C add thermal agitation, and evaporation is removed68g water, dehydration percentage is 54.4%. (3) 50 DEG C of insulation suction filtrations, obtain containing a large amount of sulphurThe filter cake of acid sodium. (4) filtrate suction filtration being obtained is transferred to rapidly in open-top receptacle, under room temperatureLeave standstill after being cooled to 15 DEG C and keep 1 hour, normal temperature suction filtration, obtains transparent sodium acetate crystal.Sodium acetate purity after mensuration is amounted to is 99.3%, and sodium sulphate clearance is 93.2%.
Embodiment 3
(1) get the sodium acetate mother liquor of 165mL contains sodium sulfate for subsequent use, wherein sodium sulfate concentration is0.34mol/L, sodium acetate concentration is 6.38mol/L. (2) 85 DEG C add evaporation under thermal agitation and remove52g water, dehydration percentage is 41.6%. (3) 100 DEG C of insulation suction filtrations, obtain containing a large amount of sulphurThe filter cake of acid sodium. (4) filtrate suction filtration being obtained is transferred to rapidly in open-top receptacle, under room temperatureLeave standstill after being cooled to 20 DEG C and keep 0.5 hour, normal temperature suction filtration, obtains transparent sodium acetate crystal.Sodium acetate purity after mensuration is amounted to is 99.2%, and sodium sulphate clearance is 91.9%.
Embodiment 4
(1) get the sodium acetate mother liquor of 165mL contains sodium sulfate for subsequent use, wherein sodium sulfate concentration is0.23mol/L, sodium acetate concentration is 4.29mol/L. (2) 98 DEG C add evaporation under thermal agitation and remove60g water, dehydration percentage is 48.0%. (3) 80 DEG C of insulation suction filtrations, obtain containing a large amount of sulphurThe filter cake of acid sodium. (4) filtrate suction filtration being obtained is transferred to rapidly in open-top receptacle, under room temperatureLeave standstill after being cooled to 15 DEG C and keep 1 hour, normal temperature suction filtration, obtains transparent sodium acetate crystal.Sodium acetate purity after mensuration is amounted to is 99.0%, and sodium sulphate clearance is 91.6%.
Embodiment 5
(1) get the sodium acetate mother liquor of 165mL contains sodium sulfate for subsequent use, wherein sodium sulfate concentration is0.28mol/L, sodium acetate concentration is 4.80mol/L. (2) 98 DEG C add evaporation under thermal agitation and remove63g water, dehydration percentage is 50.4%. (3) 75 DEG C of insulation suction filtrations, obtain containing a large amount of sulphurThe filter cake of acid sodium. (4) filtrate suction filtration being obtained is transferred to rapidly in open-top receptacle, under room temperatureLeave standstill after being cooled to 18 DEG C and keep 1.5 hours, normal temperature suction filtration, obtains transparent sodium acetate crystal.Sodium acetate purity after mensuration is amounted to is 99.3%, and sodium sulphate clearance is 94.2%.
The above is the preferred embodiment of the present invention, it should be pointed out that for the artThose of ordinary skill, not departing under the prerequisite of principle of the present invention, can also doGo out some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. a separation method for the SAS of contains sodium sulfate, is characterized in that, by steamingSend out and make fractional crystallization that mixed solution dehydration realizes sodium sulphate and sodium acetate and separate, specifically compriseFollowing steps:
(1) mixed solution is prepared: get the SAS of contains sodium sulfate, wherein solution sulfur-bearingAcid na concn is 0.17～0.35mol/L, and sodium acetate concentration is 3.33～6.38mol/L;
(2) evaporation water loss: the ready solution of step (1) is added to thermal agitation, be evaporated to moltenLiquid dehydration percentage is 41.6～54.4%, and to be wherein that evaporation water loss quality accounts for former molten for dehydration percentageIn liquid, containing the percentage of water quality, along with the evaporation of moisture, it is muddy that solution becomes gradually, has sulphurAcid sodium crystal is separated out;
(3) sodium sulphate separates: step (2) gained dirty solution is incubated to filtration while hot,To filter cake be hard blocks of solid, the filter cake obtaining is the solid filter residue containing 75～90% sodium sulphate,In solution, the clearance of sodium sulphate is 90.0～98.0%;
(4) sodium acetate crystallization: the filtrate obtaining in step (3) is transferred to rapidly cleanOpen-top receptacle, leaves standstill under room temperature, keeps 0.5～2 after being cooled to 10～20 DEG C under this temperature rangeHour, make sodium acetate perfect crystalline, after crystallization completes, normal temperature filters, obtain containing adsorbed water andThe sodium acetate crystal of the crystallization water, removes the rate of recovery of sodium acetate after adsorbed water and the crystallization water and is60～90%, purity is 99.0～99.6%.
2. the separation method of the SAS of contains sodium sulfate according to claim 1, itsBe characterised in that, in described step (1) sodium sulfate concentration be 0.23mol/L, 0.26mol/L,One in 0.28mol/L, the concentration of sodium acetate is 4.29mol/L, 4.66mol/L, 4.80mol/LIn one.
3. the separation method of the SAS of contains sodium sulfate according to claim 1,It is characterized in that, the temperature that adds thermal agitation and evaporation operation in described step (2) is60～100 DEG C, mixing speed is 50～300rpm, and dehydration percentage is 48.0% or 52.0%.
4. the separation method of the SAS of contains sodium sulfate according to claim 1,It is characterized in that, in described step (3), insulation filtration temperature is 50～100 DEG C, is incubatedFilter is insulation decompress filter or insulation press filtration, and insulation decompress filter is selected Buchner funnel operation, protectsTemperature and pressure filtering operates with filter press.
5. the separation method of the SAS of contains sodium sulfate according to claim 1,It is characterized in that, in described step (4), normal temperature is filtered into normal temperature decompress filter or normal temperature pressureFilter, normal temperature decompress filter is selected Buchner funnel operation, and filter press operation is selected in normal temperature press filtration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610006575.3A CN105601499B (en) | 2016-01-04 | 2016-01-04 | A kind of separation method of the sodium acetate solution of sulfur acid sodium |
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| CN201610006575.3A CN105601499B (en) | 2016-01-04 | 2016-01-04 | A kind of separation method of the sodium acetate solution of sulfur acid sodium |
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| CN105601499A true CN105601499A (en) | 2016-05-25 |
| CN105601499B CN105601499B (en) | 2018-02-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605336A (en) * | 2022-04-06 | 2022-06-10 | 荆州三才堂化工科技有限公司 | Method for post-treatment of synthesis of 4, 6-dihydroxypyrimidine and resource utilization of wastewater thereof |
Citations (4)
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|---|---|---|---|---|
| EP1132488A1 (en) * | 2000-03-07 | 2001-09-12 | Va Tech Wabag AG | Installation with cooled crystallisers and method for operating the installation |
| CN101774903A (en) * | 2010-03-04 | 2010-07-14 | 陈庸彪 | Method for extracting n-butyric acid, valeric acid and hexoic acid from lyechange as by-product of cyclohexanone production |
| CN101898953A (en) * | 2009-05-27 | 2010-12-01 | 薛平 | Technological research for producing sodium acetate by comprehensively utilizing chemical waste liquid |
| CN104086398A (en) * | 2014-07-15 | 2014-10-08 | 中南大学 | Method for separating and recovering oxalic acid from waste oxalic acid liquor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1132488A1 (en) * | 2000-03-07 | 2001-09-12 | Va Tech Wabag AG | Installation with cooled crystallisers and method for operating the installation |
| CN101898953A (en) * | 2009-05-27 | 2010-12-01 | 薛平 | Technological research for producing sodium acetate by comprehensively utilizing chemical waste liquid |
| CN101774903A (en) * | 2010-03-04 | 2010-07-14 | 陈庸彪 | Method for extracting n-butyric acid, valeric acid and hexoic acid from lyechange as by-product of cyclohexanone production |
| CN104086398A (en) * | 2014-07-15 | 2014-10-08 | 中南大学 | Method for separating and recovering oxalic acid from waste oxalic acid liquor |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114605336A (en) * | 2022-04-06 | 2022-06-10 | 荆州三才堂化工科技有限公司 | Method for post-treatment of synthesis of 4, 6-dihydroxypyrimidine and resource utilization of wastewater thereof |
| CN114605336B (en) * | 2022-04-06 | 2024-01-26 | 荆州三才堂化工科技有限公司 | Post-treatment and waste water resource utilization method for synthesizing 4, 6-dihydroxypyrimidine |
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