DE2225511A1 - PROCEDURE FOR REDUCING THE CONCENTRATION OF AN ORGANIC COMPOUND IN AN AQUATIC SOLUTION OR SUSPENSION - Google Patents

Description

PATENT LAWYERS

Munich: Frankfurt / M .:

Dipi.-Chem. Dr. D.Thomsen Dlpl.-Ing. W. Weinkauff

Dipl.-Ing. H. Tiedtke (Fudiehohl 71)

Dipl.-Chem. G. Buehling
Dipl.-Ing. R. Kinne
Dipl.-Chem. Dr. U. Eggers

8000 Munich 2

Kaiser-Ludwig-Platz6 2 May 5, 1972

Imperial Chemical Industriea Limited London, Great Britain

Method for reducing the concentration of an organic compound in an aqueous solution

or suspension

The invention relates to a method for treating a discharge. In particular, relates they refer to a method of reducing the concentration of an organic halogen-containing compound in an aqueous one Solution or suspension.

According to the invention, a method for reducing the concentration of an organic halogen-containing compound in aqueous solution or suspension created, in which

309811/1104

the solution or suspension is brought into contact with an organic polymer or copolymer for a period of time, Many marriage is sufficient to reduce the concentration of the halogen-containing compound to a predetermined level, wherein the method is characterized in that the polymer or copolymer at least one of the components paraffin waxes, Polyolefins, vinyl polymers or their halogenated derivatives.

The term "suspension" is intended here to include a liquid / liquid emulsion.

This method is particularly suitable for the treatment of dilute solutions or suspensions, which for example Contain 0.1 to 20,000 parts per million of a halogen-containing compound. Is it preferably containing halogen? Bond in solution, that is, it forms one with deia Uasser single homogeneous phase.

Many halogenated compounds are aln in water considered insoluble, but are in very low concentrations actually miscible with water. Such compounds include halogenated benzenes or phonols, for example chlorobenzene or dichlorobenzene «* j halogenated alkanes, for example Ethylene dichloride (1,2-dichloroethane) or propylene dichloride (1,2-dichloropropane); halogenated alkenes, for example trichlorethylene or vinylidene chloride and containing halogens «insecticides, for example 1.1.l-trichloro-2.2-bis- (p-chlorophenyl) -

309811/1104

BAD ORIGiNAU

ethane (DDT). In sufficient concentration, halogenated Substances may be incompatible with sewage treatment systems and in certain cases it is feared that they may be an ecological one Danger if they are released into the environment. The method according to the invention can be used to reduce the concentration of these substances in water to acceptable levels.

The method according to the invention is particularly suitable to remove chlorinated substances from aqueous solution or Suspension.

The polymer will have the properties of the halogen-containing Connection selected according to which is to be removed. In particular, the solubility characteristics of the polymer should and be similar to the halogen-containing compound. Solubility parameters for many organic polymers are compiled in J. Brandrup and E. H, Immergut - Polymer Handbook, page IV 3 ^ 1 (Interscience Publishers, New York, London and Sydney, 1966) and can for the halogen-containing compounds on the basis of the relationship:

can be calculated in which vein the solubility value, is the evaporation energy, and V is the molar volume.

In any procedure in which a loosened 3 0 9 8 11/110 /. "'.'

BATH

Substance from solution on an absorbent absorbent are the two most important factors in deciding which one to use Working conditions and procedural costs, the achievement?; Rate the equilibrium distribution of the solute between the Solution and the absorbent, and the capacity of the absorbent for the solute. When according to the invention Process are the absorbent polymers, for example? Polyethylene, which often starts with different molecular weights and varying degrees of crosslinking and crystal, can get v / ground. In general, the recovery rate tends the equilibrium between the polymer and the aqueous Phase and the Absorptiohskapazit'it of the polymer to with the decrease in the crystallinity, the molecular weight and the To increase the degree of crosslinking of the polymer,

The above factors should be taken into account when choosing the polymer and making simple experiments readily show suitable polymer / halogen-containing combinations Links,

Suitable polymeric substances include low or high density polyethylene, polypropylene, polystyrene, polymethylpentane, chlorinated polyethylene, or polypropylene, polyvinyl chloride), chlorinated poly (vinyl chloride), polyvinylidene chloride) and polyimethyl methacrylate), copolymers, for example Cop ("lomerej wcj'-hr - :?« - ohijijri substances include or acrylonitrile-lutadiene-styrene copolymers, can also can be used, as well as natural or synthetic rubbers. Paraffin wax and halogenated, for example

<O 3 8 1 1 1 1 P ι

chlorinated waxes, are also useful polymeric substances.

Low density polyethylene and poly (vinyl chloride) are particularly effective and therefore preferred.

The polymer (this term is also intended to include the copolymers) is preferably in the form with a large Surface area, for example as granules or powder. This also includes the use of a rigid or flexible one Foam, preferably with an open cell structure, or the use of a fiber mat or the like. The polymer can but also in the form of a film or sheet, which preferably has a sheaf-shaped surface, or that Polymers can be used as two- or three-dimensional meshwork.

The aqueous solution or suspension can be brought into contact with the polymer in any way, which is suitable for bringing about a liquid / solid contact and such contact can either be discontinuous or be continuous.

For example, the aqueous solution or suspension by a bed of polymer particles or by a let through the porous mass of the polymer. Especially when a continuous process is used, the particle bed in upstream direction in relation to the aqueous disturbance

309811 / 11QÄ

be moved. But you can also use the aqueous solution or suspension with an amount of polymer particles moving and then dissolving the particles by filtration or Separate sedimentation. The polymer particles can float onto the surface of the water or the aqueous solution or the suspension can be allowed to pass over a bed of the polymer. The aqueous solution or suspension can be over a sheet or film of the polymer, or passing through a tube or mesh of the polymer.

The polymer can be used as a moving web or disk, part of which is absorbed into the aqueous Solution or suspension is immersed, so that the polymer is moved in a circle through the liquid.

The time during which the aqueous solution or Suspension remains in contact with the polymer is dependent on the speed with which the halogen-containing Compound distributes itself between the polymer and the water, rapidly reaching an equilibrium distribution shorter contact times needed. In general, contact times are from one second to a few hours, particularly from 1 to 10 minutes, preferred. Suitable contact times can be selected through routine experimentation.

The temperature of the aqueous solution or suspension is not critical and can be between 0 and 80 C, for example be. Working at ambient temperature is advisable

303811/1104

and preferred «

The amount of halogen-containing compound which can be taken up by the polymer varies with the nature of the halogen-containing compound and the polymer. The amount can be as much as 50 % by weight but usually does not exceed 10%.

The polymer can be regenerated for reuse, if necessary with recovery of the halogen-containing material retained from the polymer, a variety of methods being applicable. Be j Spielßweise You can use the halogen-containing; Ver-Linauni; by ablation by means of steam or by solution extraction, preferably an organic solvent, or the polymer can be of sufficient IV Mporature to remove the halogenated Compound v, n volatilize. Such volatilization is preferably carried out by passing a stream of hot gas, for example air or nitrogen, over or through the polymer. Particularly, when the halogen compound is absorbed by the polymers, it may by applying pressure to the polymer, eefrebeiienfalls ^ - ⁿ connection with a high temperature can be expressed.

The erfindungsEeiafif ^"three methods can also help Hey? Rabretzunß the concentration of halogenated compounds in wet gases used \ example mruen _s the volatile effluent from the Wasserdampfdestillation.-A solches'Verfahren

3098Π / Τ10 / -

BATH ORIGINAL '

- 8 is also within the scope of the invention,

Even if the above description refers to the extraction a single halogen-containing compound from an aqueous .System, it is clear that the process in is equally applicable to systems which are a mixture of halogen-containing compounds or a mixture of a halogen-containing Contains compound with other organic or inorganic substances.

It has been found that in general the equilibrium distribution a halogenated pre-bond between the Uaπser and the polymer of the equation:

Q = Kc

follows, in which Q is the equilibrium concentration on the polymer, c is the equilibrium concentration in the water And
K is a constant (the ennobling coefficient).

PUi 'non-halogenated substances is the relationship between Q and c not always linear. In particular hydroxylic ones Substances such as alkanols and phenols tend to be in addition, an absorption isotherm of the type:

Q = Kc *

own, in which η is greater than 1 ,

^ O 9 8 1 1/1 1 Π I, rr-

It can be seen that the absorption efficiency for such substances (measured by the ratio Q / c) is omitted at low values of c and the inventive method is therefore particularly useful for selective Removal of halogen-containing compounds from an aqueous mixture of the halogen-containing compound and an organic. see hydroxyl compound.

The invention is now illustrated by the following exemplary embodiments explains in which parts by weight and parts by volume bear the same relationship as kg and dm.

example 1

An aqueous solution which contains 5 parts per million (based on weight) of o-dichlorobenzene is run at a temperature of 25 ° C. through a bed of low-density polyethylene in the form of 300 μm particles. The flow rate is such that the mean residence time of the solution in the bed is 2 minutes. After 115 bed volumes have been treated, analysis of the effluent solution shows that the concentration of o-dichlorobenzene is 2 parts per million. After treating 1 * 18 bed volumes, the effluent is found to contain H parts per million of o-dichlorobenzene. After 200 bed volumes have been treated, the concentration of o-dichlorobenzene in the effluent begins to rise to the initial concentration in the feed solution. At this point the passage of the solution is interrupted and dna Pott rt> generated by

3 0 9 8 11/110 4 - = *

BATH ORIGINAL

- ίο -

water vapor is allowed to pass through it ^{at 10O 0 C for one hour.} By condensing the water vapor and separating off the aqueous solution, β parts of o-pichlorobenzene are obtained. The polyethylene is used again in the following experiments.

example 2

200 parts by weight of an aqueous solution, which contains parts per million chlorobehaol, is brought into contact at 15 ° C. with 10 parts of a low-density polyethene film with a high surface area for 1 ^E > minutes. After removing the film, the concentration of chlorobenzene in the aqueous solution is 10 parts per million. The chlorobensol can be removed from the film by washing with petroleum ether for 30 minutes, flat for one hour. with fio '(, the film can be used again for the absorption of further (' chlorobenzene.

Example 5

^E 50% weight of an aqueous solution with a content of 33 parts per ml of ion o-diochlorobensol, one brings with 1 part of particles 10000 mm in diameter olncis t / nrjncirrfor; stretched polymers (manufactured by copolymers olnuii fU> iiL « ; c! iof; from Ci Clev / .S Poly (propylfunarate) unt! 35 (Jew.'i iltyrol) for 21;> Ld. at 15 C in contact.! lach dem!. 'ntfernen il «·« Τ' ο1 «ΐΗτ <η futliilt the aqueous solution ;; unq 13 parts per flillion of o-dichloroenzene.

308811/1104. & »D Original

- '11 -
Example k

500 parts by weight of an aqueous solution with a Content of 150 parts per million o-dichlorobenzene, one brings tiiit a part of beads made of chlorinated polyethylene with a Particle size of 200 µm in diameter, in contact for 3 days at 15 ° C. After removing the polymer by filtering off, analysis shows that the aqueous solution is 71 parts each Million contains o-dichlorobenzene. The degree of chlorination of the Polyethylene can range from 27 to Ό.

Example 5

100 Gewichtstei Ie an aqueous solution having a Gthalt to I800 parts per million of 1,2-dichloropropane, brings nan with a Toil Polyäthylenkügelchen with a diameter of 300 jim 12 hours at 0 ° l6 into contact. After removing the polymer by Abi nitration: one finds that the aqueous solution contains 80H parts per Hillion dichloropopan.

Example 6

Poly (vinyl chloride) as 250 to 350 µm beads one with different volumes of an aqueous solution in contact, which 50 parts per million (on the weight be-κι, Ι ', ίπ) Contains trichlorethylene. After 3 days the fetal Concentration of Triehloräthylens in the aqueous Phase (c) and measured on the polymer (Q). ■:

30981 1 / 11P4

It is found that Q / c = 320 for values of c between 0.5 and 32 parts per million.

Example 7

In order to determine the distribution coefficient K, a number of tests are carried out as follows: Different weights (V) of an aqueous solution containing Co parts per million (based on weight) of o-dichlorobenzene are mixed with m parts by weight of polyethylene particles with a Diameter of 250 to 350 μτα brought into contact for a time which is long enough to ensure equilibrium (typically 3 to Ί days). At the end of this time, the polymer is removed by filtration and the concentration ar. O-dichlorobenzene in water (c) is measured by gas-liquid chromatography using an electron capture detector.

The results are shown below in Table I for "Alkathene" particles ("Alkathene" is a registered trademark Imperial Chemical Industries Limited) grade 11/03/00, which has a melt flow index of 2.0 and a nominal density, measured according to British Standard 3 ^ 12: 1966, owned by 0.918.

The equilibrium concentration of o-dichlorobenzene on the polyethylene (Q) can be calculated from the analyzes.

30981 1/1104

Fig. 1 shows a logarithmic plot of Q versus c and it can be seen that the results are in a straight line, what with the equation

Q = Kc

coincides, where K, the partition coefficient, 'is 120,

Table I.

o-DichlorobenzDl on polyethylene c _Q = 106 parts per million

V / m

4: 1

8: 1

1 S: 1

20: 1

30: 1

'10: 1

;, u; 1

80: 1 100: 1 I ¹ JO: 1 200: 1 250: 1 300: 1 350: 1

c (parts per million)

0.75 1.6 2.7 3.8

5.1

6.7

10.2

13.5 25.5 21.8

27
32
31 35

30981 1/1

222551 I.

- in -

For comparison, the above procedure is repeated, replacing the o-dichlorobenzene with phenol. The results are shown in Table II:

Table II

Phenol on polyethylene
c _o = 100 parts per million

V / m c (first attempt) c (second attempt) Parts per mi lliori

10: 1 18

20: 1 M 52

40: 1 yy 4l

50: 1-49

80: 1 42

100: 1 5 3 55

150: 1 55 58

200: 1 60 6.5

250: 1 65 67

300: 1 71 72

400: 1 78 80

The results are shown graphically in FIG. 1, and it can be seen that the distribution isotherm of the equation:

Q = Kc ²

BATH ORIGINAL

309811/1104

follows, where K = 2.5 x 10 ⁶ .

For further comparison, the above procedure is repeated again, the o-dichlorobenzene being replaced by ethanol replaced.

The results are set out in Table III and are shown graphically in FIG. 2 (! Logarithm! Β rather a scale). The polyethylene particles, which have a diameter of 250 to 350 μm, are "Alkathene ¹¹ , quality 19/03/03 with a melt flow index of 20 and a nominal density of 0.916.

Table III
Ethanol on polyethylene

Co = 116 parts per million

Q V / m c (parts per million) (g ethanol / g polymer)

400: 1 68

300: 1 60.5

200: 1 58

100: 1 47.3

40: 2 19

20: 2 12.5

Co = 120 parts per million

500: 1 78

400: 1 70

300: 1 65

250: 1 61.5

200: 1 60

_{150: 1} 57 3098117110Λ :. _{9> 5 x}

19.2 χ 10 "5 16.6 χ ΙΟ " ³ 11.6 χ ΙΟ " ³ 6.8 χ 10 "5 2 χ 10-5 1 χ ΙΟ " ³ 21 χ ίο- ³ 2b χ ΙΟ " ⁵ 16.5 χ 10 "5 14.6 χ ΙΟ " ³ 12 χ ΙΟ "'

100: 1 - 52 5.8 χ ΙΟ " ³

50: 1 38 4.9 χ 1θ " ³

40: 1 35. 3.4 χ 1θ " ³

40: 2 24 2.1 χ ΙΟ " ³

20: 2 15 1.1 x ΙΟ "· ^5th

500: 1 81 19.5 χ ΙΟ " ³

400: 1 75 18 χ 1θ "3

300: 1 68 15.6 χ 1θ " ³

250: 1 63 14.3 x ΙΟ " ³

200: 1 58 12.4 χ ίο " ³

150: 1 51 10.4 χ 10-3

100: 1 47 7.3 χ 1θ " ³

50: 1 31 4.5 χ ΙΟ " ³

40: 1 30 3,6 χ ίο " ³

20: 1 28 1.8 χ ΙΟ " ³

40: 2 25 1.9 x 1θ "3

20: 2 18 1.0 χ 10-3

It can be seen that the distribution isotherm with the equation:

Q = Ko ¹ * ⁸

is consistent, where K = 4.6 χ 10 *.

Similar results are obtained with poly (vinyl chloride) and polypropylene.

309811/1104

Example 8

The procedure of Example 7 is repeated, replacing the o-dichlorobenzene with trichlorethylene. The polymer consists of polyethylene particles with a diameter of 250 to 350 μm, "alkathene", quality 23/04/00 with a melt flow index of 200 and a nominal density of 0.913.

The results are shown in Table IV and graphed in Figure 3 on a linear scale.

Table IV Trichlorethylene on polyethylene

co = 50 parts per million

V / m (c) (Parts per million) 100: 1 26.6 60: 1 21.2 20: 1 12.5 10: 1 6.2 5: 1 5 Co = 11 parts per million 100: 0.93 6.5 80: 1.03 7.3 '10: 0.99 5 20: 1 2.9 PO: 1.893 ?,8th

1.8

0 9 8 1 1 /! i 0

BATHROOM ORIGINAL

- 18 Example 9

The procedure of Example 7 is repeated using trichlorethylene and a copolymer of ethylene and vinyl acetate - repeats (2 wt% vinyl acetate.). The results are shown in Table V and plotted graphically on a linear scale in Pig, ^,

Table V

Trichlorethylene on ethylene / vinyl acetate copolymers Co = 100 parts per million

V / m C parts per million g, trichlorethylene /

g polymer

200: 1 'S 3

100: 1--30

80: 1 23, ^

ΊΟ: 1 16 , 2

20: 1 11.1

20: 2 3 _s i

'10: 2 2.2

K = 260-15

If the above experiment is repeated with a copolymer containing 18 % vinyl acetate, then:

κ = ob - in,

The all-in-one employee in example 7 becomes ί U :) H 1! / I 1 Γ) Α

11, Ί X ΙΟ " ³ 7 x 1.0 -3 6.12 X ΙΟ " ³ 3.35 X ΙΟ " ³ 1.78 X ΙΟ " ³ 0.97 X ΙΟ " ³ O ₁ Il X 10 " ³

repeated using a number of polymers and halogen-containing Substances used. The results -. are shown in Table VI:

309811/1104

j- au tr j. ie ν χ

at
game
No. Ilalogates
substance Polymer Enamel
flow
index
of the poly
meren Polymer-
density Particles
size of the
Polymers
At the Co (parts
per million) 50 K 10 Trichlorethylene Polyethylene
"Alkathenes · ¹
14/05/00
H _w = 28,000 7.0 0.917 250-350 50 91 - 6 11 rt Polyethylene
"Alkathene"
19/03/00
Γ? = 24,000
W. 20th 0.916 dd 50 100-13 12th ti Polyethylene
"Alkathene"
23/12/00
Ή = 19,000
W. 200 0.913 1200
1400 50 92 i 15 13th ti ethylene / pro
pylene copcly
meres
25 wt
Ethylene, 250-350 64 200 ± 40 14th tr Polyethylene
with soot
"Alkathene"
19/04/01 / H 20th 0.916 25Ο-35Ο 64 250-45 15th ti Paraffin wax - - unreasonable- cu
ger solid 107 t 16 16. ti Poly (vinyl
chloride) "Corvic ¹
D5O / 16 25Ο-35Ο 560 ± 61 ^H w = 70,000

17th

18th

19 20

21

Trichlorethylene

22nd

23

24

25 26

27 · 28

Carbon tetrachloride

Poly (vinyl chloride). "Corvic" D65 / 1O2 M> 140,000

Poly (vinyl chloride). "Corvic" XD50 / 38

Poly (vinyl chloride)

Poly (vinyl chloride). "Corvic" H55 / 34

Vinyl chloride / vinyl acetate copolymer 15 % vinyl acetate. ⁿ Corvic "R46 / 88

Vinyl chloride / vinyl acetate copolymer 8 % vinyl acetate "Corvic" R58 / 94

Vinyl chloride / vinyl acetate. 2 % vinyl acetate. "Corvic" XR 54/71

Vinyl chloride / vinyl acetate copolymers 13% vinyl acetate "Corvic" Q44 / 62

Polypropylene. 28 % atactic

Chlorinated wax "Cereclor" 56L

Chlorinated wax "Cereclor" S

Chlorinated wax "Cereclor" S 250-350

50-500

as delivered

120-170

250-350

50

50

50 50

100

50

50

as delivered 1OO

250-350

fluid

50

480

480

480

154

328 +

se

127 80 +

265 360

72

62 +

902 + 1070 + 1176 +

29 Tetrachlor
carbon Chlorinated wax
"Cereclor" 65L - - fluid 480 1637 + 500 30th μ Polyethylene "Alka
thene "23/04/00 200 0.913 250-350 20th 84 + 15 31 η Poly (vinyl chloride)
"Corvic" D50 / I6 - - 50-400 20th 123 + 11 32 dd Vinyl chloride / Viny33-
denchloride copoly-
neres - - 50-400 100 202 + 32 33 o-dichlorobenzene Polyethylene. "Alka
thene "19 / Ο3 / ΟΟ
M _w = 24,000 20th 0.916 250-350 40 730 + 52 34 «Ι Polyethylene. "Alka
thene "14/03/00.
M ^ = 28,000 7.0 0.917 Il 48.3-
106 570 + 101 35 Chlorobensol 7.0 0.917 dd 170 163 36 1.2-dichloro
propane η η dd IO5O 85 + 20 37 Hexaehlor
buta-1.4-diene ti dd dd ff 50 14th 38 η Poly (vinyl chloride).
("Corvic" D50 / 16 - - 50-400 50 23 ! 39 Iodobenzene Polyethylene. "Alka
thene "I9 / O3 / OO 20th 0.916 250-350 500 20 + 4

"Alkathene", "Corvic" and "Cereclor" are registered trademarks of Imperial Chemical Industries Limited. The K value of "Corvic" vinyl chloride polymers is through the first number shown which follows the alphabetical prefix in the polymer code.

Example HO

An aqueous solution containing 85 parts by weight per million o-dichlorobenzene is passed through at 25 ° C a bed made of low density polyethylene ("Alkathene" 19 / O3 / OO) go with a particle size of 250 to 350 µm. The middle Residence time is 2.1 minutes. After passage of 113 bed volumes, the effluent contains 2 parts per million of o-dichlorobenzene.

Example * J1

An aqueous solution containing 6 ^ by weight Trichlorethylene parts per million is passed through a bed of poly (vinyl chloride) particles ("Corvic" D50 / 16) (10 parts by weight). The mean residence time is 1 minute. the Concentration of trichlorethylene in the effluent is analyzed at intervals by gas-liquid chromatography and the results are shown in Table VII.

3 09 8 11 /.11 0

Table VII Trichlorethylene on poly (vinyl chloride)

through the bed concentration of trichlorethylene passed solution volume in the drain (parts $ e million) (parts)

24 Example 42 3.2 IkM 2 216 5.8 288 10.3 360 6th 432 5.7 505 4.5 576 1 648 1.3 720 3 792 2.9 865 H

Weight parts of an aqueous solution with an oil content of equal parts phenol and o-dichlorobenzene (50 parts ^ e million) are in contact with m parts by weight of poly (vinyl chloride> particles ("Corvic" D50 / 16) with a diameter of 120 to 180 μm The mixture is left to stand for 3 days in order to ensure the oil weight and the concentration of o-chlorobenzene in the water (c) is then measured by gas chromatography

- 25 VIII shown.

Table VIII

o-dichlorobenzene and phenol on poly (vinyl chloride)

V / m c (parts per million)

100: 1 23

80: 1 20

60: 1 15.5

40: 1. 12th

20: 1 8.5

10: 1 5

5: 1 1.5

Example 43

The procedure of Example 42 is repeated using poly (vinyl chloride) from 120 to l80 μπι ("Corvic" D65 / IO2) and an aqueous solution containing trichlorethylene (10 parts per million) and phenol (50 parts per million). The analyzes for trichlorethylene after 4 days are shown in Table IX:

Table IX

Trichlorethylene and phenol on poly (vinyl chloride) V / m c (parts per million)

..100: 1 -. . ■■ =. - .- ■ 4.45 ■■ - ■ ■. = ■ - ■,

60: 1 30 98 11 7 11 04 ² » ^8: · ■■ - ■■

40: 1 K = 120 ί 20 (cf. 1.5 154 is). 20: 1 example 1.25 10: 1 0.7 5: 1 0.4 Example 17 where K = 44

The procedure of Example 42 is repeated using poly (vinyl chloride), 120-180 µm ("Corvic" D65 / IO2) and an aqueous mixture of trichlorethylene (10 parts per million, phenol (50 parts per million) and o-dichlorobenzene (100 parts per million). The analyzes on Trichlorethylene and o-dichlorobenzene after 4 days are shown in Table X.

Table X

Trichlorethylene, o-dichlorobenzene and phenol on poly (vinyl chloride)

Wm concentration
in water
Trichlorethylene
(Parts each
Million) Concentration in
Water on o-tue
chlorobenzene
(Parts each
million Concentration on
Polymer at 0-
Dichlorobenzene
(mg / g) 100: 1 5.35 25th 80: 1 4.4 20th M, = 60: 1 3.5 16.3 5.0 40: 1 1.7 11 * >> (> 20: 1 1.6 5.3 1.9

309811/1104

10: 1 0.9 2.7 0.97

5: 1 0.5 1 0.495

K = 100 £ 22 K = 310

example k5

An aqueous solution of trichlorethylene is left at 15 C through a bed of poly (vinyl chloride) particles of 120 to 180 pm ("Corvic" D5O / I6) (bed volume - 10 parts by volume) go through. The concentration of trichlorethylene in the effluent is analyzed at intervals by gas-liquid chromatography and the flow continues until the bed is saturated.

Dry steam is then allowed to pass through the bed » The steam running off is condensed and analyzed for ethylene Ethylene cleaned, the steam flow stopped, and Tri eh Io advises hy len solution again guided through the bed. This way of working is repeated several times. The results are shown below:

First cycle

Initial concentration of TricfelorEtlsylen, 50 parts per million. Dwell time 1.4 minutes fairies,

3088Π / 110.4

Amount of enforced solution
(Parts by volume) Concentration of trichlor
ethylene in the drain (parts
per million Regeneration I250 parts by volume each
minute 175 6.5 Gas flow rate
moderate steam 535 5 700 6th 785 8th 870 10.5 96O 13.5 Passed through when saturated
Solution set 13OO parts by volume Tri-
amount of chlorethylene 4.2 10 " ² parts by weight

Amount of condensed vapor that has passed through (parts by volume)

80 Second cycle 2 , 52 χ 10 210 * ,1 χ 10 ~ ²

Amount of trichlorethylene recovered (parts by weight)

-2

Initial concentration of trichlorethylene

Dwell time

Amount of solution passed through (parts by volume)

50 parts per million

1.1 minutes

Concentration of trichlorethylene in the drain (parts per million)

5.5

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530 620

725 800

895 985

Amount of solution passed through at saturation

9, 5 6, 5 5, 8th 6th 10 13th , 5 ge 13 ^ 0 parts by volume Regeneration

Flow velocity of the gaseous vapor

Amount of condensed steam passed through (parts by volume) 625 parts by volume / min.

Amount of trichlorethylene recovered (parts by weight)

80 Third 3, 26 χ ΙΟ " ² 100 3, 8 χ ΙΟ " ² l60 * · 1 χ ίο " ² cycle

Initial concentration of trichlorethylene

Dwell time

Amount of solution soaked through (parts by volume) 50 parts by volume

11.8 minutes

Concentration of trichlorethylene in the drain (parts per million)

23 35 65

150 0
1
1.5

3 0 9 8 1 1/1 1 0

255 400

500 6oo

Amount of solution passed through when saturated

Amount of trichlorethylene absorbed when saturated 3.5 5.5 6.25 8.7 1000 parts by volume

3.52 10 ² parts by weight

Regeneration

Flow velocity of the gaseous vapor

Amount of condensed steam passed through (parts by volume)

60 2.40 Fourth cycle X X 10 80 3.18 X 10 100 3.34 X 10 130 3.5 10 '

625 parts by volume / min.

Amount of recovered trichlorethylene (weight parts)

-2

-2

-2

Initial concentration of trichlorethylene

Dwell time

Amount of solution passed through (parts by volume) 60 parts per million

11.8 minutes

Concentration of trichlorethylene in the drain (parts per million)

21 45

309811/1104

75

125

180

232

278

iiOO

600

Amount of solution passed through when saturated

Amount of trichlorethylene absorbed when saturated

5 6

7.1

7.5

15.2

850 parts by volume

4.0 10 ² parts by weight

Example 46

The procedure of Example 45 is repeated using o-dichlorobenzene on polyethylene particles from 250 to 350 µm ("alkathenes" I9 / O3 / OO). The bed volume is again 10 parts by volume. Initial concentration 10. parts by volume.

Initial concentration of o-dichlorobenzene 50 parts per million. Residence time 1.6 minutes.

Amount of solution passed through (parts by volume)

120

25O

825

955

Concentration of o-dichlorobenzene in the outlet (parts per million)

9.5

3 0 9 P 1 1/1 1 0 4

Amount of solution passed through when saturated

Amount of o-dichlorobenzene absorbed when saturated

1600 parts by volume

H χ 10 " ² parts by weight

Regeneration

Residence time of the gaseous vapor

Enforced
(Parts by volume) Amount of condensate 176 530 Example St.

0.16 sec.

Amount of recovered o-dichlorobenzene (parts by weight)

1.6 10 3.6 χ 10

-2

-2

An aqueous solution of carbon tetrachloride (500 parts per million) is passed through a bed of polyethylene particles, 150 to 250, ("Alkathene" 23/04/00) go. the The residence time of the solution is 2 minutes and the bed is saturated after the passage of 1190 parts by volume of the solution,

Hexane is then allowed to pass through the bed at the same flow rate and concentration carbon tetrachloride in the effluent is determined at intervals by gas-liquid chromatography, whereby one Electron capture detector used. The results are shown below:

309811/1104

Amount of passed hexane (parts by volume)

50

108

145

205

310 Carbon tetrachloride concentration (parts per million)

> 135O 1300 800 450 130

below detection limit

3O901J / 1KU

Claims (1)

- 34 claims / Ώ Procedure for reducing the concentration of a organic compound in an aqueous solution or suspension, the solution or suspension with an organic Polymers or copolymers is brought into contact for a time which is sufficient to reduce the concentration of the organic Reduce connection to a predetermined level, characterized in that a solution or suspension an organic halogen-containing compound with a polymer or copolymer in contact, which at least one of the components contains paraffin waxes, polyolefins, vinyl polymers or their halogenated derivatives or from them consists. 2, method according to claim 1, characterized in, that one uses an aqueous solution or suspension which also has an organic hydroxylic compound. 3. The method according to claim 1 or 2, characterized in that the polymer or copolymers after use regenerated by wiping with steam. 30981 1/1104 sr L e r s e i t e