DE1519819A1 - Crystallization process - Google Patents

Description

PATENT LAWYERS. .4P ₁ QQ ₁ Q

DR.-ING. H. FINCKE IO ΙϋΟ Ιί3 ₉ Munich s,

DtPL.-ING. H. BOHR Mütlerstrasse 31: ZQl.

DIPL.-ING. S. STAEGER

Telephone: 22 49 41

Bite; 20640
Case: H "18547

description eum patent grant

IMPBRIAI. CHBMICAIi INDUSTRIES LtMIaJBD _n London ₀ 3oW “1

concerning;

¹¹ Crystalization Proceedings "Priority! July 20, 1965 and July 11, 1966, Great Britain

The invention relates to crystallization processes

Yorgesohlagen was already used in the separation of a crystalline egg and arene component from a coating material by means of vigorous cooling of the same, whereby a slurry is obtained from the component and its mother liquor and then the slurry is filtered to separate the component ₀ a pulsating pressure on the treated material to exercise j to facilitate the movement of the slurry through apparatus as "and to control the filtration"

SO 981 1/1133

The invention spoils a crystallization process in which the öröasa of the crystals obtained increases and thus facilitates dia! Filtration of the slurry becomes «while allowing a resonance and the formation of standing pressure waves in the treated material, so that efficient movement of the slurry is allowed

Invention game 33 is an apparatus for the separation of a crystallizable component from a loading material created by strong cooling »the off

a) a check valve through which the feed material can be introduced,

b} a cooling or quenching device for the seehlaking material coming out of the specified valve to form a slurry ₀

ο) a device for recycling the feed material -ffη the outlet end of the cooling device ssu its BinXaBOGiFJör which consists of at least one tube and _{impeller 9} the sum drive of the recycled material

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the pipe suitable 1st- _s composed, wherein in di <a * AFES; The distance traveled by the reocyclized booohiocing material is approximately the same as the distance that the booing material takes

80S8 11/113 3 bath original

■ = 5

on its way from the point at which it recycles is "up to the point" from which it is recycled is put back o

d) a filtration device o which the one in the abbreviation = processing device to form, a slurry cooled feed material is fed, and

e) a device for applying a pulsating pressure to the treated material _p are able _c iet a pulsating pressure having a frequency to generate? which enables a resonance and the formation of standing waves in the treated material between the gate direction generating a pulsating pressure and the check valve _r consists o.

The apparatus can be used to carry out a method be, in which a crystallizable component from a »; Charge material, separated by rapid cooling; this process consists in that the feed material through a check valve of a cooling device; added ~ leads to "in which that material is strongly cooled to form a slurry?" a portion of the feed material from the outlet end of the cooler to its Entrance end is guided »with the distance covered being in« ner length equal to that in the cooling device eurüokleger The first distance is »the mother liquor is removed from the slurry-

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separately _f a pulsating pressure is exerted on the material to be treated with a frequency that Keaonarus and the formation of standing pressure waves in the material but the result «and the crystal!

You cooling device can, for example, from one or consisting of several surface heaters provided with scraping devices in a conventional manner

The device for recycling the polluting material from the outlet end of the cooling device eu its inlet end may optionally contain one or more valves «

The filter should preferably consist of a permeable tube through which the crystals can exit in an axial manner; the pulsating pressure-generating device oolite must be attached to the side of the filter opposite the check valve. It is normally surrounded by a metal braid. It is also preferable that the crystals, after passing through a filter described above, pass through a reflux zone in which they are washed with a liquid of molten crystals until they reach a level of heating. n _f in which they themselves are geaohmoleen, where dit get * liquid represents the purified product. • ttllt *

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This part de.;? Apparatus can .therefore consist of a vertical pipe, through which the initial threading is descending. Righteousness is directed? The upper part of the tube is made of a perforated point "to allow the exit""o" liquid "while oils crystals remain in the tube, a heating device in the lower part of the tube and a pulsating bridge "When the process is carried out, a large rope of the mother liquor of the slurry passes the filter walls; a molten liquid from below the heater is periodically propelled forward through the pulsation device", flowing past the heating device and the crystals wäsoh.t the filter and the Brhitzer _fi the sißh gwiaohen

The apparatus aur Irzeugung of the pulsating pressure can consist of a KOLBON extending ± n · a Sylinder back νκ herbewegte

BisBrfindung tst particularly for one- .erfolgende by strongly cooling © Abteeratung Yon p-xylene .bxh: s mixtures suitable »Λ-Χ -p-Xjlol (vorssugBVe.lee as Hauptmenge- _c example wenigei-a SeWeSS 65) and at least one isomeric ο ■ xylene and / or ethyl = - enthaäton »

BATH ORIGINAL

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A particular aspect of the present invention is disclosed in accordance with standing closer

A feed check valve (1) is connected to a substantially horizontal pipe (2) 15.0 m (50 feet) long and 203 mm (8 inches) in diameter, which in turn has four internal scraper surface gauges (3) with a length of 7.8 m (26 feet) and a diameter of 152 mm (6 inches) "which are connected in series and parallel" are "connected" from the outlet of the fourth cooler to a spiral-type recycling pipe (6) with a length of about 30 m (10Ö fixed) and a diameter of 50 mm (2 inches) to the inlet of the first cooler _? wherein a Pum »pe interposed in the tube (4) _t iet to the quenched to HeeyeIiei he USLg d @ 9 Besohickungematerials required. Pressure su supply ..

A waitsres kurssos pipe (?) About 152 mm (6 inches) in diameter leads from the outlet end of the fourth radiator to an itonifiehen top (8) of an 8-column (9) _s where you see this part 152 mm in diameter (6 inches ^! At the holy point; su a diameter of 559 mm (22 inehes) at its base eirweiteriSj the solder connected to the cylindrical remainder of the sule · The part (10) of the column which see the

f & lX (8) is a simple one with a bupelimueefir of 559 aim (<! 2 inches) j 5! »9 mm

09811 / 1.133

ÖAD ORIGINAL

(22 inches) underneath tie the column walls holed and surrounded with a metal mesh to a filter section (11) form su; below this section, tie the column walls closed again. At the bottom of the column is a heating element (12) attached, which is protected against the weight of the column contents β by a support plate (13) »die eich below the heating element is »Sin Mantelex-Hitzer (5) is also provided »at the end of a cylinder (14)» the contains a reciprocating piston (15) is with connected to the column below the heating device. the Total length o this column is 2.7 m (9 feet) »

In performing the process, a feed material is used cooled to form a slurry by passing it through a check valve (1) and the pipe (2) is passed to the coolers (3); a part of this collection material becomes recycled to the inlet end of the first cooler, during the The remainder is fed to the upper end of the column (9) »At the When entering the column, there is a loss of liquid and 5th result of an outflow in and out of the filter section (U the slurry buckling one mainly firm hatred becomes »the piston (15) in the cylinder (H)» the one with the column below the heater is connected to 240 facts per minute moved back and forth “eo that on this one Weieo apply 240 pulses per minute to the slurry and must use the Liquid to be treated exercised! are · During the off »

909811/1133 ORIGINAL BATHROOM

With each pulse, the liquid is moved in front of the heater (12), "washing the solid substance above the heater and displacing the liquid in contact with the crystals in the filter zone (11)" which passes the walls of the column and acts as mother liquors -Current is drawn off. When the piston moves backwards, fresh feed material flows through the check valve (1) _P and a fresh slurry is introduced into the column (9)

Using the system described above, has pointed out »that there is sufficient resonance between the conical tip of the column and the check valve, which allows the slurry to move freely through this section the apparatus allows! there is little tendency for the pulsing effect in the column to interfere Damping effect from the preceding toilet of the apparatus on ge is raised · Since the Puloierungßfrequens; comparatively low and the (Irena layer between the semi-solid components and the slurry in the conical part of the column as Barrier acts »which divides the apparatus in this respect» does not become a significant reao within the column itself « nanze effect achieved »The apparatus is particularly suitable for. separation of p ~ xylene from mixtures containing 70% by weight of p-xylene, where the skin consists of o <~ and m xylene and ethy! benzene, ge suitable «

9098 11/1133

Claims (1)

εrse r ?. ■ '"■■■. Pat e η t a η a ρ r ü e h β 1 Process for separating an oil-crystallizable component from a feed material by means of strong cooling, in which the feed material is fed through a non-return valve to a cooler, in which the cooler is strongly cooled to form a slurry, the mother liquor is filtered off from the disintegration, TERIAL a pulsating pressure is applied to the au treated Ma and the crystallizable component is separated, characterized ₉ that a portion of the feed from the outlet of the radiator is reqyolisiert to its inlet "on a way ₀ of its length the BNTF RECOVERY by ä & n Cooler hindu is the same around * the pulsating bridge a Prequema besitat ₉ which caused the formation of standing waves in the treated material Beaonana imä 2 * gate direction aur implementation of the method according to claim i _t which consists of a non-return valve ₉ through which the Beschiokimga material is supplied to the cooler, from a filtration in the deia ufeter formation of a slurry from BeBchicilmngeraaterißl ßugei'üiiK t, and from a device aw Exertion of a pulöier and en pressure on the strongly: cooled ffe-fcerial ordered “thereby marked ₉ 90 9 8 1 T / 11 3 3 BAD ORIGINAL ~ 10 - that a device ame recycling iet dea Beschiokunga "materials provided by the outlet end of the Cooler to its inlet end" consisting of at least one pipe and a pump "dia sura driving the reoyclisierten material is adapted through the tube Wobot in this apparatus, the reoyolisierten of the The distance traveled by the loading material is approximately equal to that traveled by the loading material when θβ from the point ₉ to which the loading material is cycled _f to the point from which it is recycled; wandered, and the device z \ xv exertion of a pulsating pressure is able to deliver a pulsating pressure with a frequency which is sufficient to resonate and the formation of standing waves in the strongly cooled material swiochan the pulsing device and to enable the check valve MITNrANWXLTf DR-INO. H. f HUCKt, DIPL.-ING. H. BOHR CSPUtNO. S. STASOCR 90981171133 BATH ORIGINAL