CN1127671A - Process and apparatus for the recovery of water-immiscible solvents - Google Patents

Process and apparatus for the recovery of water-immiscible solvents Download PDF

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Publication number
CN1127671A
CN1127671A CN95115992.5A CN95115992A CN1127671A CN 1127671 A CN1127671 A CN 1127671A CN 95115992 A CN95115992 A CN 95115992A CN 1127671 A CN1127671 A CN 1127671A
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CN
China
Prior art keywords
water
solvent
proportion
outlet
phase boundary
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN95115992.5A
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Chinese (zh)
Inventor
H·斯特拉瑟
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Hoechst AG
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Hoechst AG
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Publication date
Application filed by Hoechst AG filed Critical Hoechst AG
Publication of CN1127671A publication Critical patent/CN1127671A/en
Pending legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/0208Separation of non-miscible liquids by sedimentation
    • B01D17/0211Separation of non-miscible liquids by sedimentation with baffles
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/24Treatment of polymer suspensions
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/02Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polymers & Plastics (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Removal Of Floating Material (AREA)
  • Physical Water Treatments (AREA)

Abstract

Recovery of a water-immiscible solvent, having a lower density than water is carried out in a separation tank. The separation tank has an outflow port for water determining the lower limit of a phase boundary, an introducing port provided at a position higher than the phase boundary, a partition arranged so that a liquid flows above and under the partition alternately and guiding liquid flow in the direction of the outflow port and an outflow port for the solvent determining the upper limit of the height of a liquid.

Description

The recovery method and the equipment of the solvent that can not mix with water
The present invention relates to from the mixture of organic solvent and water, reclaim its proportion organic solvent littler than the proportion of water.The invention particularly relates to the mixture that separates more such solvents and water, as the mixture that produces in the fluoropolymer granulation.
US-A4439385 has illustrated a kind of method of moulding powder of continuous preparation agglomeration, and this moulding powder is a kind of can not being made by melt processing, the first green powder of particulate tetrafluoroethylene polymer.Polymer is in the case at first through a pretreatment process, and then through an agglomeration processes, after this again through a postprocessing working procedures, then continuous blow-down goes out this polymer, and isolates the powder of this sintering from liquid medium with known method.Forms by water and a kind of organic liquid through this liquid medium of overall process, the wetting above-mentioned tetrafluoro ethylene polymer of this organic liquor physical efficiency, and in water maximum solvable 15 weight %, and keep certain weight or measurement (WM) ratio.Through after the postprocessing working procedures, answer continuous blow-down to go out and thisly be present in agglomerating powder in the liquid medium with suspended substance, and for the powder that makes this agglomeration with the main water yield with separate with a part of organic liquid and be added in the filter of a continuous operation.Such filter is deserved to reclaim employed this organic solvent as far as possible.But do not find more detailed description.
Known a kind of method and a kind of equipment from US-A3265769, this equipment also are used for agglomeration polytetrafluoroethylene (PTFE) moulding powder.The not only comparable water of employed organic solvent is light, and comparable water is heavy.Separate this organic solvent by aspirating with a water jet pump.The outlet of water jet pump reaches in the buffer container in the case.Under the represented in the drawings situation, this organic liquid deposits out as lower floor, and it is discharged by bottom valve, and water then flows out by a side exit.
Prove in practice: if realize bigger production capacity, so, it is very expensive reclaiming these organic liquids.Especially owing to filter and line clogging appear in the solid matter of bringing into, therefore need often to shut down and clean.
If produce big water gaging, this big water gaging contains quite a small amount of organic liquid, but also contains solid impurity, so, with organic liquid and moisture from significant difficulties is also arranged.Especially the solid matter that brings with the slurry form of exquisiteness is given to resemble and need can't harm being separated rapidly the lost territory recovery organic facies as far as possible and cause difficulty, because the wetability of the particle that is surrounded by solvent is poor, and these particles accumulate in the phase boundary scope.
Therefore existing of task is, with small charge from addition with big water gaging and may with recovery organic solvent that can not mix with water, that proportion is littler than the proportion of water as far as possible quantitatively the ORGANIC SOLVENT MIXTURES that solid impurity mixes.
The present invention solves this task like this: polluted solvent-aqueous mixtures below liquid surface, but on the phase boundary that produces, be directed to a container that injects water, and in this container, make polluted solvent-aqueous mixtures by be contained in below the dividing plate (bypass damper) of upper strata in mutually and above the one section enough distance of alternately turning back be separated.These dividing plates are fixed on the antetheca and rear wall of container.
What " be contained in upper strata mutually in " said is, all these dividing plates all the upper strata mutually in, but concerning the phase of separating, but in order to cause turning back that the solvent/water logistics exports from entering the mouth to, these dividing plates also alternately reach lower floor mutually in.What meet purpose is, only reaching the dividing plate of upper strata in mutually, partly to stretch into distance in the beginning of Disengagement zone longer, that is to say almost to reach phase boundary that stretch into distance with rear bulkhead with the Disengagement zone and shorten, in other words, the lower end of dividing plate is more and more far away from phase boundary always.That alternately install with the dividing plate of upper strata in mutually and reach the dividing plate of lower floor in mutually stretch into distance in whole Disengagement zone be same length all.Prolongation in mutually only extends to and guarantees have enough liquid stream to turn back on the one hand these dividing plates in lower floor, and enough liquid stream is arranged on the other hand, and last this liquid stream only is made up of the water that flows out.
As long as guaranteeing has enough liquid stream to turn back, dividing plate can be vertical, inclination or also can be crooked.The professional can be chosen in optimal in this case arrangement and configuration by means of simple trial test in case of necessity.
Equipment of the present invention is made up of the separating tank 1 of a band water out 2, a dividing plate 5 and solvent outlet 6 that flow towards outlet 2 at charging aperture 4 and some guided liquid-flows of the position that is higher than phase boundary 3, and wherein: overfall 2 is used for the position of definite phase boundary 3; Dividing plate 5 be installed into can make liquid stream on them and below alternately turn back; Outlet 6 is used for determining the position of liquid level 7.
Preferred arrangement of the present invention is described in more detail below.
Advantageously provide charging aperture 8 again, in order that water is sent in the equipment on demand, even, also can keep liquid level constant so that when in pipeline 4, compression shock occurring.
Suitable in addition is, this equipment also has a bottom outlet 9, and this outlet 9 is equipped with a dump valve 10, so that give off the slurry of deposition serially or off and on.
Favourable arrangement of the present invention is: by a suitable device, but advantageously by one in height the pipe 11 of appropriate change isolate, for example aspirate out accumulate in phase boundary 3 scope in solid phase components.Therefore obtain the fine component that the form with a kind of easy processing exists.
The size of equipment determines, especially the length of the arrangement of dividing plate 5 and quantity and the solvent streams that therefore causes depends on the density contrast between solvent and the water and depends on the solvent purity of requirement.The professional also can do some simple trial test here in case of necessity.
The selection of material is depended on the solvent types that will separate He will purify and is depended on possible impurity.If the first dispersion liquid of fluoropolymer for example also contains low amount of fluorinated hydrogen, the plastics that then can select a kind of resistance are as the material of this equipment or as the lining material of this equipment.
Therefore the present invention has avoided because all problems that the impurity of bringing into causes.Because no longer need to stop up easily and require the ultrafilter of corresponding high power pump, so can avoid a considerable investment and operating cost.Can simplify separation in addition greatly to the valuable substance of bringing into.
The present invention can be from a large amount of water not only but also than isolating the solvent that can not mix with water, proportion is littler than the proportion of water continuously entirely the mixture of small amount of water, so efficient is very high.Because the outlet of solvent and water separates, under any circumstance, the throughput of solvent and water all may be higher.Because two outlets all are arranged in the end of common turn back distance and Disengagement zone, the refining effect that separates a kind of solvent of common generation of the solid matter on this arrangement and the phase boundary.
The following examples illustrate in greater detail the present invention.
Embodiment
Being that the mixture input formed of 80-110 ℃ 1 parts by volume gasoline and 14 parts by volume water is by in the equipment shown in Figure 1 by boiling point.This water is to produce in the granulation according to the embodiment 1 described polytetrafluoroethylene (PTFE) of US-A4439385.This liquid mixture contains small amount of polymer and solid impurity.Do not contain solid matter from exporting the gasoline that obtains 6, only contain about 0.05 volume % water.
Solid impurity accumulates in the bottom of this container, but not timing ground is separated by bottom outlet 9.By the accumulation of polymer carried secretly on phase boundary 3, but not timing ground pumps out this polymer by managing 11.The separable about 8 kilograms of solid matters of the per 10000 liters of liquid mixtures that passed through, and can be processed into polytetrafluoroethylene (PTFE).

Claims (5)

1. from the mixture of solvent and water, reclaim the method for its proportion than the proportion solvent little, that can not mix with water of water, it is characterized in that: may polluted solvent-aqueous mixtures below the liquid surface of a container that has injected water but on phase boundary, be directed to this container, and in this container, make polluted solvent-aqueous mixtures by be contained in below the dividing plate of upper strata in mutually and above the one section enough distance of alternately turning back be separated.
2. be used for from solvent-water mixes, reclaiming the equipment of solvent that can not mix with water, that its proportion is littler than the proportion of water, it is characterized in that: this equipment is by a separating tank (1) with a water out (2), this outlet (2) limits phase boundary (3), one to be formed towards a dividing plate (5) and a solvent outlet (6) that outlet (2) direction flows at charging aperture (4) and some guided liquid-flows of the position that is higher than phase boundary (3), wherein: dividing plate (5) be installed into can make liquid stream on them and below alternately turn back; Outlet (6) is used for determining the position of liquid level (7).
3. by the described equipment of claim 2, it is characterized in that: another charging aperture (8) also is provided, this charging aperture (8) be contained in charging aperture (4) below.
4. by claim 2 or 3 described equipment, it is characterized in that: be equipped with a bottom outlet (9) and/or a pipe (11) with a dump valve (10) maybe can be installed, its mounting means can make that solid matter is separated in phase boundary (3) scope to be fallen.
5. by the application of claim 2,3 or 4 described equipment, be used for reclaiming solvent that can not mix with water, that its proportion is littler than the proportion of water in the mixture of the water from solvent and fluoropolymer granulation.
CN95115992.5A 1994-10-22 1995-10-19 Process and apparatus for the recovery of water-immiscible solvents Pending CN1127671A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE4437837A DE4437837A1 (en) 1994-10-22 1994-10-22 Recovering low density, water-immiscible solvent
DEP4437837.8 1994-10-22

Publications (1)

Publication Number Publication Date
CN1127671A true CN1127671A (en) 1996-07-31

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ID=6531475

Family Applications (1)

Application Number Title Priority Date Filing Date
CN95115992.5A Pending CN1127671A (en) 1994-10-22 1995-10-19 Process and apparatus for the recovery of water-immiscible solvents

Country Status (5)

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JP (1) JPH08206406A (en)
CN (1) CN1127671A (en)
DE (1) DE4437837A1 (en)
IT (1) IT1276961B1 (en)
NL (1) NL1001469C2 (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474494A (en) * 2008-01-04 2009-07-08 靖江市华通机电设备制造有限公司 Copper extractive agent water diversion system
CN101856569A (en) * 2009-11-20 2010-10-13 山东金正大生态工程股份有限公司 Solvent purifying device in controlled release fertilizer production
CN103357197A (en) * 2013-07-01 2013-10-23 内乡县乌克生物化学制品有限公司 Equipment for continuously and automatically separating mutually insoluble liquid mixture

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998049101A1 (en) * 1997-04-24 1998-11-05 Unisearch Limited Oil from water separator
WO2001076716A1 (en) * 2000-04-06 2001-10-18 Lisopharm Ag Method and apparatus for separation of a mixture of non-miscible liquids

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR328403A (en) * 1903-01-10 1903-07-10 Frederic Moore Oil and grease separator
US1116903A (en) * 1913-03-25 1914-11-10 William Mcclintock Oil-separator.
US3278041A (en) * 1962-08-06 1966-10-11 Phillips Petroleum Co Apparatus for separating threephase dispersions
DE3905864A1 (en) * 1988-03-03 1990-08-30 Dieter Braeuer DEVICE FOR WASTE WATER DISPOSAL
DE3841198A1 (en) * 1988-12-07 1990-06-13 Ossenkop Maschinenbau Apparatus for oil separation
JP3405750B2 (en) * 1992-12-02 2003-05-12 日本電産株式会社 Spindle motor

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474494A (en) * 2008-01-04 2009-07-08 靖江市华通机电设备制造有限公司 Copper extractive agent water diversion system
CN101856569A (en) * 2009-11-20 2010-10-13 山东金正大生态工程股份有限公司 Solvent purifying device in controlled release fertilizer production
CN101856569B (en) * 2009-11-20 2012-09-05 山东金正大生态工程股份有限公司 Solvent purifying device in controlled release fertilizer production
CN103357197A (en) * 2013-07-01 2013-10-23 内乡县乌克生物化学制品有限公司 Equipment for continuously and automatically separating mutually insoluble liquid mixture
CN103357197B (en) * 2013-07-01 2015-03-25 内乡县乌克生物化学制品有限公司 Equipment for continuously and automatically separating mutually insoluble liquid mixture

Also Published As

Publication number Publication date
ITMI952149A0 (en) 1995-10-19
DE4437837A1 (en) 1996-04-25
NL1001469C2 (en) 1998-07-15
IT1276961B1 (en) 1997-11-03
JPH08206406A (en) 1996-08-13
ITMI952149A1 (en) 1997-04-19
NL1001469A1 (en) 1996-04-22

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