CN105732422A - Method for utilizing microchannel for extracting diacetylmonoxime in ammonium sulfate water solution - Google Patents
Method for utilizing microchannel for extracting diacetylmonoxime in ammonium sulfate water solution Download PDFInfo
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- CN105732422A CN105732422A CN201610237495.9A CN201610237495A CN105732422A CN 105732422 A CN105732422 A CN 105732422A CN 201610237495 A CN201610237495 A CN 201610237495A CN 105732422 A CN105732422 A CN 105732422A
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- diacetylmonoxime
- ionic liquid
- ammonium sulfate
- microchannel
- phase
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- FSEUPUDHEBLWJY-HWKANZROSA-N diacetylmonoxime Chemical compound CC(=O)C(\C)=N\O FSEUPUDHEBLWJY-HWKANZROSA-N 0.000 title claims abstract description 76
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910052921 ammonium sulfate Inorganic materials 0.000 title claims abstract description 37
- 235000011130 ammonium sulphate Nutrition 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 22
- 239000002608 ionic liquid Substances 0.000 claims abstract description 58
- 239000012071 phase Substances 0.000 claims abstract description 42
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000012546 transfer Methods 0.000 claims abstract description 19
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008346 aqueous phase Substances 0.000 claims description 41
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 102000029749 Microtubule Human genes 0.000 abstract 1
- 108091022875 Microtubule Proteins 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 210000004688 microtubule Anatomy 0.000 abstract 1
- 108091006146 Channels Proteins 0.000 description 36
- 239000007864 aqueous solution Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 11
- 238000002798 spectrophotometry method Methods 0.000 description 11
- 102000010637 Aquaporins Human genes 0.000 description 10
- 108010063290 Aquaporins Proteins 0.000 description 10
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 10
- 238000007865 diluting Methods 0.000 description 10
- 238000002347 injection Methods 0.000 description 10
- 239000007924 injection Substances 0.000 description 10
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 description 2
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- WHIVNJATOVLWBW-SNAWJCMRSA-N methylethyl ketone oxime Chemical compound CC\C(C)=N\O WHIVNJATOVLWBW-SNAWJCMRSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- ODUCDPQEXGNKDN-UHFFFAOYSA-N nitroxyl Chemical group O=N ODUCDPQEXGNKDN-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C249/00—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton
- C07C249/04—Preparation of compounds containing nitrogen atoms doubly-bound to a carbon skeleton of oximes
- C07C249/14—Separation; Purification; Stabilisation; Use of additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a method for utilizing a microchannel for extracting diacetylmonoxime in an ammonium sulfate water solution.The method comprises the following steps that 1, an ammonium sulfate water solution containing diacetylmonoxime is used as a water phase, ionic liquid [BMIM]PF6 is adopted as an extracting agent, the water phase and the ionic liquid phase are injected into the microtubule channel through two flow pumps, the flow of the water phase is 0.25-19.8 mL/min, the flow of the ionic liquid phase is 0.25-1.32 mL/min, the extraction temperature is 20 DEG C, and the standing time of the two phases inside the microchannel is 1-48 s; 2, the two phases flow out of the microchannel after mass transferring is performed, products are collected at an outlet, standing and phase splitting are performed, and diacetylmonoxime is extracted from the water phase to the ionic liquid phase, wherein the inner diameter of the microchannel is 0.5-1 mm, the outer diameter of the microchannel is 1.50 mm, and the length is 1 m; the content of diacetylmonoxime in the ammonium sulfate water solution containing the diacetylmonoxime is 1000-10000 ppm, and the concentration of ammonium sulfate is lower than 40 wt%.The microchannel is adopted for extracting the diacetylmonoxime in the ammonium sulfate water solution, the method has the advantages of being rapid in mass transfer, small in size, easy to integrate and magnify and the like, defects of a traditional extraction device are overcome, and the extraction efficiency is improved.
Description
Technical field
The present invention relates to canalicular channel abstraction technique field, particularly relate to one and utilize microchannel to extract sulphuric acid
The method of diacetylmonoxime in aqueous ammonium.
Technical background
2-butanone oxime (hereinafter referred to as diacetylmonoxime) is widely used in polyurethane closed agent as antioxidant, and boiler removes
Oxygen agent, coating, paint, ink anti skinning agent in, it is possible in the organic synthesis as silicone rubber kinds sealant
Mesosome.At present, the method for domestic production diacetylmonoxime is ketoamine method, and this method can contain diacetylmonoxime by by-product
(1000-10000ppm) ammonium sulfate solution.Owing to during ammonium sulfate crystallization, the diacetylmonoxime of discharge can dirt
Dye environment, is also unfavorable for the recycling of post-crystallization processes waste water, therefore in ammonium sulfate solution simultaneously
Diacetylmonoxime should separate and recover.The research of applicant place seminar shows hydrophobic ionic liquid
[BMIM]PF6Good effect (publication number is had in terms of diacetylmonoxime in extraction and recovery ammonium sulfate solution
CN103588675A, entitled utilizes ionic liquid [BMIM] PF6The method of diacetylmonoxime in extraction ammonium sulfate
Patent of invention), conventional organic solvents used in technique before comparing, the most green, safe and energy-conservation.
And in traditional extraction process, use the equipment such as mixer-settler, extraction tower more, generally there is efficiency
The shortcoming such as low, equipment volume is big, operation and maintenance costs is high.Therefore, for butanone in ammonium sulfate solution
The extraction of oxime, develops new efficient extraction and separation technology and equipment is significant.
Micro-chemical system is the miniaturization chemical system utilizing micro Process and precision processing technology to manufacture, its feature
It is that " transport " process occurs to be in nanoscale in micron-sized short space at characteristic dimension.Micro-logical
Road is basic composition unit and the key components of micro-chemical system, and compared with legacy equipment, microchannel has
Have that specific surface area is big, mass-and heat-transfer fast, consumption is few, security performance is high, volume is little in reaction, be easily integrated with
The advantages such as amplification, are with a wide range of applications in fields such as chemistry, chemical industry, biology, medical science, the energy.
At present, existing correlational study and the application in terms of the extract and separate in microchannel, but specific to ion
Liquid [BMIM] PF6In extraction diacetylmonoxime production process, the diacetylmonoxime in the ammonium sulfate of by-product yet there are no report
Road.
Summary of the invention
The efficiency that it is an object of the invention to overcome traditional extraction equipment to exist is low, volume big, Operation and maintenance
The shortcomings such as expense is high, it is provided that a kind of utilize the method for diacetylmonoxime in canalicular channel extraction ammonium sulfate solution.
The method of diacetylmonoxime in microchannel extraction ammonium sulfate solution is utilized to comprise the steps:
(1) using the ammonium sulfate solution containing diacetylmonoxime as aqueous phase, ionic liquid [BMIM] PF6As extractant,
Aqueous phase and ionic liquid are injected in microchannel apparatus by two flow pumps the most respectively, and aqueous phase flow is
0.25-19.8mL/min, ionic liquid phase flow rate is 0.25-1.32mL/min, and extraction temperature is 20 DEG C, two
The time of staying in microchannel apparatus is 1-48s；
(2) biphase carry out flowing out after mass transfer microchannel apparatus, collect product in exit, stand split-phase, fourth
Ketoxime be extracted to from aqueous phase ionic liquid mutually in.
Method the most according to claim 1, it is characterised in that described microchannel apparatus includes microring array
Device and canalicular channel, after fluid mixes in micro-mixer, carry out mass transfer in canalicular channel, and described is micro-
The internal diameter of tube passage is 0.5-1mm, and external diameter is 1.50mm, a length of 1m, and micro-mixer is T-shaped threeway,
Aperture is 0.5-1mm, and the diacetylmonoxime content in the ammonium sulfate containing diacetylmonoxime is 1000-10000ppm, sulfur
Acid ammonium concentration is less than 40wt%.
Compared with existing traditional extraction equipment extracting process, the innovative point of the present invention is to utilize canalicular channel
Diacetylmonoxime in extraction ammonium sulfate solution, the method has that specific surface area is big, mass transfer is fast, volume is little, easy
In integrated with amplification etc. advantage.
Detailed description of the invention
The method of diacetylmonoxime in microchannel extraction ammonium sulfate solution is utilized to comprise the steps:
(1) using the ammonium sulfate solution containing diacetylmonoxime as aqueous phase, ionic liquid [BMIM] PF6As extractant,
Aqueous phase and ionic liquid are injected in microchannel apparatus by two flow pumps the most respectively, and aqueous phase flow is
0.25-19.8mL/min, ionic liquid phase flow rate is 0.25-1.32mL/min, and extraction temperature is 20 DEG C, two
The time of staying in microchannel apparatus is 1-48s；
(2) biphase carry out flowing out after mass transfer microchannel apparatus, collect product in exit, stand split-phase, fourth
Ketoxime be extracted to from aqueous phase ionic liquid mutually in.
Described microchannel apparatus includes micro-mixer and canalicular channel, after fluid mixes in micro-mixer,
Carrying out mass transfer in canalicular channel, the internal diameter of described canalicular channel is 0.5-1mm, and external diameter is 1.50mm,
A length of 1m, micro-mixer is T-shaped threeway, and aperture is 0.5-1mm, in the ammonium sulfate containing diacetylmonoxime
Diacetylmonoxime content be 1000-10000ppm, ammonium sulfate concentrations be less than 40wt%.
Beneficial effects of the present invention: what the present invention provided utilizes ion liquid abstraction ammonium sulfate in canalicular channel
The method of the diacetylmonoxime in aqueous solution, extraction efficiency is high, substantially reduces extraction and reaches the time of balance, from
The dozens of minutes of traditional extraction mode shortens to second level scope.
The present invention by water by Spectrophotometry mutually in diacetylmonoxime concentration, analysis principle is: diacetylmonoxime exists
Hydrolyzed under acidic conditions, generates butanone and azanol, and under conditions of adding Ammonium persulfate., azanol is anti-with formaldehyde
Should generate formyl hydroxamic acid, formyl hydroxamic acid can generate red complex with ferric ion, uses UV, visible light
The absorbance of this complex of spectrophotometer measurement i.e. can get the concentration of diacetylmonoxime in aqueous phase.
Present invention following example are described further, but are not limited to following example, without departing from front
In the range of rear described objective, change is included in the technical scope of the present invention.
Embodiment 1
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 0wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.735mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.75mm is biphase
The time of staying is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 32.7%.
Embodiment 2
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.735mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.75mm is biphase
The time of staying is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 66.5%.
Embodiment 3
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 40wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.735mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.75mm is biphase
The time of staying is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 86.0%.
Embodiment 4
Be 1g/L (1000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.735mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.75mm is biphase
The time of staying is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 62.9%.
Embodiment 5
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Phase flow rate is set to 0.25mL/min, and ionic liquid phase flow rate is set to 1.25mL/min, and the time of staying is
17.7s, two pipelines connect with three way cock, and biphase mixed at three way cock to be incorporated in follow-up 1m length micro-
Carrying out mass transfer, canalicular channel internal diameter 0.75mm in tube passage, the biphase time of staying is 18s, and temperature control is
20℃.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase, and lower floor is ionic liquid phase.Take upper water
Phase, by the concentration of spectrophotometric analysis diacetylmonoxime contained therein after diluting with deionized water, then further according to
The conservation of mass of total system diacetylmonoxime, can calculate the concentration of ionic liquid middle diacetylmonoxime mutually.Thus can count
Calculating extraction yield is 65.0%.
Embodiment 6
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Phase flow rate is set to 1.25mL/min, and ionic liquid phase flow rate is set to 0.25mL/min, and the time of staying is
17.7s, two pipelines connect with three way cock, and biphase mixed at three way cock to be incorporated in follow-up 1m length micro-
Carrying out mass transfer, canalicular channel internal diameter 0.75mm in tube passage, the biphase time of staying is 18s, and temperature control is
20℃.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase, and lower floor is ionic liquid phase.Take upper water
Phase, by the concentration of spectrophotometric analysis diacetylmonoxime contained therein after diluting with deionized water, then further according to
The conservation of mass of total system diacetylmonoxime, can calculate the concentration of ionic liquid middle diacetylmonoxime mutually.Thus can count
Calculating extraction yield is 35.5%.
Embodiment 7
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.325mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.5mm is biphase
The time of staying is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 71.4%.
Embodiment 8
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 1.305mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, canalicular channel internal diameter 1mm, biphase stops
Staying the time is 18s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase, under
Layer is ionic liquid phase.Take upper strata aqueous phase, contained therein with spectrophotometric analysis after diluting with deionized water
The concentration of diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid phase
The concentration of middle diacetylmonoxime.Thus can calculate extraction yield is 59.4%.
Embodiment 9
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Being 0.275mL/min with ionic liquid phase flow rate mutually, two pipelines connect with three way cock, biphase in threeway
Joint is mixed to be incorporated in the long canalicular channel of follow-up 1m and is carried out mass transfer, and canalicular channel internal diameter 0.75mm is biphase
The time of staying is 48s, and it is 20 DEG C that temperature controls.Collecting and flow out the biphase of canalicular channel, upper strata is aqueous phase,
Lower floor is ionic liquid phase.Take upper strata aqueous phase, with spectrophotometric analysis wherein institute after diluting with deionized water
Concentration containing diacetylmonoxime, then further according to the conservation of mass of total system diacetylmonoxime, can calculate ionic liquid
The concentration of mutually middle diacetylmonoxime.Thus can calculate extraction yield is 73.2%.
Embodiment 10
Be 10g/L (10000ppm) using diacetylmonoxime concentration, ammonium sulfate concentrations be the aqueous solution of 20wt% as aqueous phase,
Ionic liquid [BMIM] PF6As extractant, respectively by two flow pumps by biphase injection canalicular channel, water
Phase flow rate is set to 19.8mL/min, and ionic liquid phase flow rate is set to 1.32mL/min, and two pipelines are with three
Pass joint connects, biphase at three way cock mixed being incorporated in the long canalicular channel of follow-up 1m carry out mass transfer, micro-
Tube passage internal diameter 0.75mm, the biphase time of staying is 1s, and it is 20 DEG C that temperature controls.Collect and flow out canalicular channel
Biphase, upper strata is aqueous phase, and lower floor is ionic liquid phase.Take upper strata aqueous phase, use after diluting with deionized water
The concentration of spectrophotometric analysis diacetylmonoxime contained therein, then further according to the conservation of mass of total system diacetylmonoxime,
The concentration of ionic liquid middle diacetylmonoxime mutually can be calculated.Thus can calculate extraction yield is 13.9%.
Claims (2)
1. utilize the method for diacetylmonoxime in microchannel extraction ammonium sulfate solution, it is characterised in that include walking as follows
Rapid:
(1) using the ammonium sulfate solution containing diacetylmonoxime as aqueous phase, ionic liquid [BMIM] PF6As extractant,
Aqueous phase and ionic liquid are injected in microchannel apparatus by two flow pumps the most respectively, and aqueous phase flow is
0.25-19.8mL/min, ionic liquid phase flow rate is 0.25-1.32mL/min, and extraction temperature is 20 DEG C, two
The time of staying in microchannel apparatus is 1-48s；
(2) biphase carry out flowing out after mass transfer microchannel apparatus, collect product in exit, stand split-phase, fourth
Ketoxime be extracted to from aqueous phase ionic liquid mutually in.
Method the most according to claim 1, it is characterised in that described microchannel apparatus includes microring array
Device and canalicular channel, after fluid mixes in micro-mixer, carry out mass transfer in canalicular channel, and described is micro-
The internal diameter of tube passage is 0.5-1mm, and external diameter is 1.50mm, a length of 1m, and micro-mixer is T-shaped threeway,
Aperture is 0.5-1mm, and the diacetylmonoxime content in the ammonium sulfate containing diacetylmonoxime is 1000-10000ppm, sulfur
Acid ammonium concentration is less than 40wt%.
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| CN201610237495.9A CN105732422B (en) | 2016-04-15 | 2016-04-15 | The method that diacetylmonoxime in ammonium sulfate solution is extracted using microchannel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106214838A (en) * | 2016-07-20 | 2016-12-14 | 南京工业大学 | A kind of method utilizing microchannel extraction equipment to reclaim total flavonoids extract from vegetable polysaccharides Aqueous extracts |
| CN110711524A (en) * | 2019-11-29 | 2020-01-21 | 福州大学 | Micro-fluidic device for measuring liquid-liquid phase balance |
| CN111116410A (en) * | 2020-01-12 | 2020-05-08 | 浙江锦华新材料股份有限公司 | Preparation method of butanone oxime |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570582A (en) * | 2013-10-28 | 2014-02-12 | 中建安装工程有限公司 | Method for extracting diacetylmonoxime in ammonium sulfate solution by using ionic liquid [BMIM]NTf2 |
| CN103588675A (en) * | 2013-10-28 | 2014-02-19 | 中建安装工程有限公司 | Method for extracting butanone oxime from solution by utilizing ionic liquid [BMIM]PF6 |
| CN105112658A (en) * | 2015-08-28 | 2015-12-02 | 昆明理工大学 | Method for extracting rare-earth elements through micro channels |
-
2016
- 2016-04-15 CN CN201610237495.9A patent/CN105732422B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103570582A (en) * | 2013-10-28 | 2014-02-12 | 中建安装工程有限公司 | Method for extracting diacetylmonoxime in ammonium sulfate solution by using ionic liquid [BMIM]NTf2 |
| CN103588675A (en) * | 2013-10-28 | 2014-02-19 | 中建安装工程有限公司 | Method for extracting butanone oxime from solution by utilizing ionic liquid [BMIM]PF6 |
| CN105112658A (en) * | 2015-08-28 | 2015-12-02 | 昆明理工大学 | Method for extracting rare-earth elements through micro channels |
Non-Patent Citations (3)
| Title |
|---|
| W.埃尔菲尔德: "《微反应器 现代化学中的新技术》", 31 October 2004 * |
| 唐静等: "微通道内液-液两相流研究进展", 《化工进展》 * |
| 王丽军: "T形微通道结构中液液两相流动与传质规律", 《化工学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106214838A (en) * | 2016-07-20 | 2016-12-14 | 南京工业大学 | A kind of method utilizing microchannel extraction equipment to reclaim total flavonoids extract from vegetable polysaccharides Aqueous extracts |
| CN106214838B (en) * | 2016-07-20 | 2020-04-07 | 南京工业大学 | Method for recovering total flavone extract from plant polysaccharide water extract by using microchannel extraction device |
| CN110711524A (en) * | 2019-11-29 | 2020-01-21 | 福州大学 | Micro-fluidic device for measuring liquid-liquid phase balance |
| CN111116410A (en) * | 2020-01-12 | 2020-05-08 | 浙江锦华新材料股份有限公司 | Preparation method of butanone oxime |
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