DE1296294B - Process for the production of furnace soot post-treated by oxidation - Google Patents

Process for the production of furnace soot post-treated by oxidation

Info

Publication number
DE1296294B
DE1296294B DEC37892A DEC0037892A DE1296294B DE 1296294 B DE1296294 B DE 1296294B DE C37892 A DEC37892 A DE C37892A DE C0037892 A DEC0037892 A DE C0037892A DE 1296294 B DE1296294 B DE 1296294B
Authority
DE
Germany
Prior art keywords
oxidation
treated
furnace
production
furnace soot
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.)
Pending
Application number
DEC37892A
Other languages
German (de)
Inventor
Thornhill Fred S
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.)
Continental Carbon Co
Original Assignee
Continental Carbon Co
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 Continental Carbon Co filed Critical Continental Carbon Co
Publication of DE1296294B publication Critical patent/DE1296294B/en
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/44—Carbon
    • C09C1/48—Carbon black
    • C09C1/50—Furnace black ; Preparation thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Description

Es ist bekannt, durch pyrolytisch^ Zersetzung von Kohlenwasserstoffen Ruß zu erzeugen, z. B. nach dem Kanalverfahren durch Zersetzung in offener Flamme oder nach dem Ofenverfahren durch Zersetzung mittels eingeschlossener direkter Flamme. Je nach dem Herstellungsverfahren haben die erzeugten Rußsorten unterschiedliche Eigenschaften. Die vorliegende Erfindung betrifft die Verbesserung der Eigenschaften von Ofenruß.It is known to produce soot by pyrolytic decomposition of hydrocarbons, e.g. B. after the canal method by decomposition in an open flame or by the furnace method by decomposition by means of an enclosed direct flame. Depending on the manufacturing process, the generated Types of carbon black have different properties. The present invention relates to improving the Properties of furnace soot.

Beim Ofenverfahren wird das Kohlenwasserstoffmaterial in einem zylindrischen Reaktor zersetzt, welcher am Auslaßende einen Ablöschabschnitt besitzt. In einem anschließenden Sammelabschnitt wird der erzeugte feinteilige Ruß von den Abgasen getrennt und sodann meistens in einem Trocken- oder Naß-Pelletisierer mit nachgeschalteter Trockentrommel weiterverarbeitet.In the furnace process, the hydrocarbon material is decomposed in a cylindrical reactor, which has a quenching section at the outlet end. In a subsequent collection section the fine soot produced is separated from the exhaust gases and then mostly in a dry or Wet pelletizer with downstream drying drum processed further.

Es ist weiterhin bekannt, Ofenruß durch verschiedene Oxydationsverfahren nachzubehandeln, z. B. durch Erhitzen mit Salpetersäure, Ozon, Sauerstoff, nitrosen Gasen usw. Durch solche Oxydationsbehandlungen werden dem Ofenruß Eigenschaften verliehen, die den Eigenschaften eines Kanalrußes (EPC) ähnlich sind. Von Nachteil ist dabei, daß gleichzeitig die Alterungseigenschaften der Rußprodukte durch diese Behandlung verschlechtert werden, insbesondere wenn Metallspuren wie solche von Cu, Fe, Ni, Mg u. a. anwesend sind.It is also known to post-treat furnace soot by various oxidation processes, z. B. by heating with nitric acid, ozone, oxygen, nitrous gases, etc. Such oxidation treatments give the furnace soot properties which are similar to the properties of a sewer carbon black (EPC). The disadvantage here is that at the same time the aging properties of the carbon black products worsened by this treatment especially when traces of metal such as Cu, Fe, Ni, Mg and others. present are.

Es wurde nun gefunden, daß diese Nachteile durch Behandlung des Ofenrußes mit Ammoniumphosphat vermieden werden können.It has now been found that these disadvantages can be overcome by treating the furnace soot with ammonium phosphate can be avoided.

Das erfindungsgemäße Verfahren zur Herstellung von durch Oydation nachbehandeltem Ofenruß ist dadurch gekennzeichnet, daß dem Ruß vor oder nach der Oxydationsbehandlung ein saures Ammoniumphosphat in einer Menge entsprechend einem Gehalt von 0,1 bis 1,0 Gewichtsprozent Phosphor, bezogen auf den Ruß, zugegeben wird.The process according to the invention for the production of furnace soot post-treated by oxidation is characterized in that an acidic ammonium phosphate is added to the carbon black before or after the oxidation treatment in an amount corresponding to a content of 0.1 to 1.0 percent by weight of phosphorus, based on the carbon black, is added.

In bevorzugten Ausführungsformen des Verfahrens erfolgt die Zugabe des Ammoniumphosphats mit dem Ablöschwasser und/oder mit dem zur Pelletisierung zugesetzten Wasser.In preferred embodiments of the process, the ammonium phosphate is added with the quenching water and / or with the water added for pelletizing.

Der erfindungsgemäß behandelte und nachoxydierte Ofenruß hat ähnlich günstige Eigenschaften wie der Kanalruß, der bekanntlich leichter zu verarbeiten ist. Als weiterer Vorteil ergibt sich durch die erfindungsgemäße Behandlung eine erheblich gegenüber unbehandeltem Ruß erhöhte Zündungstemperatur. The furnace soot treated and post-oxidized according to the invention has similarly favorable properties like sewer soot, which is known to be easier to process. Another advantage results from the treatment according to the invention has an ignition temperature that is considerably higher than that of untreated soot.

Zum Nachweis der verbesserten Alterungseigenschäften wurden verschiedene Rußproben in Kautschukzusammensetzungen nach ASTM D-1522-60 T eingearbeitet und getestet. Die Alterung der Proben erfolgte durch 72stündiges Erhitzen im Luftofen bei 105° C.To prove the improved aging properties various carbon black samples were used in rubber compositions according to ASTM D-1522-60 T incorporated and tested. The samples were aged by heating in an air oven for 72 hours 105 ° C.

so Als Vergleichsprobe wurde Kanalruß (EPC) verwendet. sewer carbon black (EPC) was used as a comparison sample.

In Probe 1 wurde ein mit HNO3 oxydierter Ofenruß verwendet.In sample 1, furnace soot oxidized with HNO 3 was used.

In Probe 2 wurde ein Ofenruß verwendet, der a5 zunächst mit NH4H2PO4 (entsprechend 0,2 Gewichtsprozent P) behandelt und beim Trocknen in der Trockentrommel mit HNO3 oxydiert worden war.In sample 2 a furnace soot was used which a5 had first been treated with NH 4 H 2 PO 4 (corresponding to 0.2 percent by weight P) and oxidized with HNO 3 during drying in the drying drum.

In Probe 3 wurde ein mit HNO3 oxydierter Ofenruß (wie Probe 1) verwendet, der nach der Oxydation mit NH4H2PO4 (entsprechend 0,2 GewichtsprozentP) behandelt worden war.In sample 3 a furnace soot oxidized with HNO 3 (like sample 1) was used which, after the oxidation , had been treated with NH 4 H 2 PO 4 (corresponding to 0.2 percent by weight P).

Aus den in der Tabelle aufgeführten Testergebnissen geht die Überlegenheit der Proben 2 und 3 hervor.The superiority of samples 2 and 3 can be seen from the test results listed in the table emerged.

In der Spalte »Zeit, Minuten« ist die Vulkanisationszeit der Kautschukproben bei 145° C in Minuten angegeben.The "Time, minutes" column shows the vulcanization time of the rubber samples at 145 ° C in Minutes specified.

Zeit (Minuten)Time (minutes)

EPCEPC

frisch I alt Probe 1
frisch I altfresh I old sample 1
fresh I old

Probe 2
frisch I altSample 2
fresh I old

Probe 3 frisch I altSample 3 fresh I old

Festigkeit, kg/cm2 Strength, kg / cm 2

Dehnung, % Strain, %

Modul, 200% ...
Modul, 300% ...Module, 200% ...
Module, 300% ...

30 60 9030 60 90

30 60 9030 60 90

30 60 9030 60 90

30
60
9030th
60
90

29,71 28,83 27,0729.71 28.83 27.07

565 530 530565 530 530

765 880 845765 880 845

1555 1710 16201555 1710 1620

17,39 16,05 14,7517.39 16.05 14.75

325 285 275325 285 275

1155 1405 13551155 1405 1355

2125 27,91
26,58
24,082125 27.91
26.58
24.08

540
525
500540
525
500

775
825
800775
825
800

1555
1605
15351555
1605
1535

13,87
13,72
12,3213.87
13.72
12.32

290
265
255290
265
255

1115
1435
11951115
1435
1195

28.72
28,12
26,7128.72
28.12
26.71

535
525
520535
525
520

795
885
830795
885
830

1630
1735
16701630
1735
1670

21,79 19,11 18,7321.79 19.11 18.73

330
295
320330
295
320

1555
1585
14501555
1585
1450

2730
2700
25002730
2700
2500

27,35 26,01 23,9727.35 26.01 23.97

570 545 535570 545 535

650 720 685650 720 685

1350 1425 13501350 1425 1350

19,64 17,49 16,5119.64 17.49 16.51

365 330 320365 330 320

1270 1235 12251270 1235 1225

2200 2240 21252200 2240 2125

Bei Zündproben eines erfindungsgemäß behandelten Ofenrußes wurde festgestellt, daß bei einem Phosphatzusatz entsprechend 0,1 bis 1,0 Gewichtsprozent P bei 4000C keine Entzündung und bei 500° C eine Zündung erst nach 2,5 Stunden eintrat. Vergleichsproben entzündeten sich in beiden Fällen bereits nach wenigen Minuten.In Zündproben an inventively treated furnace black, it was found that occurred at a phosphate additive corresponding to 0.1 to 1.0 percent by weight P at 400 0 C and no ignition at 500 ° C an ignition only after 2.5 hours. Comparative samples ignited in both cases after just a few minutes.

Claims (1)

Patentanspruch:Claim: Verfahren zur Herstellung von durch Oxydation nachbehandeltem Ofenruß, dadurch gekennzeichnet, daß dem Ruß vor oder nach der Oxydationsbehandlung ein saures Ammoniumphosphat in einer Menge entsprechend einem Gehalt von 0,1 bis 1,0 Gewichtsprozent Phosphor auf den Ruß zugegeben wird.Process for the production of furnace soot post-treated by oxidation, characterized in that that an acid ammonium phosphate in an amount corresponding to one is added to the carbon black before or after the oxidation treatment Content of 0.1 to 1.0 percent by weight of phosphorus is added to the carbon black.
DEC37892A 1965-02-16 1966-01-14 Process for the production of furnace soot post-treated by oxidation Pending DE1296294B (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US43318665A 1965-02-16 1965-02-16
US43315965A 1965-02-16 1965-02-16

Publications (1)

Publication Number Publication Date
DE1296294B true DE1296294B (en) 1969-05-29

Family

ID=27029765

Family Applications (1)

Application Number Title Priority Date Filing Date
DEC37892A Pending DE1296294B (en) 1965-02-16 1966-01-14 Process for the production of furnace soot post-treated by oxidation

Country Status (6)

Country Link
DE (1) DE1296294B (en)
ES (1) ES321793A1 (en)
FR (1) FR1465920A (en)
GB (1) GB1074664A (en)
NL (1) NL6601753A (en)
SE (1) SE333032B (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2178383A (en) * 1937-06-17 1939-10-31 Columbian Carbon Carbon black

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2178383A (en) * 1937-06-17 1939-10-31 Columbian Carbon Carbon black

Also Published As

Publication number Publication date
SE333032B (en) 1971-03-01
NL6601753A (en) 1966-08-17
GB1074664A (en) 1967-07-05
ES321793A1 (en) 1966-06-16
FR1465920A (en) 1967-01-13

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