US3645699A - Solid-liquid continuous countercurrent purifier method and apparatus - Google Patents

Solid-liquid continuous countercurrent purifier method and apparatus Download PDF

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US3645699A
US3645699A US858596A US3645699DA US3645699A US 3645699 A US3645699 A US 3645699A US 858596 A US858596 A US 858596A US 3645699D A US3645699D A US 3645699DA US 3645699 A US3645699 A US 3645699A
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recovery
zone
refining
liquid
section
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John Alfred Brodie
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Tsukishima Kikai Co Ltd
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Union Carbide Australia Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0004—Crystallisation cooling by heat exchange
    • B01D9/0013—Crystallisation cooling by heat exchange by indirect heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives
    • C07C17/392—Separation; Purification; Stabilisation; Use of additives by crystallisation; Purification or separation of the crystals
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/685—Processes comprising at least two steps in series
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/14—Purification; Separation; Use of additives by crystallisation; Purification or separation of the crystals

Definitions

  • ABSTRACT Assigneei Union Cirbide Australia Limited At least one component of a multicomponent molten mixture [22] Filed: Sept. 17, 1969 is separated from the mixture and purified by introducing the mixture into the recovery section of an array of apparatus 1 PP N05 358,596 comprising a recovery section, a refining section and a purifying section.
  • the recovery and purifying sections each have [30] Foreign Applicafion Priority Dam helical scraper-conveyors to move crystals through them, in-
  • SHEET 1 [IF 5 INVENTOR JOHN A. BROD/E W I I 4 ATTORNE PATENTEUFEB 29 I972 SHEET 2 BF 5 INVENTQR JOHN A. BROD/E 7 [4V ATTORNE% J BE- PAIENTEDFEB29 m2 3, 645.699
  • the present invention was made to provide a process and means to achieve separations of components from multicomponent mixtures through crystallization procedures.
  • the design and operating parameters are so related that they may be readily adapted to computerized control if desired, though it must be recognized that considerable change in certain design parameters of equipment will be necessary if there is a radical change in feed stocks or products. Where feed stocks suffer from minor fluctuations, operating parameters can be adjusted to achieve equilibrium operation; larger fluctuations may be dealt with by minor changes, such as alteration of point of feed stock entry, or the incorporation of comparatively simple surge absorbing zones. Gross changes will call for design variation, which however need not involve major rebuilding, as will become apparent hereafter in the discussion of forms of equipment that can be employed in practicing the invention.
  • Another advantage of the present invention lies in the fact that it allows a complete separation of one of the components of the feed stock, within the limits set by an eutectics, in one totally sealed continuous piece of equipment. This is of extreme importance where hazardous or toxic substances are involved.
  • While the invention is primarily described as separating mixtures of organic materials, it can be adapted to solutions wherein an equilibrium liquid phase is substituted by a saturated solution, 'which may include an aqueous solution of a substantially nonfusible inorganic salt.
  • a process and apparatus for the separation in very pure form of at least one component of a multicomponent mixture whereby the mixture is fed into a solid-liquid continuous countercurrent purifier, which includes of a purifying section, a refining section and a crystal-forming recovery section, all in series.
  • the mixture is fed into the recovery station at a point near the junction of the recovery section and the refining section.
  • a continuous downward temperature gradient is provided from the junction of the refining section with the purifying section to the end of the recovery section remote from the purifying section by continuous heat extraction throughout the length of said sections which are fitted with cooling jacket or the like means.
  • a liquid phase velocity at any point in a direction opposite to the direction of crystal movement is maintained which velocity is greater than the back mixing velocity of liquid at said point under the influence of agitation, crystal transport, and convection instability.
  • the crystal phase is maintained in suspension in the liquid phase in each section in a state intermediate between sedimentation and fiuidization by the control of agitating means and liquid flow velocity.
  • all such unscraped surfaces are provided with a sufficient small positive heat input.
  • the purifying section is operated under essentially adiabatic conditions modified only by a small heat input throughout its length to keepthe temperature of its wall and agitating means just above the crystallizing point of the liquid immediately adjacent thereto. Crystals are transferred slowly from the crystal forming recovery section through the refining section to the purifying section to maximize equilibrating crystal contact with the countercurrent flow of liquid and to cause adequate growth and purity of crystals finally fed into the purifying section.
  • the arrangement of a purifying section a refining section and a crystal forming recovery section in series, with a feed point near the junction of the refining section and the recovery section, a pure product output at the end of the purifying section remote from said feed point and a second product or mother liquor output at the end of the recovery section remote from said feed point represents a development of the center-fed type crystallization apparatus. Its construction and operation have distinct differences from known types end-fed crystallization apparatus which generally feature a crystal forming section and purifying section operating without the limitations and structures of the process of the present invention.
  • the endfed crystallization apparatus usually employ flash chillers to cool the mix introduced to the purifying section, said chillers having their coolant circulation so arranged that there exists an upward temperature gradient from the junction of the chiller with the purifying section to the feed point remote from the purifying section; that is, the end-fed crystal forming section operates with a low-temperature feed to the refining or purifying section.
  • the countercurrent purifier of this invention operates with a feed at a temperature practically identical to the temperature obtaining in the apparatus where it enters close to the junction of the refining and recovery sections, which temperature is intermediate of that of the low temperature liquid discharge from the remote end of the recovery section and the maximum temperature in the refining section where reflux liquid enters from the purifying section.
  • this downward temperature gradient through the length of the refining section when associated with the slow crystal transport and maximized equilibrating contact provided by the invention, means that crystals transported through the refining section pass in succession through a series of equilibrating stages characterized by increasing temperature: consequently the length of the refining and recovery sections and the temperature difference between their remote ends will determine the number of equivalent plates" available in these sections for the purification of a mixture in terms of a liquid-solid composition whose temperature and composition can be represented on an associated phase diagram.
  • the downward temperature gradient in the direction of liquid flow within the sections of the apparatus requires that the coolant circulation moves in a direction opposite to that of the flow of the liquid phase of the mix with the consequent benefit of enhanced thermodynamic efficiency.
  • One or more coolant circuits may be employed, according to required temperature and heat loads required. Separate control of the countercurrent coolant to the refining and recovery sections, for instance, makes it possible to attain preselected temperature gradients downwards from the end of the refining section contiguous to the purifying section and upwards from the remote or liquid discharge end of the recovery section so that the two gradients meet at the point of feed stock inlet to produce a temperature there equal to the crystallization point of the product of interest.
  • the liquid phase flow is in a direction opposite to that of crystal movement, and of a velocity that exceeds the back mixing velocity of the liquid under the influence of agitation, crystal transport and convection instability.
  • agitators or conveying means which operate at relatively high speeds. This causes turbulence and a back-mixing effect which tends to negate the progress in purification achieved in the crystal phase. Since the passage of the scraper-conveyor blades through the liquid crystal mixture inherently causes a certain amount of backmixing and, further, since there is always a tendency for a liquid to adhere in layer formation to crystals suspended in it, backmixing cannot be completely avoided.
  • a feed stock denuded of one component by crystallization and perhaps also affected by a temperature reduction, may have a higher density than the original or initially introduced form or a partially denuded form thereof.
  • Such more dense liquid may, in certain arrangements of apparatus, tend to graviate undesireably into zones holding comparative pure product.
  • the apparatus of the invention is therefore designed, fabricated and operated to insure that the desired liquid phase velocity can be maintained throughout the length of the refining section and the recovery section.
  • This is achieved by providing refining and recovery sections each having decreasing cross sectional areas in the direction of fluid flow.
  • Each such section may be made in tapered form or, alternatively of a series connected array of cylindrical elements each having a cross-sectional area smaller than the preceding element along the fluid flow direction.
  • the larger cross sectional areas in each of such sections are associated with relatively higher temperatures relatively larger liquid-crystal mix volumes while the smaller cross sectional areas are associated with relatively lower temperatures, and relatively smaller liquid-crystal mix volumes.
  • an agitator and/or scraper conveyor may in a given case operate at the slow speed of half a revolution per minute, which contrasts strongly with agitator speeds described in some of the prior art.
  • a significant integer of the invention is therefore the requirement that the operation shall allow, where necessary to prevent such crystal buildup, a small evenly distributed heat input to such unscraped surfaces. Electrical tracing with power led in through an agitator shaft is an effective means of achieving such heat input.
  • the present invention maintains a crystal bed in the purifying section in a state intermediate between sedimentation and fluidization, preferably allowing the crystal bed to form under gravity, and to reform after the small disturbance produced by a very slowly revolving agitating means and the countercurrent flow of liquid reflux.
  • the present invention further pro vides that the purifying section operates adiabatically, modified only by a small heat input at least to keep the temperature of the wall and agitating means above the crystallizing point of adjacent liquid. This includes compensation for heat lost by conductivity along the purifying section wall and agitating means.
  • a gravity-operated purifying section performs best with a comparatively large crystal size.
  • large crystals are not grown by shock cooling or steep temperature/time gradients.
  • a temperature/time gradient can be transformed into a temperature/length gradient.
  • crystals which form in the recovery section pass only slowly through it and the refining section. This insures that the crystals are subjected to a relatively small temperature/time gradient.
  • the recovery and refining sections are designed to be sufficiently long so that maximized equilibrating contact of crystal and liquid through these zones of relatively small temperature/time gradients is achieved. The consequent melting, recrystallization, remelting and further recrystallization steps then insure a feed of adequate crystal purity and size passing into the purifying section from the refining section.
  • the point of entry for the multicomponent feed stock is selected so that its entry into the system effects minimum thermodynamic disturbance. This involves a comparison of the composition-temperature conditions obtaining within the continuous countercurrent purifier, and the composition'temperature conditions in the feed stock when entering the purifier. Thermal stock'of the system by the entering feed stock will thus be minimized.
  • FIG. 1 is a partly sectionalized elevational view showing an apparatus arrangement which includes a recovery section, a refining section and a purifying section according to the invention.
  • FIG. 2 is a sectional view taken along the line 22 of FIG. 1, showing the interiors of the purifying section and the refining section at its junction with the purifying section.
  • FIG. 3 shows an alternative partially sectionalized arrangement of apparatus utilizing a multiplicity of cylindrical elements each to constitute the recovery and refining sections according to the invention.
  • FIG. 4 is a sectional view taken along the line 4-4 of FIG. 3 showing the interiors of two elements of the refining section of the apparatus of FIG. 3.
  • FIG. 5 is an elevational sectionalized view of an alternative arrangement of apparatus according to the invention involving a completely vertical disposition of the recovery, refining and purifying sections.
  • FIG. 6 is a schematic or block diagram illustrating a variation of apparatus elements according to the invention.
  • FIGS. 1 and 2 One arrangement of the equipment of this invention is illustrated in FIGS. 1 and 2.
  • a refining section 1 and a recovery section 2 arranged end to end on one substantially horizontal axis are coupled to a vertical purifying section 3.
  • Helical scraper-conveyors 4 and 5 are provided in the recovery section and refining section respectively, and slowly revolve to urge precipitated crystals towards the purifying section, while producing minimum back-mixing of liquid which moves in a direction countercurrent to the crystal progression from the purifying section 3 through the refining section 1, and, together with some feedstock from its admission point, through the recovery section 2.
  • Both the refining section 1 and the recovery section 2 are shown as uniformly tapered cylindrical vessels, but in altemative form they each may be built of a succession of cylindrical vessels of decreasing diameter as outlined at 6, 7, 8 and 9.
  • Cooling jackets l0 and 11 are provided for the refining section 1 and the recovery section 2, the coolant entering at 12 into the jacket 11, thereafter passing into jacket via the bridging connection 13, and leaving jacket 10 at 14.
  • the helical scraping-conveyors are mounted on a shaft 17 supported by bearings and 16, and articulated at 31, and provision is made to supply a small heat input to the shaft 17, the scraper-conveyor blades 4 and 5 and the spokes 18 to prevent crystal buildup on these unscraped surfaces.
  • the discontinuity in diameter which marks the junction 19 of the recovery section 2 and the refining section 1 is designed for maximum performance to be adjacent to the feed inlet point 20.
  • a liquid product is discharged at 21 at a relatively low temperature achieved in the operation of the equipment.
  • the apparatus is for a liquid feed stock, feed stocks which are themselves crystalline can be processed according to the invention.
  • the feed stock enters the apparatus at inlet point 20 on the recovery section. Should a crystal feed be used, the inlet point 20 would be located on the refining section I, again just adjacent the refining section/recovery section junction 19.
  • the purifying section 3 is contiguous to and connected with the larger end of the refining section 1.
  • a weir 22 which may be provided with means to adjust its height relative to the shaft 17 serves to retain in the refining section I a body of crystals which are'slowly transferred to the purifying section 3 as the scraper-conveyor 5, rotating clockwise as shown in FIG. 2, raises the crystals to the edge of weir 22, over which they fall into the purifying section 3.
  • the purifying section is fitted with a slowly rotating stirrer 23 mounted on a shaft 24 supported in bearings 26 and 27 carrying blades 25 which are designed to prevent agglomeration of the crystal bed forming in the body of the purifying section 3 while minimizing turbulence and back-mixing.
  • the insulated wall 28 incorporates heating means to provide a small heat input just sufficient to keep the wall temperature at each point above the melting point of the crystals accumulated adjacent thereto in effect compensating for the conduction of heat upward through the vessel wall toward the colder end 26 of the purifying section and offsetting heat losses through the outer insulation.
  • One or more inspection ports 32 are an advantage in the purifying section construction.
  • Heating means 29 are provided at the base of the purifying section 3 to provide the heat of fusion for the melting of the mass of crystals which continuously reach the base of the purifying section. A portion of the molten material can be withdrawn through an outlet 30, the balance of the molten material being displaced upward through the purifying section 3 by the descending mass of crystals of higher specific gravity.
  • the heat furnished by heating means 29 must be sufficient to melt the crystals adjacent thereto at the bottom of the purifying section and thus permit liquid product withdrawn through outlet 30 but must not be so great as to cause increase in the relative velocities of the descending crystals and/or the rising liquid reflux stream at any point in the purifier section.
  • This arrangement of the equipment operates in the following manner.
  • Coolant at an appropriate temperature and in appropriate quantity is caused to pass through the jacket system 12- l 1 13-10-14.
  • the multicomponent feedstock enters the recovery section 2 at the point 20, and under equilibrium conditions it is preferred that the feedstock temperature be at the crystallizing point if liquid or for a crystal feed at the melting point, which temperature in either case should closely approximate the temperature of the solid-liquid mixture within the apparatus adjacent to the feed inlet point 20. This provision will prevent partial melting of the already-formed crystals and avoid shock cooling and excessive fine nucleation at the point of feedstock entry.
  • the feedstock will tend initially to pass toward the end 15 of the recovery section, and because of the temperature gradient will deposit an increasing amount of solid crystal which will be conveyed toward the refining section, leaving a reduced amount of liquid to pass to the discharge point 21.
  • the refining section 1 receives the crystal deposited in the recovery section 2 by reason of the rotation of the scraperconveyor 4.
  • the refining section also receives a liquid component of high purity returning from the purifying section 3 over the weir 22.
  • the temperature gradient through the refining section from 19 to 16 causes the crystals being carried by the scraper-conveyor 5 to be subject to melting or partial melting; on the other hand, the same temperature gradient causes the liquid component returning from the purifying section 3 over the weir 22 into the refining section 1 to be subject to crystallization.
  • the temperature gradient of the refining section together with the reflux into the refining section from the purifying section combine to produce a quality gradient in the refining section.
  • FIGS. 3 and 4 As an alternative to the end-to-end arrangement of refining and recovery sections, a cascade arrangement is shown in FIGS. 3 and 4.
  • the succession of three jacketed cylinders la, lb and 1c of reducing diameters constitutes the refining section
  • the succession of three jacketed cylinders 2a, 2b and also of reducing diameters constitutes the recovery section.
  • FIG. 4 represents a cross section in the plane of the line 44 of FlG. 3 showing the connection between the cylinders lb and la.
  • a scraper-conveyor 43 lifts crystals from the cylinder lb over an adjustable weir 45, whence they fall downward into the cylinder la, to be conveyed by the scraper-conveyor 44 toward the purifying section 47.
  • An inspection port 46 is provided.
  • the feedstock 48 inlet is placed in proximity to the junction of the refining section 1c and the recovery section 2a.
  • the liquid discharge point 49 is provided at the end of the recovery section 2c.
  • the direction of coolant flow is from the entry point at 50 in the direction marked by the arrow connecting the jacket elements to the discharge point at 51.
  • a third arrangement is illustrated by reference to FIG. 5.
  • a refining section 61, a recovery section 62 and a purifying section 63 are assembled in line on a vertical axis.
  • the feedstock entry point is at 64
  • the liquid discharge point is at 66
  • the melted solid product discharge is at 67, below the heating element 68.
  • a modified scraper system 69, 70 is provided to maintain heat transfer through the walls of the recovery and refining sections.
  • a common shaft 71 driving the scrapers 69 and 70 and the agitator 73 is provided with articulating means at 72.
  • separate control of coolant flow temperature to the jackets of. the refining and recovery sections may be of advantage.
  • This vertical form of the equipment of this invention operates with a substantially continuous crystal bed extending from a level just above the heating element 68 in the purifying section upward through the refining section 61 and into the recovery section 62, the upper level of the crystal bed being a variable determined by variation of the heat input and heat removals, the upper level of the crystal bed being maintained between the sight glasses or other level detecting devices associated with the inspection ports 77 and 78.
  • the crystal mass reaching the base of the purifying section is melted by heating means provided within the base of the purifying section to allow withdrawal of part of the melt as product.
  • FIGS. 1, 3 and 5 show recovery sections and refining sections of approximately equal length, in practice this relation will be varied.
  • a feedstock rich in the desired higher melting component will in general require a shortened refining section and lengthened recovery section.
  • a feedstock poor in that material will require a shortened recovery section and a lengthened refining section.
  • a crystal feedstock may require a crystal-forming recovery section of minimum cross section.
  • the recovery section becomes shorter, until when said liquid component reaches eutectic composition the recovery section disappears to be replaced by some auxiliary crystal forming means.
  • An important feature of the invention is that it can accept a feed of any concentration within the limits set by the phase diagram, in liquid, crystal or slurry form, and can make a complete separation within the same limits.
  • FIG. 6 A variation applicable to any one of these three arrangements is illustrated by the block diagram of FIG. 6.
  • crystal is withdrawn through a rotary valve or equivalent 81 and passes to a separating device 82 serving to separate crystal 83 from adhering liquid 84.
  • the crystal mass is divided by a splitter 85 into crystal product 86 which is drawn off and a return fraction 87.
  • the return fraction 87 passes to a heat exchanger 88 with heat input means 89 and is thereby melted.
  • the resultant liquid together with the liquid stream 84, passes by a return line 90 into thebase of the purifying section where it is distributed by a ring jet or equivalent to become the reflux liquid stream passing up through the crystal mass in the purifying section in countercurrent.
  • EXAMPLE 1 An arrangement of the equipment of this invention in the form shown and described in relation to FIGS. 3 and 4 was used to prepare paradichlorobenzene from a feedstock consisting of mixed dichlorobenzenes containing 75 percent of the paraisomer.
  • the feed was run in at a rate of 60 gallons per hour, and the reflux/product ratio was maintained at 0.5: l.
  • a tails product containing 75 percent orthodichlorobenzene was withdrawn at a rate of 20 gallons per hour l5 gallons DCB and 5 gallons p DCB).
  • the retention time of crystals conveyed in the refining and recovery sections in countercurrent to the liquid was adjusted so that they increase in temperature at approximately the same rate of 3 C. per hour.
  • theutility heat required to effect the above almost complete separation within the limits set by the eutectic percent paradichlorobenzene and 85 percent orthodichlorobenzene) is that required to provide latent heat to melt the product and the reflux, where a molten product is taken off, and that required to melt the reflux only where the product is taken off in crystal form and also in both cases the sensible heat to raise the product temperature from feed temperature to that of the melting point of product material.
  • the heat removed by the coolant is the latent heat required to crystallize the product and the reflux, and to cool the outgoing cold end impurity stream from feed temperature to that of the outgoing stream.
  • Extra cooling is required for the removal of this additional heat. Extra heating and cooling is also required to offset normal heat losses or gains through external insulation. in a unit of the capacity indicated an efficiency exceeding 50 percent of the theoretical basis described above was obtained.
  • the power consumption in the apparatus is extremely low, the connected power being 1.5 hp. per million pound per annum of product including that required for the feed pump and the coolant circulating pump. This does not include power associated with the supply of refrigerant to cool the circulating coolant.
  • EXAMPLE 2 The plant employed in Example 1 was caused to operate under different rates of feed and product withdrawal.
  • Apparatus for the separation, purification and recovery of a at least one selected component of a multicomponent mixture of materials comprising, in combination,
  • first enclosure means defining a recovery zone having increasing cross sectional areas from a first end to a second end
  • second enclosure means defining a refining zone having increasing cross sectional areas from a first end which communicates with the second end of the enclosure means defining said recovery zone to a second end
  • third enclosure means defining a purifying zone having a first end communicating with the second end of the enclosure defining said refining zone and a second end,
  • stirrer means disposed substantially throughout the respective lengths of each of said enclosure means
  • inlet means for introducing a multicomponent mixture into the apparatus at a point adjacent the juncture of the second end of said first enclosure means and the first end of said second enclosure means
  • cooling means operably connected to said first and said second enclosure means adapted to provide a downward temperature gradient along the respective lengths thereof from each said respective second end thereof towards each said respective first'end thereof, and
  • stirrer means in the first enclosure means and the stirrer means in the second enclosure means are adapted to move crystals therein away from each of said respective first ends towards each of said respective second ends.
  • Apparatus according to claim 7 which includes crystalmovement-restra'ining weirs at the internal junctions between each element of said first enclosure means and said second enclosure means.
  • a process for the separation of at least onelco'mponent of a multicomponent mixture comprising:

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US858596A 1968-09-18 1969-09-17 Solid-liquid continuous countercurrent purifier method and apparatus Expired - Lifetime US3645699A (en)

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AU43524/68A AU416845B2 (en) 1968-09-18 1968-09-18 Solid-liquid continuous countercurrent purifier

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JP (1) JPS5434705B1 (de)
AT (1) AT324280B (de)
AU (1) AU416845B2 (de)
BE (1) BE739072A (de)
DE (1) DE1947251C3 (de)
FR (1) FR2018315A1 (de)
GB (1) GB1275798A (de)
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JPS53116340A (en) * 1977-03-15 1978-10-11 Wacker Chemie Gmbh Improved methoh of producing phthalic acid anhydride
US4235796A (en) * 1978-09-26 1980-11-25 Scm Corporation Process for fractional crystallization of lipids
US4296072A (en) * 1979-03-21 1981-10-20 Richter Gedeon Vegyeszeti Gyar Apparatus for the treatment of wet solids, especially pulpy materials, by heating or cooling
US4508553A (en) * 1980-07-24 1985-04-02 Douwe Egberts Koninklijke Tabaksfabriek-Koffiebranderijen-Theehandel N.V. Process for countercurrent crystallization with recirculation
US4597768A (en) * 1982-06-22 1986-07-01 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Method for treatment in counter current of suspended particles with a liquid
US20060013748A1 (en) * 2002-09-13 2006-01-19 Stefan Nordhoff Washing Apparatus, A Method Of Purifying A Wash Material And Use Of The Washing Apparatus
CN101400667B (zh) * 2006-03-20 2013-12-04 三菱化学株式会社 碳酸亚乙酯的纯化方法、纯化的碳酸亚乙酯的制造方法和碳酸亚乙酯
CN111905399A (zh) * 2020-08-31 2020-11-10 常熟龙飞医药设备科技有限公司 卧式双螺旋多级逆流结晶方法与装置
US20210394093A1 (en) * 2019-08-01 2021-12-23 Yanshan University Consumption-free high-efficiency filter
US20220001310A1 (en) * 2018-11-14 2022-01-06 Bollfilter Nordic Aps Filter candle and method for operating such filter candle
US20220339562A1 (en) * 2019-10-04 2022-10-27 Mimbly Ab Improved filter assembly with self-cleaning

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JPS5518521B2 (de) * 1974-02-19 1980-05-20
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JPS53116340A (en) * 1977-03-15 1978-10-11 Wacker Chemie Gmbh Improved methoh of producing phthalic acid anhydride
US4235796A (en) * 1978-09-26 1980-11-25 Scm Corporation Process for fractional crystallization of lipids
US4296072A (en) * 1979-03-21 1981-10-20 Richter Gedeon Vegyeszeti Gyar Apparatus for the treatment of wet solids, especially pulpy materials, by heating or cooling
US4508553A (en) * 1980-07-24 1985-04-02 Douwe Egberts Koninklijke Tabaksfabriek-Koffiebranderijen-Theehandel N.V. Process for countercurrent crystallization with recirculation
US4597768A (en) * 1982-06-22 1986-07-01 Nederlandse Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Method for treatment in counter current of suspended particles with a liquid
US4743434A (en) * 1982-06-22 1988-05-10 Nederlandsche Centrale Organisatie Voor Toegepast Natuurwetenschappelijk Onderzoek Apparatus for treatment of suspended particles with a liquid in countercurrent
US20060013748A1 (en) * 2002-09-13 2006-01-19 Stefan Nordhoff Washing Apparatus, A Method Of Purifying A Wash Material And Use Of The Washing Apparatus
US8252120B2 (en) 2002-09-13 2012-08-28 Evonik Stockhausen Gmbh Washing apparatus, a method of purifying a wash material and use of the washing apparatus
CN101400667B (zh) * 2006-03-20 2013-12-04 三菱化学株式会社 碳酸亚乙酯的纯化方法、纯化的碳酸亚乙酯的制造方法和碳酸亚乙酯
US20220001310A1 (en) * 2018-11-14 2022-01-06 Bollfilter Nordic Aps Filter candle and method for operating such filter candle
US11872507B2 (en) * 2018-11-14 2024-01-16 Bollfilter Nordic Aps Filter candle and method for operating such filter candle
US20210394093A1 (en) * 2019-08-01 2021-12-23 Yanshan University Consumption-free high-efficiency filter
US11845023B2 (en) * 2019-08-01 2023-12-19 Yanshan University Filter with passive-rotation filter flements
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US12208348B2 (en) * 2019-10-04 2025-01-28 Mimbly Ab Conical filter with turbine powered scraper
CN111905399A (zh) * 2020-08-31 2020-11-10 常熟龙飞医药设备科技有限公司 卧式双螺旋多级逆流结晶方法与装置
CN111905399B (zh) * 2020-08-31 2024-02-23 常熟龙飞医药设备科技有限公司 卧式双螺旋多级逆流结晶方法与装置

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AU4352468A (en) 1971-04-22
NL149384B (nl) 1976-05-17
DE1947251B2 (de) 1978-04-06
GB1275798A (en) 1972-05-24
SE368775B (de) 1974-07-22
FR2018315A1 (de) 1970-05-29
DE1947251A1 (de) 1970-05-06
AU416845B2 (en) 1971-08-27
AT324280B (de) 1975-08-25
BE739072A (de) 1970-03-02
NL6914190A (de) 1970-03-20
DE1947251C3 (de) 1978-12-07
JPS5434705B1 (de) 1979-10-29

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