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CN107602373A - A kind of method that sodium acetate is extracted from furfural production waste water - Google Patents

A kind of method that sodium acetate is extracted from furfural production waste water Download PDF

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Publication number
CN107602373A
CN107602373A CN201710821652.5A CN201710821652A CN107602373A CN 107602373 A CN107602373 A CN 107602373A CN 201710821652 A CN201710821652 A CN 201710821652A CN 107602373 A CN107602373 A CN 107602373A
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waste water
sodium acetate
production waste
furfural production
dope
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CN201710821652.5A
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CN107602373B (en
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王永红
宗锁弟
刘永忠
张爱雄
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Shanxi Hengde Yi Biotechnology Co
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Shanxi Hengde Yi Biotechnology Co
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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Fertilizers (AREA)
  • Heat Treatment Of Water, Waste Water Or Sewage (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a kind of method that sodium acetate is extracted from furfural production waste water, it is to add sodium carbonate in the furfural production waste water that 2.5 ~ 3%, pH value is 1 ~ 2.5 to be neutralized, filter, preheat, evaporate, concentrate, decolourize, filter, condense, crystallize, centrifuge out sodium acetate to the acetic acid content discharged by destilling tower bottom of towe, sodium acetate is packed after being down to room temperature, is put in storage.The present invention realizes that sodium acetate does not crystallize or can not form sodium acetate in waste water conversion process by adjusting process step and technological parameter, only after processing is completed, by crystallizing, separating, packing sodium acetate, line clogging and the wasting of resources are avoided, ensures being normally carried out for production.

Description

A kind of method that sodium acetate is extracted from furfural production waste water
Technical field
The invention belongs to furfural production technical field, is related to a kind of method that sodium acetate is extracted from furfural production waste water.
Background technology
Current Chinese furfural production manufacturer is numerous, and the primary raw material due to producing furfural is corncob, furfural production producer Distribution is more scattered, is concentrated mainly on the corn place of production, and is distributed in rural area mostly, and production technology falls behind, and environmental consciousness is not strong.Chaff Aldehyde production technology uses hydrochloric acid catalysis using sulfuric acid catalysis method is a small number of more, pollutes quite serious.Furfural traditional processing technology waste water Yield is big, and substantial amounts of acetic acid, furfural and other organic pollutions are contained in waste water.Hydrolyzer bottom discharge largely containing sulfuric acid, The hot and humid aldehyde slag of acetic acid and furfural.
Domestic furfural industry, the processing of furfural production technology waste water is always a hard nut to crack, without more ripe Processing method, pollution of the in line formation to environment after waste water is aerified using directly evaporation of most of manufacturers, simultaneously Waste resource.A few studies are also at theoretic discussion and experimental stage.
Refined sodium acetate is a kind of Organic Chemicals for having extensive use.In medical industry, for producing benzyl green grass or young crops Mycin sodium, mordant is used as in printing and dyeing industry, the buffer solution of bath pH values is used as in electroplating industry, make coating crystallization thin Cause;Photograph setting agent, preservative for meat and chemical reagent can be done, can also produce glacial acetic acid, acetone, acetate, monoxone etc. A variety of chemical products.
Because sodium acetate is widely used, it is thought that the acetic acid in furfural production waste water is changed into sodium acetate is subject to profit With.But in order to balance cost, small hollow on industrial tube wall inevitably be present, and containing a variety of in furfural production waste water Impurity so that the acetic acid in furfural production waste water only forms mucus collophore or crystallized in advance in pipeline when changing into sodium acetate Block pipeline, cause production to be difficult to, force furfural production to stop because waste water method can not handle.
The content of the invention
In order to solve problems of the prior art, the invention discloses one kind to extract acetic acid from furfural production waste water The method of sodium, it is intended to realize that sodium acetate does not crystallize in waste water conversion process by adjusting process step and technological parameter, only After processing is completed, by crystallizing, separating, packing sodium acetate, line clogging is avoided, ensures being normally carried out for production.
During furfural production, corncob string is hydrolyzed, the aldehyde of output under diluted acid catalysis by high-temperature steam Gas steams furfural on destilling tower top through cooling down and distilling, while production waste water is discharged in destilling tower bottom, and the present invention is exactly will Furfural production waste water containing the plurality of impurities including acetic acid avoids sodium acetate from crystallizing by the adjusting process parameter of creativeness, has Body is achieved by the following technical solution:
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)It is to add carbon in the furfural production waste water that 2.5 ~ 3%, pH value is 1 ~ 2.5 to the acetic acid content discharged by destilling tower bottom of towe Sour sodium is neutralized, then filtrate is delivered to preheater by regulation pH value to being filtered after 5.8 ~ 6.2,170 ~ 197 DEG C, Temperature raising preheats under the conditions of 0.8 ~ 1.2MPa, and it is that 1.06 ~ 1.15, flow is 6.5 ~ 7.0m that evaporation and concentration, which obtains relative density,3/ h's Half dope;
(2)Half dope is drained to enrichment device and is further concentrated to give the dope that relative solubility is 1.25 ~ 1.30;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.0 ~ 6.5kg/ m3
(4)Step will be passed through(3)The dope of processing is condensed to less than 70 DEG C, then the crystallisation by cooling at 40 DEG C, then through centrifugation point Sodium acetate is separated out, sodium acetate is packed after being down to room temperature, is put in storage.
As a kind of preferred embodiment, step(1)Furfural production waste water is by sending with slag boiler after middle preheating 200 ~ 210 DEG C, 1.2 ~ 1.3MPa primary steam and progress heat exchange concentrate obtain half dope, and caused indirect steam is used for water Solution furfural dregs or condensation are back in furfural production waste water.
As a kind of preferred embodiment, the mass ratio of sodium carbonate and furfural waste-water is 0.03 ~ 0.05.
It is preferred that the acetic acid content of destilling tower bottom of towe discharge is that the furfural production waste water that 2.5 ~ 3%, pH value is 1 ~ 2.5 is advanced After row oil removal precipitation, then sodium carbonate is added thereto and is neutralized.
Preferably, step(4)In when centrifuging out sodium acetate, caused mother liquor is back to step(1)Furfural Produce in waste water, participate in neutralizing again, filtering, preheating, a series of operation such as evaporation, continuously move in circles, until by furfural Sodium acetate contained in waste water is produced all to extract.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, without having to pay creative labor, may be used also To obtain other accompanying drawings according to these accompanying drawings.
Fig. 1 is the process chart in embodiment and comparative example.
Embodiment
Describe to be used to disclose the present invention below so that those skilled in the art can realize the present invention.It is excellent in describing below Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Embodiment 1
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)After the furfural production waste water that the acetic acid content discharged by destilling tower bottom of towe is 2.5%, pH value is 1 carries out oil removal precipitation, With sodium carbonate according to 1:0.03 mass ratio is neutralized, and is filtered after regulation pH value to 5.8, then in 170 DEG C, 0.8MPa Under the conditions of temperature raising preheat, then by the furfural production waste water after preheating by sent with slag boiler 200 DEG C, the one of 1.2MPa Secondary steam obtains 1.06, flow 6.5m with carrying out heat exchange concentrate3/ h half dope, caused indirect steam are used to hydrolyze chaff Aldehyde slag or condensation are back in furfural production waste water and re-start circulation;
(2)Half dope is further concentrated to give the dope that relative solubility is 1.25;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.0kg/m3
(4)Step will be passed through(3)The dope of processing is condensed to 69 DEG C, then the crystallisation by cooling under the conditions of 40 DEG C, then through centrifugation point Sodium acetate is separated out, sodium acetate is packed after being down to room temperature, is put in storage;When centrifuging out sodium acetate, produce Mother liquor be back to step(1)Furfural production waste water in, again participate in neutralize, filtering, preheating, evaporation etc. a series of behaviour Make, continuously move in circles, until sodium acetate contained in furfural production waste water is all extracted.
Embodiment 2
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)After the furfural production waste water that the acetic acid content discharged by destilling tower bottom of towe is 3%, pH value is 2.5 carries out oil removal precipitation, With sodium carbonate according to 1:0.05 mass ratio is neutralized, and is filtered after regulation pH value to 6.2, then in 197 DEG C, 1.2MPa Under the conditions of temperature raising preheat, then by furfural production waste water after preheating by sent with slag boiler 210 DEG C, 1.3MPa once Steam obtains 1.15, flow 7.0m with carrying out heat exchange concentrate3/ h half dope, caused indirect steam are used to hydrolyze furfural Slag or condensation are back in furfural production waste water and re-start circulation;
(2)Half dope is further concentrated to give the dope that relative solubility is 1.30;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.5kg/m3
(4)Step will be passed through(3)The dope of processing is condensed to 68 DEG C, then the crystallisation by cooling under the conditions of 40 DEG C, then through centrifugation point Sodium acetate is separated out, sodium acetate is packed after being down to room temperature, is put in storage;When centrifuging out sodium acetate, produce Mother liquor be back to step(1)Furfural production waste water in, again participate in neutralize, filtering, preheating, evaporation etc. a series of behaviour Make, continuously move in circles, until sodium acetate contained in furfural production waste water is all extracted.
Embodiment 3
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)The furfural production waste water that the acetic acid content discharged by destilling tower bottom of towe is 2.8%, pH value is 1.7 ~ 2 carries out oil removal precipitation Afterwards, with sodium carbonate according to 1:0.04 mass ratio is neutralized, regulation pH value to being filtered after 6.0, then 190 DEG C, Temperature raising preheats under the conditions of 1.0MPa, then by furfural production waste water after preheating by sent with slag boiler 203 DEG C, 1.25MPa primary steam is 6.7 ~ 6.8m with carrying out heat exchange concentrate to obtain 1.10 ~ 1.12, flow3/ h half dope, produce Indirect steam be used to hydrolyze furfural dregs or condensation is back in furfural production waste water and re-starts circulation;
(2)Half dope is further concentrated to give the dope that relative solubility is 1.27;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.2kg/m3
(4)Step will be passed through(3)The dope of processing is condensed to less than 68 DEG C, then the crystallisation by cooling under the conditions of 40 DEG C, then through from The heart isolates sodium acetate, and sodium acetate is packed after being down to room temperature, is put in storage;When centrifuging out sodium acetate, Caused mother liquor is back to step(1)Furfural production waste water in, again participate in neutralize, filtering, preheating, evaporation etc. it is a series of Operation, continuously moves in circles, until sodium acetate contained in furfural production waste water is all extracted.
Comparative example 1
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)The furfural production waste water that the acetic acid content discharged by destilling tower bottom of towe is 2.2%, pH value is 0.9 carries out oil removal precipitation Afterwards, with sodium carbonate according to 1:0.025 mass ratio is neutralized, regulation pH value to being filtered after 5.6, then 168 DEG C, Temperature raising is preheated under the conditions of 0.8MPa, and furfural production waste water after preheating then is passed through into 198 DEG C, 1.2MPa being sent with slag boiler Primary steam with carry out heat exchange concentrate obtain 1.05, flow 6.4m3/ h half dope, caused indirect steam are used for water Solution furfural dregs or condensation are back in furfural production waste water and re-start circulation;
(2)Half dope is further concentrated to give the dope that relative solubility is 1.24;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.0kg/m3
(4)Step will be passed through(3)The dope of processing is condensed to less than 68 DEG C, then the crystallisation by cooling at 40 DEG C, then through centrifugation point Sodium acetate is separated out, sodium acetate is packed after being down to room temperature, is put in storage;When centrifuging out sodium acetate, produce Mother liquor be back to step(1)Furfural production waste water in, again participate in neutralize, filtering, preheating, evaporation etc. a series of behaviour Make, continuously move in circles, until sodium acetate contained in furfural production waste water is all extracted.
Comparative example 2
A kind of method that sodium acetate is extracted from furfural production waste water, is achieved by the steps of:
(1)The furfural production waste water that the acetic acid content discharged by destilling tower bottom of towe is 3.2%, pH value is 2.7 carries out oil removal precipitation Afterwards, with sodium carbonate according to 1:0.055 mass ratio is neutralized, regulation pH value to being filtered after 6.4, then 198 DEG C, Temperature raising preheats under the conditions of 1.25MPa, then by furfural production waste water after preheating by sent with slag boiler 212 DEG C, 1.35MPa primary steam obtains 1.18, flow 7.1m with carrying out heat exchange concentrate3/ h half dope, caused secondary steaming Vapour is used to hydrolyze furfural dregs or condensation is back in furfural production waste water and re-starts circulation;
(2)Half dope is further concentrated to give the dope that relative solubility is 1.32;
(3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 6.5kg/m3
(4)Step will be passed through(3)The dope of processing is condensed to less than 69 DEG C, then the crystallisation by cooling under the conditions of 40 DEG C, then through from The heart isolates sodium acetate, and sodium acetate is packed after being down to room temperature, is put in storage;When centrifuging out sodium acetate, Caused mother liquor is back to step(1)Furfural production waste water in, again participate in neutralize, filtering, preheating, evaporation etc. it is a series of Operation, continuously moves in circles, until sodium acetate contained in furfural production waste water is all extracted.
Table 1 is the situation of the pipeline crystallization situation of embodiment and comparative example.
Adjusting process step can be can be seen that with chase experiment situation by embodiment 1-3 and comparative example 1-2 and technique is joined Number realizes that sodium acetate does not crystallize in waste water conversion process, only after processing is completed, by crystallizing, separating, packing sodium acetate, Line clogging is avoided, ensures being normally carried out for production, achieves good effect.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of the industry For personnel it should be appreciated that the present invention is not limited to the above embodiments, that described in above-described embodiment and specification is the present invention Principle, various changes and modifications of the present invention are possible without departing from the spirit and scope of the present invention, these change and Improvement is both fallen within the range of claimed invention.The protection domain of application claims by appended claims and its Equivalent defines.

Claims (5)

  1. A kind of 1. method that sodium acetate is extracted from furfural production waste water, it is characterised in that be achieved by the steps of:
    (1)It is to add carbon in the furfural production waste water that 2.5 ~ 3%, pH value is 1 ~ 2.5 to the acetic acid content discharged by destilling tower bottom of towe Sour sodium is neutralized, then filtrate is delivered to preheater by regulation pH value to being filtered after 5.8 ~ 6.2,170 ~ 197 DEG C, Temperature raising preheats under the conditions of 0.8 ~ 1.2MPa, and it is that 1.06 ~ 1.15, flow is 6.5 ~ 7.0m that evaporation and concentration, which obtains relative density,3/ h's Half dope;
    (2)Half dope is drained to enrichment device and is further concentrated to give the dope that relative solubility is 1.25 ~ 1.30;
    (3)Add activated carbon into dope to be decolourized, filtered, the mass volume ratio of activated carbon and dope is 5.0 ~ 6.5kg/m3
    (4)Step will be passed through(3)The dope of processing is condensed to less than 70 DEG C, then the crystallisation by cooling at 40 DEG C, then through centrifugation point Sodium acetate is separated out, sodium acetate is packed after being down to room temperature, is put in storage.
  2. 2. the method for sodium acetate is extracted from furfural production waste water as claimed in claim 1, it is characterised in that:Step(1)In After preheating furfural production waste water by sent with slag boiler 200 ~ 210 DEG C, 1.2 ~ 1.3MPa primary steam with carrying out heat Exchange concentrate and obtain half dope, caused indirect steam is used to hydrolyze furfural dregs or condensation is back in furfural production waste water.
  3. 3. the method for sodium acetate is extracted from furfural production waste water as claimed in claim 1, it is characterised in that:Sodium carbonate and chaff The mass ratio of aldehyde waste water is 0.03 ~ 0.05.
  4. 4. the method for sodium acetate is extracted from furfural production waste water as claimed in claim 1, it is characterised in that:Destilling tower bottom of towe The acetic acid content of discharge is after the furfural production waste water that 2.5 ~ 3%, pH value is 1 ~ 2.5 first carries out oil removal precipitation, then adds thereto Sodium carbonate is neutralized.
  5. 5. the method for sodium acetate is extracted from furfural production waste water as claimed in claim 1, it is characterised in that:Step(4)In When centrifuging out sodium acetate, caused mother liquor is back to step(1)Furfural production waste water in.
CN201710821652.5A 2017-09-13 2017-09-13 Method for extracting sodium acetate from furfural production wastewater Active CN107602373B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109053416A (en) * 2018-08-30 2018-12-21 河北春蕾实业集团有限公司 Furfural exhaust gas produces sodium acetate new process
CN109354211A (en) * 2018-10-29 2019-02-19 侨昌现代农业有限公司 The method for preparing efficient carbon source sewage-treating agent needed for denitrifying microorganism with by-product sodium acetate
CN109724440A (en) * 2018-12-10 2019-05-07 安徽金禾实业股份有限公司 Total energy approach method and device in furfural production
CN117023917A (en) * 2023-10-10 2023-11-10 单县鲁顺糠醛有限公司 Furfural production wastewater comprehensive utilization treatment system of industrial Internet
CN118812347A (en) * 2024-07-17 2024-10-22 江苏赛德力制药机械制造有限公司 A sodium acetate salt recovery process

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101337953A (en) * 2008-08-14 2009-01-07 河南宏业化工有限公司 Method for producing furfural by cleaning hydrolysis of biomass
CN103043843A (en) * 2012-12-28 2013-04-17 山东金缘生物科技有限公司 Device and method for extracting sodium acetate from tower bottom wastewater of primary tower in furfural production
CN203144228U (en) * 2012-12-28 2013-08-21 山东金缘生物科技有限公司 Device for extracting sodium acetate from waste water at bottom of primary distillation tower during production of furaldehyde

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101337953A (en) * 2008-08-14 2009-01-07 河南宏业化工有限公司 Method for producing furfural by cleaning hydrolysis of biomass
CN103043843A (en) * 2012-12-28 2013-04-17 山东金缘生物科技有限公司 Device and method for extracting sodium acetate from tower bottom wastewater of primary tower in furfural production
CN203144228U (en) * 2012-12-28 2013-08-21 山东金缘生物科技有限公司 Device for extracting sodium acetate from waste water at bottom of primary distillation tower during production of furaldehyde

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109053416A (en) * 2018-08-30 2018-12-21 河北春蕾实业集团有限公司 Furfural exhaust gas produces sodium acetate new process
CN109354211A (en) * 2018-10-29 2019-02-19 侨昌现代农业有限公司 The method for preparing efficient carbon source sewage-treating agent needed for denitrifying microorganism with by-product sodium acetate
CN109724440A (en) * 2018-12-10 2019-05-07 安徽金禾实业股份有限公司 Total energy approach method and device in furfural production
CN117023917A (en) * 2023-10-10 2023-11-10 单县鲁顺糠醛有限公司 Furfural production wastewater comprehensive utilization treatment system of industrial Internet
CN117023917B (en) * 2023-10-10 2024-01-09 单县鲁顺糠醛有限公司 An industrial internet-based comprehensive utilization and treatment system for furfural production wastewater
CN118812347A (en) * 2024-07-17 2024-10-22 江苏赛德力制药机械制造有限公司 A sodium acetate salt recovery process
CN118812347B (en) * 2024-07-17 2025-03-18 江苏赛德力制药机械制造有限公司 A sodium acetate salt recovery process

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