CA1052290A - Separation of carbon black by liquid hydrocarbons - Google Patents

Separation of carbon black by liquid hydrocarbons

Info

Publication number
CA1052290A
CA1052290A CA233,308A CA233308A CA1052290A CA 1052290 A CA1052290 A CA 1052290A CA 233308 A CA233308 A CA 233308A CA 1052290 A CA1052290 A CA 1052290A
Authority
CA
Canada
Prior art keywords
carbon black
hydrocarbon
liquid
carbon
mixture
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CA233,308A
Other languages
French (fr)
Inventor
Heinz P. Giesen
Josef Hibbel
Willi Jansen
Sebastian Speth
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ruhrchemie AG
Original Assignee
Ruhrchemie AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ruhrchemie AG filed Critical Ruhrchemie AG
Application granted granted Critical
Publication of CA1052290A publication Critical patent/CA1052290A/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/02Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
    • C01B3/32Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air
    • C01B3/34Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents
    • C01B3/36Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of gaseous or liquid organic compounds with gasifying agents, e.g. water, carbon dioxide, air by reaction of hydrocarbons with gasifying agents using oxygen or mixtures containing oxygen as gasifying agents
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
    • C01B3/50Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465Composition of the impurity
    • C01B2203/0475Composition of the impurity the impurity being carbon dioxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465Composition of the impurity
    • C01B2203/0485Composition of the impurity the impurity being a sulfur compound
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2203/00Integrated processes for the production of hydrogen or synthesis gas
    • C01B2203/04Integrated processes for the production of hydrogen or synthesis gas containing a purification step for the hydrogen or the synthesis gas
    • C01B2203/0465Composition of the impurity
    • C01B2203/049Composition of the impurity the impurity being carbon

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Hydrogen, Water And Hydrids (AREA)
  • Industrial Gases (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

SEPARATION OF CARBON BLACK
BY LIQUID HYDROCARBONS

Abstract of the Disclosure A process for the separation of carbon black from liquids containing it comprising washing water containing said carbon black with a liquid hydrocarbon whereby said carbon black passes into the hydrocarbon phase. The hydro-carbon phase containing the carbon black is then passed through a disk centrifuge thereby separating said phase into (1) the bulk of said liquid hydrocarbon and (2) a mixture comprising the carbon black and the remainder of the liquid hydrocarbon. If desired, the mixture of carbon black and liquid hydrocarbon can be distilled in order to separate the hydrocarbon completely.

Description

~6~5~

This application is related to copending Canadian application 233,307, filed August 12, 1975.
One very useful source of energy is a product known as synthesis gas. This is an equimolar mixture of carbon ~
monoxide and hydrogen and is produced from petrochemical raw materials. More specifically, any hydrocarbons such as -propane, gasoline, liquefied gas, natural gas, and including crude oil, heavy oil, tar and asphalt are reacted with hy- -drogen under conditions creating incomplete combustion.
Usually, these hydrocarbons are reacted with oxygen in an amount 16~5;~Z910 which is insufficient for complete combustion in an open flame and in the absence of a catalyst. The reaction is generally carried out at temperatures of approximately 1300 C. and at pressures up to 90 bar. It has been known that pressures can go as high as 160 bar at least in pilot plants.
The products of this reaction include hydro-gen sulfide, carbon monoxide, methane, carbon dioxide and hydrogen, all of which are thermodynamically stable under the reaction conditions. Carbon black, although not an equilibrium partner under these conditions, is unavoidably formed. When natural gas is reacted, a minor amount of carbon black is produced. In the case of residual oils, the quantity of carbon black will normally amount to ap-proximately 2 to 4% of the carbon content.
When producing synthesis gas from petro-chemical raw materials by processes carried out on a com-mercial scale, the hydrocarbons and oxygen are separately preheated and introduced into the reactor through one or more burners. The burners may be water-cooled and they permit rapid and intimate mixing of the reactants. The hot gas leaving the reactor (having a temperature of 1400 to 1500 C.) is cooled in a waste heat boiler. Thereafter the carbon black is removed from the raw gas by scrubbing with water. Then the pre-purified gas is desulfurized and, if necessary or desired, passed to a carbon monoxide convert-l~S'~CI~O
er. Finally, carbon dioxide, hydrogen sulfide and carbon~xysulfide are largely removed in the gas scrubbing unit downstream of the converter. In certain cases, e.g. if the gas is to be used for synthesis of ammonia, a more complete purification is necessary.
Carbon black can be removed from the raw synthesis gas without any difficulty by simple scrubbing with water. However, problems are encountered when attempt-ing to further utilize the carbon black, especially when returning it into the process, which is desirable for rea-sons of economy.
In one known process, the total carbon black is returned into the reactor in a closed system. To this end, the carbon black-containing water is mixed in a decanter with naphtha, i.e. a gasoline fraction having a boiling range of about 70 to 112 C. This has the result that the total carbon black passes over into the naphtha phase. After having separated the two phases, water which is free from carbon black is withdrawn from the decanter.
The carbon black-containing naphtha is mixed with part of the feed oil and distilled off as the overhead fraction in a distilling column. The oil with the total carbon black remains as bottoms in the column. After being mixed with the remaining feed oil, it is passed to the preheater and thence into the reactor where it is completely gasified.

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In another known process, small amounts of feed oil are admixed with the carbon black-containing water.
The carbon black passes over into the feed oil phase and, with an appropriately high concentration, forms semi-solid carbon black-oil pellets. The clarified water is separated from the black-oil pellets by means of screens. The clari-fied water is returned into the process and the carbon black-oil pellets are ground to a slurry with the addition of further feed oil and either passed to a combustion unit or returned into the process as gasification agent.
Both of the known processes of carbon black sepa-ration have substantial disadvantages. The separation of carbon black by means of large amounts of naphtha causes the substantial expense of distillation for the recovery of the naphtha, and the separation of carbon black with small amounts of feed oil results in a not inconsiderable pollu-tion of the environment by vapors containing noxious mater-ials. In addition, there are technical difficulties as well.
Accordingly, it is an object of this invention to provide a process which overcomes the difficulties mention-ed above and permits the treatment and processing of carbon black-containing effluent waters in a manner which is satis-factory from both the technical and economical point of view.
In accordance with the invention, carbon black is separated from water (especially from water obtained when scrubbing the synthesis gas produced by partial oxidation .
' ., . . -1~5'~2gO
of hydrocarbons) by treatment with hydrocarbons. In this process, the carbon black is separated from a liquid contain-ing it by adding 20 to 100 parts of a liquid hydrocarbon per part of carbon black to the liquid to form a first mixture~
whereby the carbon black passes into the hydrocarbon phase.
This first mixture is passed into a settling zone and the hydrocarbon and carbon black are separated from the liquid by permitting the hydrocarbon and carbon black to form a layer upon the surface of the liquid. The layer is then passed through a disk centrifuge having a plurality of conical disks. The bulk of the hydrocarbons is separated from the resultant suspension of carbon black in hydrocarbon -~
in the disk centrifuge and the remaining carbon black-hydrocarbon mixture is, if desired, distilled in known man-ner. The carbon black remaining after distillation may be used in usual manner. For example, it may be introduced into the synthesis gas reactor after being mixed with feed oil. However, the carbon black-hydrocarbon suspension may also be used to recover dry carbon black.
It was assumed heretofore when separating carbon black fr~m scrubbing water that it is necessary for the complete extraction of the carbon black from the aqueous phase to use liquid hydrocarbons which are free from carbon black.
I~ this manner, it was desired above all to avoid having very fine carbon black particles remain suspended in the water.
Therefore, the hydrocarbons have been separated from the hydrocarbon-black suspensions by distillation. Moreover, the extent and the effect of the mechanical separation of part of the suspension liquid on the economy of the overall process were underestimated.
Surprisingly, it has been found that it is not nec-essary for treating and processing carbon black-containing water to use hydrocarbons which have been thoroughly purified C

^ -~s~z~o from small carbon black particles. Rather, it is possible to use hydrocarbons which do contain small carbon black particles. Therefore, it is feasible to separate mechanic-ally the bulk of the hydrocarbons loaded with carbon black after they have been used for the separation of carbon black from water. In accordance with the invention, this is effected with the use of disk centrifuges which ensure sufficient separation of the liquid and solid phases. It is possible in this manner to separate 80 to 90% of the naphtha contained in the suspension.
The naphtha having been separated mechanically can be directly re-used for separating carbon black from suspensions of carbon black and water. From the remaining residue having a concentration of carbon black of 10 to 15%
(as compared with about 2% in the original carbon black-hydrocarbon suspension) the carbon black-containing naphtha may, after addition of feed oil in known manner, be dis-tilled off except for small traces. However, a substan-tially lower expenditure of energy is required to enable it to be used again as a suspending agent. This naphtha is also used again for separating carbon black from sus-pensions of carbon black and water. The distillation resi-due is used as feed product in the synthesis gas reactor.
The process according to the invention will now be described with reference to the flow sheet attached hereto and described hereinafter in greater detail.

., - , ~ . : .

. . .

-1~5~2gO
Oxygen and fuel oil are passed through lines 1 and 2 and into a gasification reactor 3. The synthesis gas consisting of carbon monoxide and hydrogen and containing carbon black is freed from this carbon black by means of water in a carbon black scrubber 4. The s~nthesis gas pas-ses out of the system to further use through line 5. The mixture of carbon black and water is passed through line 6 and into a decanter vessel 7 into which naphtha is simul- :
taneously introduced through line 8. Separation of phases takes place in the decanter vessel 7. The naphtha/carbon .
black phase leaves the decanter vessel 7 through line 9 while the clarified water is withdrawn through line 11 and returned as recycle water into the carbon black scrubber 4.
Excess water leaves tl-le process through line 12. The naphtha-carbon black mixture emerging through line 9 from the decanter vessel is introduced into a disk centrifuge 10 in which separation into a phase enriched with carbon black and a clarified phase takes place. The clarified phase emerging through line 13 (naphtha having a residual content of carbon black of about 0.3%) is returned into the de-canter vessel 7. The concentrated phase having a carbon black content of 10 to 15% and leaving the Separator 10 through line 14 is mixed with fuel oil in a mixer 15 and passed through line 16 and into the ~asification reactor 3.
The mixture of naphtha and feed oil withdrawn from the mix-er 15 may be subsequently distilled to recover pure naphtha.

.
-l~)S;~Z~O
Example The test was performed with a disk centrifuge which had the following characteristics:

disk diameter 160 mm number of disks 37 distance between the disks 0.5 mm diameter of the separation layer approx. 125 mm rate of revolutions9500 revolutions per minute centrifugal acceleration 5000-6000 acceleration due to gravity 300 liter per hour of a mixture coming from the carbon black separation consisting of naphtha, and carbon black (with a carbon black charge of 20 gram carbon black per liter naphtha) and residual water with a temperature of 80 C were introduced into the disk centrifuge by pipe 9.
During the test, which lasted two hours, the quantity per time unit of the introduced liquid (290 to 300 liter per hour) and the quantity per time unit of the clarified li-quid from pipe 13 (215-225 liter per hour) were measured continuously. The quantity of concentrated carbon black sludge was determined by collecting in a receiver and found to be 75 liter per hour on an average. Samples of the sludge and the clarified liquid were collected regularly at 15 min. intervals and analyzed. The analysis of all sam-ples showed that the concentration of solids in the carbon ~ -8-...
, ~ . . .

~ Os ~ ~ 9 ~ I

black sludge was in the range of 70 to 85 gram carbon black per liter naphtha. A residual amount of solid between 0.2 and 0.8 gram carbon black per liter naphtha was found in the clarified liquid. The mechanically separated naphtha could be reintroduced immediately to the separation of car-bon black from the carbon black-water suspension.

-8a-.. . . . .

,

Claims (5)

THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
1. A process for separating carbon black from a liquid containing it comprising a) adding 20 to 100 parts of a liquid hydrocarbon per part of carbon black to said liquid to form a first mixture and whereby said carbon black passes into the hydrocarbon phase, b) passing said first mixture into a settling zone, c) separating said hydrocarbon and carbon black from said liquid by the method comprising permitting said hydrocarbon and carbon black to form a layer upon the surface of said liquid, and d) passing said layer through a disk centrifuge having a plurality of conical disks.
2. The process of claim 1 wherein the step of passing said layer through said disk centrifuge further comprises, separating said layer into the bulk of said hydrocarbon and a second mixture containing the remainder of said hydro-carbon and carbon black, recycling said bulk of said hydro-carbon to contact said liquid containing said carbon black, and distilling said second mixture to remove substantially all of said hydrocarbon from said carbon black.
3. The process of claim 1 wherein said liquid is water.
4. The process according to claim 1 wherein said hydro-carbon is petroleum naphtha.
5. The process according to claim 1 wherein said hydro-carbon is initially not free from carbon black.
CA233,308A 1974-08-23 1975-08-12 Separation of carbon black by liquid hydrocarbons Expired CA1052290A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19742440472 DE2440472B2 (en) 1974-08-23 1974-08-23 PROCESS FOR THE SEPARATION OF SOOT FROM THE PRODUCTS OF PARTIAL OXYDATION OF HYDROCARBONS

Publications (1)

Publication Number Publication Date
CA1052290A true CA1052290A (en) 1979-04-10

Family

ID=5923935

Family Applications (1)

Application Number Title Priority Date Filing Date
CA233,308A Expired CA1052290A (en) 1974-08-23 1975-08-12 Separation of carbon black by liquid hydrocarbons

Country Status (13)

Country Link
JP (1) JPS5146595A (en)
AT (1) AT333672B (en)
BE (1) BE832481A (en)
BR (1) BR7505232A (en)
CA (1) CA1052290A (en)
DE (1) DE2440472B2 (en)
FR (1) FR2282458A1 (en)
GB (1) GB1457379A (en)
NL (1) NL164003C (en)
PL (1) PL99325B1 (en)
RO (1) RO66329A (en)
SE (1) SE402120B (en)
SU (1) SU592348A3 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BRPI0610659B1 (en) * 2005-04-06 2017-12-12 Cabot Corporation A method for producing at least one gas
DE102007029435A1 (en) 2007-06-26 2009-01-08 Linde Ag Method and apparatus for using soot in POX plants

Also Published As

Publication number Publication date
AU8404875A (en) 1977-03-03
SU592348A3 (en) 1978-02-05
PL99325B1 (en) 1978-07-31
NL164003C (en) 1980-11-17
JPS5146595A (en) 1976-04-21
GB1457379A (en) 1976-12-01
SE402120B (en) 1978-06-19
NL164003B (en) 1980-06-16
BR7505232A (en) 1976-08-03
BE832481A (en) 1976-02-16
FR2282458B1 (en) 1977-12-16
JPS547637B2 (en) 1979-04-09
AT333672B (en) 1976-12-10
FR2282458A1 (en) 1976-03-19
ATA744674A (en) 1976-03-15
DE2440472B2 (en) 1976-11-25
NL7509499A (en) 1976-02-25
SE7509132L (en) 1976-02-24
RO66329A (en) 1979-07-15
DE2440472A1 (en) 1976-03-04

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