DE1443066A1 - Process and device for refining crude naphthalene - Google Patents

Description

B. WEHR, H. SEILER H. STEHMANN DIPLOMA INEENIEUR PATENTANWÄLTE Nürnberg a

LYNAR8TRASSE 1 TOITNIANWALIt ESSENWEIN8TR. - »- β

RUF: 97 67 28 α. 97 67 81 CALL: OFFICE 26036 and 28047 PRIVATE: 74306

TELERAMM-AORESSEiSElLWEHRPATENT TE L EG R A M M -A D R ES S E: ST E H P AT E NT

BANK ACCOUNT: BANK ACCOUNTS:

BERUNER BANK A.-G. BERLIN-HALENSEE A 44 3066 DEUTSCHE BANKA.S. NUREMBERG NO. 14S4

DEPOSIT CASE 3β ■ GIRO ACCOUNT NO. 97 856 '' ~ ^ ^WV VOLKSBANK FÜRTH / BAYERN ACCOUNT NO. 46S4

POST CHECK ACCOUNT: BERLIN-WEST 5938 POST CHECK ACCOUNT: NUREMBERG 67081

Berlin, April 14, 1960
(Wr-M-Hs)

SOGIEIE POUR! 'EXPLOITATION OF THE PEOÖBDES AB-DEE-HALDEN

Process "and device" for refining Eohnaphtalia

The invention relates to the refining of crude naphthalene,

It is known that the Eohnaphtalin is obtained from coal tar by a fractional distillation OeI catches its distillation curve at the boiling point of the naphthalene. On cooling, this oil produces a crystalline mass that contains 50 to 80 $ naphthalene * The rest occluded oils are formed duroli between the crystals. In order to extract the naphthalene, Dian has to use the OeI separate that accompanies the naphthalene. This process, which is refining, is difficult and costly the practical implementation and increases the manufacturing costs significantly for the purified naphthalene

The suction of this crystalline mass does not allow volletändige separation, and it is established that about 6 to 8 ^r / £ of the oil, the treatment to escape. Under the best possible working conditions, ie a very slowly crystallized oil that results in particularly well-formed crystals, as well as a maximum centrifugal force that reaches a value of 1,200 g,

• 8 0 9 8 13/1267 " ² "

«2 -ρ

dooh still remain in the manufactured naphthalene 5 des Oil occluded. Other treatment methods were thus measured Take Stt HiA to order a product with a unit degree of 96 or get more m *

The most commonly used method consists of pressing » generally in the heat of a hydraulic press is carried out »The squeezing of the mockery stops This is a very costly process, and it is also expensive in terms of the materials required to be used the operating costs associated with this procedure «

Haphthalene is also obtained with a degree of unity of mediated washing of the Bohnaphtalins with solvents or cleaning or saponification products, however, the Recovery of detergents, their consumption and the final separation of the naphthalene was multiple and costly Procedural steps.

Naphthalene with a unit degree of $ 96 is also obtained by washing the Rohnaphtalins with warm water in one Centrifuge «Bas naphthalene, however, holds a certain amount of the Water BurUok, which must then be removed, and through this procedure is not possible to achieve a unit degree of more than $ 98.

Finally, haphthalene is obtained with all degrees of unity by means of repeated recrystallization during which enriches the product in naphthalene. The procedure is effective, but involves slow and costly manipulations *

BAD ORIGINAL - 3 809813/1267

According to this, this disadvantage would be overcome, invites Method and device for Haffinetion you Bahnaphtalin be proposed, dttroh dl · it is made possible to haphtalin in any desired degree of purity up to 99% ad more generally, with the Yorbekanaten expensive process white of pressing, washing, or crystallization la ForHuLl come"

Sas erflndamjEsgemajto Terfahren is lasessondsr · dadareh Rewarded, dap sea Torher doroh cooling rerfeetlgtee raw naphthalene lanfiiaa rewarmed what the Sohaelsea has to offer Teranreiaifftmgea is effected, the aas dea sarüekblelbeadea Product aitropfen, where »loh the last forteehreitend aa Vaphtalia aarelehert, whereby the faphtalla is gewoaaea »as soon as the same the eewttnsohtea Beiafcvltsfrad reached cat.

The process according to the invention is based on the folfeadea experimentally en

1. The crystallized sonaphthalene gives aas the aasgeblldetea Crystals give off a certain oil age, and the product has one Schmelepaakt, which is above that of the crude product, ron dea aan aasgegaagen 1st, Torteilhafter catfish wifd this handling » long saa guiding principle of crystallization or dripping Bohnaphtalins executed at Baamtenperatar.

2. The amount of oil that drips off or that remains with the crystals is saturated at the dripping temperature old Vaphtalln.

3. The Oelaeng · that in the crystals a dripping NaOH remains, 1st virtually the same irrespective of a Lempe _r ..τ χ-, Vischer: 1O ° C and 80 ⁰ C (melting point of the pure naphthalene)

finQfin / n <? 7 bad original

Hieraue follows that the surüokbleibende in the crystals Oei _9, the iet saturated with naphthalene even more and contains more naphthalene when the! Temperature is increased ·

The impurity thus represents an ever decreasing proportion of the practically constant amount of oil that is occluded in the crystals, depending on the temperature being increased, the degree of unity of the naphthalene in the mass remaining after dripping down to a value of ron 100 ⁰ O increases as soon as the temperature is the same as the melting temperature of the pure product

Thus, the method of the invention is practical in the carried out in the following way.

The mass of the Hohnaphthalin is slowly warmed up, and the sioh Forming oils are separated by draining. · Man increased then the temperature up to the point at which the desired temperature is reached Degree of purity

The separated oils are then put into the tar oil for the procedure the first separation of the Hohnaphtalins introduced. Thus the recovery of ifaphthalene is practically $ 100.

Ee is necessary that the mass of the Eohnaphtalins in all Parts are heated uniformly as the most effective part of the process depends on it.

It is also an inventive purpose of a device For the implementation of the above procedure, propose the creation of these working conditions in a simpler and more economical way Way can be achieved in the best way. This device is particularly characterized in that the same one

809813/1267 _{BAD 0R! G} , _n , _aT _ η -

Has trough, which duroh a filter device in «white on top of each other arranged parts is divided, this filter assembly is provided at the level of the bottom of this trough. Of the upper part of the trough contains structural elements for the circulation of a heat exchange liquid, with free between them Gaps remain for the Bohnaphtalln to pass through. The upper part of the trough has an insertion opening, wherein an emptying opening for the various components of the Hohnaphtalin is provided at the bottom of the lower part

Further characterizing features of the invention can be found in FIG the following description, with reference to the accompanying drawings, which are given by way of example only are.

FIG. 1 is a similar illustration showing the course of travel explained

Figures 2 and 3 are perspective views in partial elevation The execution forms of the inventive method

Ss is taken from FIG. 1 besug »in the dtr ▼ experienced run and the basic procedure of the Torriohtung according to the invention are shown. This device essentially has a trough a, which is divided into two parts arranged one above the other by means of a pilfering device b. The piltering device is arranged near the bottom of the trough. In the upper part of the trough there is an overflow device for a liquid such as water, which is circulated as a pump, _{AD 0R} | _GINAL

809813/1267 - 6 -

A jellyfish for a cold liquid (P, P.) As well as a source for a warm liquid (7.0.) you can optionally use the Arrangement · to be supplied to the circuit of the device ο, an overflow vessel f allowing excess liquid deduct.

Under these Vorausset zuxigQn the procedure in the following manner is set in motion. A heavy solution (SD * 5, like a soda solution) is introduced into trough a in such a way that it occupies the lower T% ± 1 of the trough. Crude naphthalene in the liquid state is then introduced over this solution.

The device then comes to equilibrium at a temperature above the so-called Eohnaphtalins point of view, where the cold liquid (PP ₄ ) is continuously fed into the circuit. then gradually cooled.

The laphtalin then crystallizes and as soon as a temperature of 50 ⁴ C (after about 6-8 hours for a trough with a height of Ton 1 α) is reached in the haphthalene mass, the supply of the cold liquid is interrupted. The Boienvereussuss is opened and the heavy solution (SD) is removed, which is used for a later procedure. The purpose of this solution is to "take care" that a free space of crystals remains at the bottom of the device. The circle is then heated by means of the warm liquid (FG ₁ ), and the oil begins to drip off. This removes the oils (H) which contain little laphthalene and which are dead in the starting product. These oils are becoming more and more common

809813/1267 _BAD original _?

Haphtalln at, and dtr melting point dee in the device τ · γ-permanent Product rises rapidly · As soon as the desired conditions are reached «the flow is interrupted, and the sohmelaen of the surllok that remains terrible is achieved by heating Product, which is then as a finished product (I.P.) is caught · You will be caught oil (H) at a later date Procedure introduced regardless of the drained oil fractions buk Bohluss der Yerverfahren as purified naphthalene tract of the same quality. The draining takes about 8-10 hours, and the final Sohmelien 1 or 2 8 hours, making the entire procedure not used for more than 24 hours "

The following table shows the practical results of Animal Trying on the coating of a laphtaline with a degree of purity Tone 96, $ 98 and over 99 # (^ of the degree of unity are indicated in brackets) as soon as the ohmic point is ascended.

Vn 4L Λλύ · "RmmnViA ftViinir

Kftfrlfil

Bohnaphtalin besohiokt

Initial products

refined ·· laphtha-colored

73f4 64.5

78 (965t)

Yersttoh 1

61 *

BohnaphtaHn besohiokt initial product

refined laphtha green

73t4 63 *

lOOjC

Tersuoh 2

»T

-Backled 73t4 (98 ^) 100 * Tersach 3 ^ - Initial Products 68 · Ot refined
^ a Haph ta * - u 79 · 50 * BATH ORIGINAL

Material Fp j » the Beaohiokung

Eohnaphthalene

beeohiokt 73.4 * 100 $ Beginning products 67

refined investigation 4

Haphthalene 78 ($ 96) $ 29

1, parliamentary group

refined

Haphthalene

2nd fraction 79t7 ° ($ 99.4) $ 25

One can treat mockery of naphthalene at a lower concentration than the crude naphthalene given below. The results are equally good, but the Yields are lower »

The following are two practical embodiments of the invention Direction of the gate indicated »which is different during the implementation of the method according to the invention as particularly satisfactory have proven.

In the case of the embodiment according to FIG. 2, the parallelepiped Trough a, which duroh the perforated cloth or meshwork b in Two parts 1 and 2 arranged one above the other are subdivided, an introduction opening for the crude naphthalene in part 1, and one Emptying opening 4 for the components of the naphthalene in part 2.

The circulation torque c for the liquid in part 1 becomes through horizontal ear rails 5 formed «the upper legs are Liquid fed through a feed opening 6, which in a water tank 7 opens, which is attached to one of the small side surfaces of the parallelepiped trough. A outer end of the tubes 5 of the first row penetrates the water

809813/1267 BAD ORfGiMAL - 9 -

container 7 while the other outer edge of this drill penetrates into a water container 7a which is arranged on the opposite small surface of the parallel container, and this also applies to an external end of the drill. The "wide range" arrangement of the pipes by means of the "appropriately arranged water tanks 7a, 7b .... 7"" It thus enables the liquid to run through all the bores 5 τοη above near below in the torrlohtung" to conclude through which a drainage opening 8 can be made. Each drilling J is provided on the outside with wings 9, which are arranged in such a way that the bands of the wings of adjacent drilling approach βion as far as possible. Xs have proven to be extremely satisfying. Dl · wing 9 »« wiping those bohnaphtalin circulates »play a double role. Initially, they require a large damming area. Then they cause the crystalline hatred of Bohnaphtalins to persist during the progressive simmering of them.

The embodiment shown in FIG. 3 differs Of those near the figure 2 only duroh the shape of the Circumferential rotation or the same is made by parallel, perpendicular Cells 10 formed "whereby" between the same free spaces remain for the passage of the Bohnaphtalin. Every cell has Deflecting sheets 11 on "which result in a labyrinth in such a way" that co the liquid has a long way between the introduction pipe

CM

* "" and the discharge pipe 13 must surüoklace. The tubes 12 and 13 J2 are in a corresponding manner with the collectors 14 and 15 Terbun-

OO

ο co

the »at which openings 6 and 8 are arranged. The cells 10

BATH

dl · tin · high · tone If 50 », have eich al · special β ■ Proven peace-making.

X *) üSwa * n. 1 "Eahmen the invention variations and modifications can be made without rom öeiat of foun same extent abiuwe blaze.

809813/1267

Claims (5)

Pat mtaai prttdhi 1, "method" or Baffination of Sohnaphtalin, characterized gckennselohnet _t that iu da · sonaohst duroh cooling rerfcetlgte Bohnaphtalin slowly heated, whereby there · Sohaelsen of the impurities is effected "dl" au "the surüokbleibenden product are drained" wherein check, as "the latter Forteohreitend to laphtalin added "because" is won "as soon as the desired degree of purity is reached. 2. Procedure naoh Anepruoh. 1, as known · T t that one has several tractions during the 'dripping' wins "either in the Eurüok procedure, or as a Tractions of the laphtaline old rersohiedenen degrees of unity can be obtained. 3. Procedure naoh Aaspruoh 1 or 2 »dadaroh g e k e η η be without, that the cooling and the warming reraittele Ualaofes an act carried out in a closed circle will* 4. The method according to any one of the preceding claims "is characterized by the fact that cooling and heating are carried out in the same system, whereby a heavy solution is introduced at the lower end of the same before cooling, which is drained off after heating", so as to crystallize des Bohnaphtalins at the lower end of this system * su prevent 5. Device sur performing the method according to claims 1-4 * is identified by the arrangement of a trough, which is arranged in a pilgrim direction one above the other 809813/1267 _{BaD 0RlsltÄL} "- g rope · is subdivided »the one adjacent to it Arranged on the bottom »with the upper rope of the trough · β the building elements for the circulation of a heat exchanger liquid For the Duron, Rohnaphtalin's whisper comes freely Two of these structural elements remain »the upper part of the Trogee has an entry stretcher opening »while the lower one Line of the same is a discharge opening for the various Components aa lower end the lower! Part has 6 · Device after address 5 »marked i ohnet through the design of the components for the circulation of the liquid in the form of rows of tubes that are provided with wings. 7 · Device according to claim 5 »marked 1 without t duroh the formation of the components for the circulation of the liquid in the form of parallel spaced apart Cells 8, device according to claim 7 »characterized by the arrangement of deflection plates inside each cell, so as to lengthen the fluid's Durohlaufwege. BATH ORIGINAL 8098 ι 3/1267