AT117484B - Process for accelerating the vulcanization of rubber and the like like - Google Patents
Process for accelerating the vulcanization of rubber and the like likeInfo
- Publication number
- AT117484B AT117484B AT117484DA AT117484B AT 117484 B AT117484 B AT 117484B AT 117484D A AT117484D A AT 117484DA AT 117484 B AT117484 B AT 117484B
- Authority
- AT
- Austria
- Prior art keywords
- sulfur
- rubber
- vulcanization
- parts
- accelerating
- Prior art date
Links
- 238000004073 vulcanization Methods 0.000 title claims description 6
- 229920001971 elastomer Polymers 0.000 title claims description 5
- 238000000034 method Methods 0.000 title claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000011593 sulfur Substances 0.000 claims description 9
- 229910052717 sulfur Inorganic materials 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 2
- -1 sulfur halogen compounds Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000006467 substitution reaction Methods 0.000 claims 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 239000003208 petroleum Substances 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920001021 polysulfide Polymers 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- FWMUJAIKEJWSSY-UHFFFAOYSA-N sulfur dichloride Chemical class ClSCl FWMUJAIKEJWSSY-UHFFFAOYSA-N 0.000 description 2
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 239000000899 Gutta-Percha Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 240000000342 Palaquium gutta Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 244000001591 balata Species 0.000 description 1
- 235000016302 balata Nutrition 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- NGDNCZPCIZNCQS-UHFFFAOYSA-N ctk3j8699 Chemical compound Cl=S NGDNCZPCIZNCQS-UHFFFAOYSA-N 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229920000588 gutta-percha Polymers 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 125000005936 piperidyl group Chemical group 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Description
<Desc/Clms Page number 1>
EMI1.1
Gegenstand der Erfindung ist die Herstellung von Polysulfiden, welche besonders für die Verwendung als Beschleuniger bei der Vulkanisation von Kautschuk, Guttapercha, Balata u. dgl. geeignet sind. Die Erfindung besteht darin, dass man Schwefelchloride oder andere Halogenide des Schwefels der allgemeinen Formel S., CI, z. B. SCI2 oder Lösungen von Schwefel in Schwefelchloriden auf Salze der Ditioearbaminsäure der allgemeinen Formel
EMI1.2
einwirken lässt, in welchem Rund R1 Wasserstoff oder gleiche oder ungleiche organische Radikale, z. B.
Methyl, Aethyl, Phenyl, Piperidyl od. dgl. und M Metallradikale, z. B. Natrium, Kalium, Ammonium od. dgl. bedeuten. Bei der Reaktion, die vorteilhaft in einem flüssigen Medium, z. B. Benzol, Petroläther, Äthyläther vonstatten geht und bei der man zweckmässig ein Molekül des Schwefelhalogenides mit zwei Mole- küken des Ditiocarbamates zusammenbringt, bilden sich neben Chloriden der zur Anwendung gelangenden 1Yietallradikale Polysulfide der allgemeinen Formel
EMI1.3
Die Vulkanisation kann in der üblichen Weise, z. B. unter Zusatz von Schwefel und anderen Materialien, wie z. B. Zinkoxyd, Russ u. dgl. vorgenommen werden. Infolge des hohen Gehaltes an Schwefel in den Beschleunigern ist es aber auch möglich, auf den Zusatz von elementarem Schwefel bei der Vulkanisation zu verzichten.
Beispiel 1 : Diphenyläthylthiuramtetrasulfid : 338 g trockenes phenyläthylditiocarbaminsaures Ammoniak werden in Petroleum suspendiert, die Mischung mit Eis gekühlt und unter Rühren allmählich 107 g Schwefelchlorür (S2Cl2), das mit Petroleum verdünnt ist, zulaufen gelassen. Der Niederschlag wird abfiltriert, mit Petroleum gewaschen, trocknen glassen, in Wasser suspendiert, filtriert, mit Wasser gewaschen und abermals getrocknet. Es wurden 276-5 g trocknen Tetrasulfids erhalten, dessen Schmelzpunkt 142 C ist.
100 Teile Kautschuk (smoked sheet) werden mit 0-5 Teilen des Tetrasulfids, 5 Teilen Zinkoxyd und 5 Teilen Schwefel gründlich durchgemischt und bei einer Temperatur von ungefähr 95-100 vul- kanisiert.
Ohne Zusatz von elementarem Schwefel kann die Vulkanisation z. B. unter Benutzung folgender Mischverhältnisse durchgeführt werden : 100 Teile smoked sheet, 5 Teile Zinkoxyd, 4 Teile Diphenyl- äthylthiuramtetrasulfid.
EMI1.4
saures Ammoniak werden in ungefähr 200 cm"Petroleumäther suspendiert. Zu der mit Eis gekühlten Mischung lässt man 5'3 cm3 Chlorschwefel SCL2, die mit Petroläther verdünnt sind, allmählich zutreten.
Der Niederschlag wird abfiltriert, erst mit Petroläther, dann mit Wasser gewaschen und getrocknet. Das erhaltene hellgelbe Pulver schmilzt bei 133 .
0-5 Teile des Trisulfids werden als Beschleuniger einer Mischung von 100 Teilen smoked sheet, 5 Teilen Zinkoxyd, 5 Teilen Schwefel zugesetzt. Nach gründlicher Durcharbeitung wird bei 95-100 vulkanisiert.
**WARNUNG** Ende DESC Feld kannt Anfang CLMS uberlappen**.
<Desc / Clms Page number 1>
EMI1.1
The invention relates to the production of polysulfides, which are particularly suitable for use as accelerators in the vulcanization of rubber, gutta-percha, balata and the like. Like. Are suitable. The invention consists in that sulfur chlorides or other halides of sulfur of the general formula S., CI, z. B. SCI2 or solutions of sulfur in sulfur chlorides to salts of ditioearbamic acid of the general formula
EMI1.2
can act, in which around R1 hydrogen or identical or different organic radicals, z. B.
Methyl, ethyl, phenyl, piperidyl or the like. And M metal radicals, e.g. B. sodium, potassium, ammonium or the like. Mean. In the reaction, which is advantageously carried out in a liquid medium, e.g. B. benzene, petroleum ether, ethyl ether takes place and in which one expediently brings one molecule of the sulfur halide together with two molecules of the ditiocarbamate, in addition to the chlorides of the metal radicals used, polysulphides of the general formula are formed
EMI1.3
The vulcanization can be carried out in the usual manner, e.g. B. with the addition of sulfur and other materials, such as. B. zinc oxide, soot u. Like. Be made. Due to the high sulfur content in the accelerators, it is also possible to dispense with the addition of elemental sulfur during vulcanization.
EXAMPLE 1 Diphenylethylthiuram tetrasulfide: 338 g of dry ammonia phenylethylditiocarbamate are suspended in petroleum, the mixture is cooled with ice and, with stirring, 107 g of sulfuric chloride (S2Cl2) diluted with petroleum are gradually added. The precipitate is filtered off, washed with petroleum, left to dry, suspended in water, filtered, washed with water and dried again. 276-5 g of dry tetrasulfide, the melting point of which is 142 ° C., were obtained.
100 parts of rubber (smoked sheet) are thoroughly mixed with 0-5 parts of the tetrasulfide, 5 parts of zinc oxide and 5 parts of sulfur and vulcanized at a temperature of approximately 95-100.
Without the addition of elemental sulfur, the vulcanization can e.g. B. be carried out using the following mixing ratios: 100 parts smoked sheet, 5 parts zinc oxide, 4 parts diphenyl äthylthiuramtetrasulfid.
EMI1.4
Acid ammonia is suspended in about 200 cm "petroleum ether. 5'3 cm 3 of chlorosulfur SCL2 diluted with petroleum ether are gradually added to the mixture, which is cooled with ice.
The precipitate is filtered off, washed first with petroleum ether and then with water and dried. The light yellow powder obtained melts at 133.
0-5 parts of the trisulfide are added as an accelerator to a mixture of 100 parts of smoked sheet, 5 parts of zinc oxide and 5 parts of sulfur. After thorough working through, it is vulcanized at 95-100.
** WARNING ** End of DESC field may overlap beginning of CLMS **.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US117484XA | 1926-01-27 | 1926-01-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| AT117484B true AT117484B (en) | 1930-04-25 |
Family
ID=21751812
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| AT117484D AT117484B (en) | 1926-01-27 | 1927-01-20 | Process for accelerating the vulcanization of rubber and the like like |
Country Status (1)
| Country | Link |
|---|---|
| AT (1) | AT117484B (en) |
-
1927
- 1927-01-20 AT AT117484D patent/AT117484B/en active
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