CN104177248B - A kind of distillation residual liquid treatment process of vat powder mother liquor - Google Patents
A kind of distillation residual liquid treatment process of vat powder mother liquor Download PDFInfo
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- CN104177248B CN104177248B CN201410420177.7A CN201410420177A CN104177248B CN 104177248 B CN104177248 B CN 104177248B CN 201410420177 A CN201410420177 A CN 201410420177A CN 104177248 B CN104177248 B CN 104177248B
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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
- C01D5/14—Preparation of sulfites
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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
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- Oil, Petroleum & Natural Gas (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention relates to a kind of distillation residual liquid treatment process of vat powder mother liquor, it is the improvement of the distillation residual liquid treatment process to existing vat powder mother liquor, comprise distillation residual liquid vacuum concentration, cross and filter the impurity of precipitation, the impurity of precipitation with in and the thick S-WAT of remanufacture after mother liquor washing; After filtrate is continued vacuum concentration, concentrated solution is proceeded to insulation separator, after sedimentation, carry out oily water separation; The oil phase separated enters waste tank, enters burning operation, and the aqueous phase separated puts into crystallizing pan, stirs lower crystallisation by cooling, centrifugation.Obtain granularity is good, sodium formiate content is high recovery dry product sodium formiate and centrifuge mother liquor.The present invention has the following advantages: the sodium formiate content of the recovery dry product of acquisition is high, can reach more than 88%, higher than existing common processes more than 8 percentage points; Enter the waste residue amount of burning operation few, be only about 1/3 of existing technique, aftertreatment cost is low.Do not need secondary recovery methyl alcohol.
Description
Technical field
The present invention relates to a kind of distillation residual liquid treatment process of vat powder mother liquor.
Background technology
Through the development of two more than ten years, sodium formate method progressively replaces the topmost method that zinc powder method becomes vat powder production.Produce at sodium formate method in the process of vat powder, need carry out synthetical recovery process to unnecessary mother liquor, it has become the important component part of sodium formate method vat powder production system.To the treatment process of vat powder mother liquor, many sections of documents are reported, as, the process of CN89102534.0 vat powder waste liquid and the recovery method of S-WAT and sodium-chlor, CN96118152.4 utilization is produced methanol-water rectifying tower distillation residual liquid in V-Brite B process and is produced the method for formic acid, and CN03112293.0 mono-kind utilizes the method for crude carbinol distillation residual liquid production sodium formiate in vat powder production process and CN200710027443.X sodium formate method to produce the treatment process of the raffinate in V-Brite B process after mother liquor rectifying recovery methyl alcohol.
Existing vat powder manufacturing enterprise produces unnecessary mother liquor to vat powder and adopts following technical process: vat powder produce unnecessary mother liquor through add alkali neutralization and filter obtain S-WAT with in and mother liquor; In and mother liquor obtain methyl alcohol and distillation residual liquid through rectifying; Distillation residual liquid must reclaim dry product sodium formiate and extraction liquid through concentrating, with refined methanol extraction, press filtration; Extraction liquid obtains methyl alcohol and waste residue through distillation; This waste residue enters waste tank, carries out burning disposal; Its technical process is see such as Fig. 1.
Production practice show, above-mentioned existing technique exists following shortcoming and defect: one, in and the requirement of operation high, otherwise the sodium formiate content of the recovery dry product sodium formiate of gained is low, of poor quality.When low for this content, ropy recovery dry product sodium formiate being used for vat powder production, vat powder being produced and produces obvious disadvantageous effect; Two, secondary recovery methyl alcohol is needed; Three, waste residue generation is large, and aftertreatment cost is high.
Summary of the invention
The present invention is the improvement of the distillation residual liquid treatment process to existing vat powder mother liquor, its object is to overcome above-mentioned defect and deficiency, provide that a kind of sodium formiate content reclaiming dry product sodium formiate is high, waste residue amount is few, aftertreatment cost is low, do not need the distillation residual liquid treatment process of the vat powder mother liquor of secondary recovery methyl alcohol, advanced technology.
Technical scheme of the present invention is: a kind of distillation residual liquid treatment process of vat powder mother liquor, it is characterized in that the distillation residual liquid treatment process steps of described vat powder mother liquor is as follows:
A, when being 95 ~ 100 DEG C by distillation residual liquid vacuum concentration to solution temperature, closing vacuum, emptying, concentrated solution during gained 95 ~ 100 DEG C is filtered, the inorganic salt impurities that removing is separated out; During the inorganic salt impurities of separating out is used and after mother liquor washing, the thick sub-sodium of remanufacture; Filtrate after filtration enters lower step;
B, when filtrate continued vacuum concentration to solution temperature is 105 ~ 110 DEG C, closes vacuum, emptying, concentrated solution during gained 105 ~ 110 DEG C is proceeded to insulation separator;
Concentrated solution when C, gained 105 ~ 110 DEG C after 5-10 minute, carries out oil, water two-phase laminated flow in the sedimentation of insulation separator; The oil phase separated enters waste tank, and waste liquid enters burning operation; The aqueous phase separated continues to enter lower step;
D, aqueous phase is put into crystallizing pan, when to stir lower crystallisation by cooling to temperature be 60 ~ 70 DEG C, adopt whizzer to carry out centrifugation, obtain granularity is good, sodium formiate content is high recovery dry product sodium formiate and centrifuge mother liquor; And be no more than 4.5% index recycled as centrifuge mother liquor to obtain the content reclaiming Sulfothiorine in dry product sodium formiate, namely when obtaining the content reclaiming Sulfothiorine in dry product and being no more than 4.5%, centrifuge mother liquor is back in distillation residual liquid and continues to concentrate; When the content of Sulfothiorine in acquisition recovery dry product is more than 4.5%, centrifuge mother liquor is entered waste tank, enter burning operation together with the oil phase that step C separates.
The technical characteristic of this technique is:
One, in the treatment process process of distillation residual liquid, first by distillation residual liquid vacuum concentration to 95 ~ 100 DEG C, the inorganic salt impurities filtering precipitation is crossed.During the inorganic salt impurities of separating out is used and after mother liquor washing, the thick S-WAT of remanufacture.
Two, in the treatment process process of distillation residual liquid, in insulation separator, oil, water two-phase laminated flow are carried out in sedimentation.
Three, centrifuge mother liquor recycles.
The present invention is the improvement of the treatment process of distillation residual liquid to existing vat powder mother liquor, this technique is adopted to overcome the deficiency of existing technique, the present invention has the following advantages: the sodium formiate content of the recovery dry product sodium formiate one, obtained is high, can more than 88% be reached, higher than common processes more than 8 percentage points; Two, enter the waste residue amount of burning operation few, be only about 1/3 of existing technique, aftertreatment cost is low.Three, secondary recovery methyl alcohol is not needed.
Accompanying drawing explanation
Fig. 1 is the existing process flow sheet of existing vat powder disposing mother liquor;
Fig. 2 is the distillation residual liquid processing technological flow figure of vat powder mother liquor of the present invention.
Embodiment
With reference to figure 2, a kind of distillation residual liquid treatment process of vat powder mother liquor, is characterized in that the distillation residual liquid treatment process steps of described vat powder mother liquor is as follows:
A, when being 95 ~ 100 DEG C by distillation residual liquid vacuum concentration to solution temperature, close vacuum, emptying, concentrated solution during gained 95 ~ 100 DEG C is filtered, the inorganic salt impurities that removing is separated out, during the inorganic salt impurities of separating out is used and after mother liquor washing, the thick S-WAT of remanufacture; Filtrate after filtration enters lower step;
B, when filtrate continued vacuum concentration to solution temperature is 105 ~ 110 DEG C, closes vacuum, emptying, concentrated solution during gained 105 ~ 110 DEG C is proceeded to insulation separator;
Concentrated solution when C, gained 105 ~ 110 DEG C after 5-10 minute, carries out oil, water two-phase laminated flow in the sedimentation of insulation separator; The oil phase separated enters waste tank, and waste liquid enters burning operation; The aqueous phase separated continues to enter lower step;
D, aqueous phase is put into crystallizing pan, when to stir lower crystallisation by cooling to temperature be 60 ~ 70 DEG C, adopt whizzer to carry out centrifugation, obtain granularity is good, sodium formiate content is high recovery dry product sodium formiate and centrifuge mother liquor; And be no more than 4.5% index recycled as centrifuge mother liquor to obtain the content reclaiming Sulfothiorine in dry product sodium formiate, namely when obtaining the content reclaiming Sulfothiorine in dry product and being no more than 4.5%, centrifuge mother liquor is back in distillation residual liquid and continues to concentrate; When the content of Sulfothiorine in acquisition recovery dry product is more than 4.5%, centrifuge mother liquor is entered waste tank, enter burning operation together with the oil phase that step C separates.
Following examples are to invention has been detailed description.
Embodiment 1
Between picking up the car, certain batch of distillation residual liquid is tested.At 25 DEG C, analytical results is: proportion 1.125, sodium-chlor 33.1 grams per liter, S-WAT 16.41 grams per liter, Sulfothiorine 50.66 grams per liter, sodium formiate 212.6 grams per liter.Add up to add 3000 milliliters of above-mentioned distillation residual liquids in 1000 milliliters of four-hole bottles of band stirring, thermometer, under vacuum tightness-0.085 ~ 0.090Mpa, heating is concentrated, when being concentrated into solution temperature 95 DEG C, stop heating, emptying, closedown vacuum, material vacuum suction filtration, filtrate continues vacuum concentration to 110 DEG C, close vacuum, emptying, material is proceeded to insulation separator, be separated and obtain 55 milliliters of oily matter and without oily filtrate.To proceed to without oily filtrate in the crystallization reactor of band stirring, crystallisation by cooling to 60 ~ 70 DEG C, centrifugation, must reclaim dry product and 145 milliliters of centrifuge mother liquors.Measure the content reclaiming sodium formiate, sodium-chlor, S-WAT, Sulfothiorine and fugitive constituent in dry product with chemical analysis analysis, measured value is respectively 90.6%, 2.8%, 1.3%, 2.5% and 2.8%.In gained recovery dry product, sodium thiosulfate content is lower than 4.5%, and centrifuge mother liquor recycles.
Embodiment 2
The workshop distillation residual liquid that Example 1 is identical is tested.The accumulative centrifuge mother liquor adding 3000 milliliters of distillation residual liquids and embodiment 1 gained in 1000 milliliters of four-hole bottles to band stirring, thermometer, under vacuum tightness-0.085 ~ 0.090Mpa, heating is concentrated, when being concentrated into solution temperature 100 DEG C, stop heating, emptying, closedown vacuum, material vacuum suction filtration, filtrate continues vacuum concentration to 110 DEG C, close vacuum, emptying, being heated up by material proceeds to insulation separator, is separated and obtains 55 milliliters of oily matter and without oily filtrate.To proceed to without oily filtrate in the crystallization reactor of band stirring, crystallisation by cooling to 60 ~ 70 DEG C, centrifugation, must reclaim dry product and centrifuge mother liquor.The content reclaiming sodium formiate, sodium-chlor, S-WAT, Sulfothiorine and fugitive constituent in dry product is measured with chemical analysis analysis, measured value is respectively 91.3%, 2.5%, 0.9%, 2.8% and 2.5%, in gained recovery dry product, sodium thiosulfate content is lower than 4.5%, and centrifuge mother liquor recycles.
Embodiment 3
The workshop distillation residual liquid that Example 3 is identical is tested.The accumulative centrifuge mother liquor adding 3000 milliliters of distillation residual liquids and recycle through 7 times in 1000 milliliters of four-hole bottles to band stirring, thermometer, under vacuum tightness-0.085 ~ 0.090Mpa, heating is concentrated, when being concentrated into solution temperature 100 DEG C, stop heating, emptying, closedown vacuum, material vacuum suction filtration, filtrate continues vacuum concentration to 115 DEG C, close vacuum, emptying, material is proceeded to insulation separator, be separated and obtain 55 milliliters of oily matter and without oily filtrate.To proceed to without oily filtrate in the crystallization reactor of band stirring, crystallisation by cooling to 60 ~ 70 DEG C, centrifugation, must reclaim dry product and centrifuge mother liquor.The content reclaiming sodium formiate, sodium-chlor, S-WAT, Sulfothiorine and fugitive constituent in dry product is measured with chemical analysis analysis, measured value is respectively 88.5%, 2.7%, 1.6%, 4.7% and 2.5%, in gained recovery dry product, sodium thiosulfate content is higher than 4.5%, and centrifuge mother liquor does not recycle.
Claims (2)
1. a distillation residual liquid treatment process for vat powder mother liquor, is characterized in that the distillation residual liquid treatment process steps of described vat powder mother liquor is as follows:
A, when being 95 ~ 100 DEG C by distillation residual liquid vacuum concentration to solution temperature, closing vacuum, emptying, concentrated solution during gained 95 ~ 100 DEG C is filtered, the inorganic salt impurities that removing is separated out; During the inorganic salt impurities of separating out is used and after mother liquor washing, the thick S-WAT of remanufacture; Filtrate after filtration enters lower step;
B, when filtrate continued vacuum concentration to solution temperature is 105 ~ 110 DEG C, closes vacuum, emptying, concentrated solution during gained 105 ~ 110 DEG C is proceeded to insulation separator;
Concentrated solution when C, gained 105 ~ 110 DEG C after 5-10 minute, carries out oil, water two-phase laminated flow in the sedimentation of insulation separator; The oil phase separated enters waste tank, and waste liquid enters burning operation, and the aqueous phase separated continues to enter lower step;
D, aqueous phase is put into crystallizing pan, when to stir lower crystallisation by cooling to temperature be 60 ~ 70 DEG C, adopt whizzer to carry out centrifugation, obtain granularity is good, sodium formiate content is high recovery dry product sodium formiate and centrifuge mother liquor; And be no more than 4.5% index recycled as centrifuge mother liquor to obtain the content reclaiming Sulfothiorine in dry product sodium formiate, namely, when obtaining the content reclaiming Sulfothiorine in dry product sodium formiate and being no more than 4.5%, centrifuge mother liquor is back in distillation residual liquid and continues to concentrate; When the content of Sulfothiorine in acquisition recovery dry product is more than 4.5%, centrifuge mother liquor is entered waste tank, enter burning operation together with the oil phase that step C separates.
2. the distillation residual liquid treatment process of a kind of vat powder mother liquor as claimed in claim 1, is characterized in that described centrifuge mother liquor recycles.
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| CN106706841B (en) * | 2016-12-13 | 2019-02-05 | 柳州化工股份有限公司 | The analysis method of sodium formate purity is recycled in sodium hydrosulfite production |
| CN107011160A (en) * | 2017-04-06 | 2017-08-04 | 济南大学 | The separation method of sodium formate in a kind of sodium hydrosulfite waste residue |
Citations (3)
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| CN1164527A (en) * | 1996-05-08 | 1997-11-12 | 谈宇清 | Method for producing formic acid by using methanol-water rectifying tower residue produced in course of producing sodium hyposulfite |
| CN1459444A (en) * | 2003-05-29 | 2003-12-03 | 烟台市金河保险粉厂有限公司 | Method for producing sodium formate by using crude methanol rectification residual liquid in sodium hydrosulfite production process |
| CN101081715A (en) * | 2007-04-06 | 2007-12-05 | 广东中成化工股份有限公司 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001259665A (en) * | 2000-03-23 | 2001-09-25 | Mitsubishi Gas Chem Co Inc | Hydrosulfite production waste liquid treating method |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1164527A (en) * | 1996-05-08 | 1997-11-12 | 谈宇清 | Method for producing formic acid by using methanol-water rectifying tower residue produced in course of producing sodium hyposulfite |
| CN1459444A (en) * | 2003-05-29 | 2003-12-03 | 烟台市金河保险粉厂有限公司 | Method for producing sodium formate by using crude methanol rectification residual liquid in sodium hydrosulfite production process |
| CN101081715A (en) * | 2007-04-06 | 2007-12-05 | 广东中成化工股份有限公司 | Method for treating residual liquid after mother liquor distillation methanol recovery during production of sodium sulphoxylate by sodium formate process |
Non-Patent Citations (2)
| Title |
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| 中国甲酸钠法制保险粉技术的发展及展望;黄力群;《无机盐工业》;20070630;第39卷(第6期);4-6 * |
| 提高保险粉生产中母液利用率的新工艺;高虹;《安徽化工》;20070228;第33卷(第1期);43-44 * |
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