PL36010B1 - - Google Patents
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- Publication number
- PL36010B1 PL36010B1 PL36010A PL3601052A PL36010B1 PL 36010 B1 PL36010 B1 PL 36010B1 PL 36010 A PL36010 A PL 36010A PL 3601052 A PL3601052 A PL 3601052A PL 36010 B1 PL36010 B1 PL 36010B1
- Authority
- PL
- Poland
- Prior art keywords
- acetone
- mercaptobenzothiazole
- mercaptobenzothiazole disulfide
- potassium hydroxide
- red color
- Prior art date
Links
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 3
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Description
Przedmiotem wynalazku jest sposób oznacza¬ nia dwusiarczku merkaptobenzotiazolu, szczegól¬ nie w mieszankach kauczukowych.Dwusiarczek merkaptobenzotiazolu (przyspie¬ szacz DM), sluzy w przemysle gumowym jako czynnik przyspieszajacy wulkanizacje. Poniewaz niewielkie jego ilosci decyduja o wlasciwosciach pólfabrykatów, a co za tym idzie i gotowych wy¬ robów, konieczne jest oznaczanie jakosciowe i ilosciowe tego zwiazku w mieszance surowej i zwulkanizowanej. Do tego celu sluzy sposób oznaczania dwusiarczku merkaptobenzotiazolu wedlug wynalazku, polegajacy na zabarwianiu sie roztworu azotanu bizmutu w razie obecnosci merkaptobenzotiazolu na kolor czerwony.Przyklad I. Dwusiarczek merkaptobenzo¬ tiazolu rozpuszcza sie w acetonie, dodaje wod¬ nego 10 %-ego roztworu azotanu bizmutu, a na¬ stepnie krysztalek wodorotlenku potasu, przy *) Wlasciciel patentu oswiadczyl, ze twórcami wynalazku sa inz. Marian Krygier i Zbigniew Trudnowski. czym wystepuje natychmiast charakterystyczne jasno-czerwone zabarwienie.Przyklad II. Mieszanke gumowa rozdra¬ bnia sie dokladnie, dodaje okolo 5 cm* acetonu i podgrzewa lekko do temperatury wrzenia ace¬ tonu. Po dodaniu do wyciagu acetonowego kilku kropel wodnego 15 %-ego roztworu azotanu biz¬ mutu, a nastepnie krysztalka wodorotlenku po¬ tasu, wystepuje natychmiast, w razie obecnosci merkaptobenzotiazolu, charakterystyczne jasno- czerwone zabarwienie roztworu, którego inten¬ sywnosc zalezy od ilosci przyspieszacza w mie¬ szance.Przyklad III. Rozdrobniony dokladnie wul- kanizat zalewa sie acetonem w ilosci okolo 10 cm8 i podgrzewa ostroznie do wrzenia. Do wy¬ ciagu acetonowego po lekkim ostudzeniu dodaje sie wodnego 20 %-ego roztworu azotanu bizmutu oraz krysztalek wodorotlenku potasu, przy czym w razie obecnosci merkaptobenzotiazolu wyste¬ puje zabarwienie jasno-czerwone, którego inten¬ sywnosc zalezy od ilosci przyspieszacza w mie¬ szance.Przy oznaczaniu ilosciowym intensywnosc za¬ barwienia roztworu porównuje sie z wzorami, zawierajacymi odpowiednio oznaczona ilosc dwu¬ siarczku merkaptobenzotiazolu. PLThe invention relates to a process for the determination of mercaptobenzothiazole disulfide, especially in rubber mixtures. Mercaptobenzothiazole disulfide (DM accelerator) serves as a vulcanization accelerator in the rubber industry. Since its small amounts determine the properties of semi-finished products, and thus also of finished products, it is necessary to qualitatively and quantitatively determine this compound in the raw and vulcanized mixture. The method for determining mercaptobenzothiazole disulfide according to the invention is used for this purpose, which consists in staining a solution of bismuth nitrate red in the presence of mercaptobenzothiazole. and then a potassium hydroxide crystal, at *) The owner of the patent stated that the inventors were Marian Krygier and Zbigniew Trudnowski. the characteristic light-red color immediately appears. Example II. The rubber mixture is crushed thoroughly, about 5 cm.sup.3 of acetone are added and slightly heated to the boiling point of acetone. After adding to the acetone extract a few drops of an aqueous 15% solution of bizmut nitrate, followed by a crystal of potassium hydroxide, immediately, in the presence of mercaptobenzothiazole, the characteristic light red color of the solution occurs, the intensity of which depends on the amount of accelerator in mixture. Example III. The finely crushed vulcanizate is poured with acetone in an amount of about 10 cm8 and carefully heated to boiling. A 20% aqueous solution of bismuth nitrate and potassium hydroxide crystals are added to the acetone extract, after slightly cooling, but in the presence of mercaptobenzothiazole there is a light red color, the intensity of which depends on the amount of accelerator in the mixture. In the quantitative determination, the color intensity of the solution is compared with the formulas containing the correspondingly determined amount of mercaptobenzothiazole disulfide. PL
Claims (1)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| PL36010B1 true PL36010B1 (en) | 1953-04-30 |
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