CS221042B1 - Method of cleaning the 2-mercaptobenzthiazole - Google Patents
Method of cleaning the 2-mercaptobenzthiazole Download PDFInfo
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- CS221042B1 CS221042B1 CS174482A CS174482A CS221042B1 CS 221042 B1 CS221042 B1 CS 221042B1 CS 174482 A CS174482 A CS 174482A CS 174482 A CS174482 A CS 174482A CS 221042 B1 CS221042 B1 CS 221042B1
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Abstract
Spósob čistenia technického 2-merkaptohenztiazolu kryštalizáciou zo zmesi irozpúš- ťadiel etanol, benzen, ktorých hmotnostný ,poměr je 1 ku 0,1 až 1 ku 10. Technický 2-merkaptQbenztlazol sa rozpusta v uvedenej zmesi za tepla, po rozpuštění filtruje a z filtrátu po ochladení vykrystalizuje 2-merkaptobenztiazol, ktorý sa izoluje z matečného luhu. Vynález možno využit pri výrobě čistých chemikálií.A method for purifying technical 2-mercaptohenzothiazole by crystallization from the i-solvent mixture ethanol, benzene, by weight the ratio is 1 to 0.1 to 1 to 10. Technical 2-mercaptobenzothlazole dissolves in said mixture, after dissolution and filtered from the filtrate after cooling 2-mercaptobenzothiazole crystallizes is isolated from the mother liquor. The invention can be used in the production of pure chemicals.
Description
Vynálezom je sposob čistenia technického 2-merkaptobeníztiazolu kryštalizáciou zo zmesi etanolu a benzénu, pričom sa získá '2-merkaptobenztiazol chromatografickej čistoty.The present invention provides a process for purifying technical 2-mercaptobenzothiazole by crystallization from a mixture of ethanol and benzene to obtain 2-mercaptobenzothiazole of chromatographic purity.
2-meirkaptobenztiazol sa vyrába různými spůsobm}.{2 - meircaptobenzothiazole is produced in various ways.
V priemyselnom meradle je najpoužívanejším postupom výroby 2-merkaptobenztiazolu (2-MBT) vysokotlaká reakcia anilínu šo sírouhlíkom a sírou (US pat. 1 631 871, ZSSR pat. 179 306, NSR pat. 1 919 420). Ku vzniku 2-MBT vedu i reakcie difenyltiomočoviny so sírou (US pat. 1 712 968). Další spůsob přípravy 2-MBT je reakcia sírouhlíka s 2,2‘-diaminodifenyldisulfidom (US pat. '1865 477, Fr. pat. 722 942) alebo reakcia sírouhlíka a aminotiofenolom (US pat. 1609 630).On an industrial scale, the most widely used process for the production of 2-mercaptobenzothiazole (2-MBT) is the high pressure reaction of aniline with carbon disulphide and sulfur (US Pat. 1,631,871, USSR Pat. 179,306, Germany Pat. 1,919,420). The reaction of diphenylthiourea with sulfur has also led to the formation of 2-MBT (U.S. Pat. No. 1,712,968). Another method of preparing 2-MBT is by reacting carbon disulphide with 2,2‘-diaminodiphenyldisulfide (US Pat. 1865 477, Fr. Pat. 722 942) or by reacting carbon disulphide and aminothiophenol (US Pat. 1609 630).
Vysokotlakou reakciou anilínu so sírouhlíkom a sírou sa získává 2-MBT o čistotě 90 %, pričom tavenina sa čistí reakciou s NaOH alebo Ca(OH)2 cez sodnú alebo vápenatú sof, alebo v organickom rozpúšťadle, napr. dichlórbenzéne (ZSSR pat. '179 309, AO 122 789, AO 122 790). Takto sa získává technický 2-MBT obsahujúci 92 až 96 o/o hmot. účinnej látky a ktorý sa ďalej nečistí a používá sa ako gumárenský urýchfovaič.By high pressure reaction of aniline with carbon disulfide and sulfur, 2-MBT is obtained with a purity of 90%, the melt being purified by reaction with NaOH or Ca (OH) 2 through a sodium or calcium salt, or in an organic solvent, e.g. dichlorobenzene (USSR Pat. 179,309, AO 122,789, AO 122,790). Technical 2-MBT containing 92 to 96% w / w is thus obtained. of the active substance and which is not further purified and is used as a rubber accelerator.
Podfa AO 168 884 sa rafinuje tavenina 2-merkaptobenztiazolu extrakciou s 2'% až 7% vodným roztokom čpavku v přítomnosti organického rozpúšťadla — s výhodou trichlóretylénu — za súčasnej oxidácie živičnatých podielov peroxidom vodíka v množstve 0,1 až 1 % na vloženu taveninu, pričom sa získává produkt obsahujúci 98,85 percenta hmot. 2-merkaptobenztiazolu s teplotou topenia 178—180 °C.According to AO 168 884, a melt of 2-mercaptobenzothiazole is refined by extraction with a 2% to 7% aqueous ammonia solution in the presence of an organic solvent - preferably trichlorethylene - while oxidizing the bituminous fractions with 0.1 to 1% hydrogen peroxide per melt. yielding a product containing 98.85 percent by weight. 2-mercaptobenzothiazole, m.p. 178-180 ° C.
Nevýhodou dosiaf zaužívaných postupov čistenia je okrem ich pracnosti to, že sa nezískává produkt chromatografickej čistoty.The disadvantage of conventional purification procedures is that, in addition to their labor intensity, the product of chromatographic purity is not obtained.
Zistili sme, že technický 2-merkaptobenztiazol obsahujúci cca 95 % účinnej látky je možné čistit kryštalizáciou zo zmesi rozpúšťadiel etanol-benzén, pričom sa získává 2-merkaptobenztiazol vysokej čistoty.We have found that technical 2-mercaptobenzothiazole containing about 95% active ingredient can be purified by crystallization from ethanol-benzene solvent mixture to obtain 2-mercaptobenzothiazole of high purity.
Podfa vynálezu sa technický 2-merkaptobenztiazol rozpustí za miešania v zmesi rozpúšťadiel etanol-benzén, ktorých hmotnostný poměr je 1 diel etanolu ku 0,1 až 10 dielom benzénu. Výhodné sa pracuje so zmesou rozpúšťadiel etanol : benzen 1 ku 1 až 3.According to the invention, the technical 2-mercaptobenzothiazole is dissolved with stirring in a mixture of ethanol-benzene solvents whose weight ratio is 1 part of ethanol to 0.1 to 10 parts of benzene. Preferably, a 1: 1 to 3 mixture of ethanol: benzene is used.
Rozpúšťanie technického 2-merkaptobenztiazolu v popísaných zmesiach rozpúšťadiel sa uskutočňuje pri zvýšenej teplote, resp. za varu zmesi rozpúšťadiel. Horúci roztok sa filtruje za tepla a 2-merkaptobenztiazol po ochladení kryštalizuje z roztoku. Po izolácii 2-merkaptobenztiazolu sa proces kryštalizácie může opakovat, pričom sa získá 2-MBT vysokej čistoty.The dissolution of the technical 2-mercaptobenzothiazole in the described solvent mixtures is carried out at elevated temperature, respectively. boiling the solvent mixture. The hot solution is filtered hot and 2-mercaptobenzothiazole crystallizes from solution after cooling. After isolation of 2-mercaptobenzothiazole, the crystallization process can be repeated to give 2-MBT of high purity.
Vynález dokumentujú příklady, ktoré však nevyčerpávajú jeho rozsah uplatnenia.The invention is illustrated by examples which, however, do not limit its scope.
PřikladlEXAMPLE
V 200 ml zmesi etanol-benzén (1:3 v hmot. dieloch) sa za varu rozpustilo 30 g technického 2-MBT, obsahujúceho 96 % účinnej látky. Roztok sa za horúca přefiltroval a nechal krystalizovat pri teplote +5 °C počas 12 hodin, pričom sa občas premiešal. Po odfiltrovaní a vysušení sa získalo 19,3 g (64,3 %] 2-merkaptobenztiazolu o čistotě 99,96 %! (stanovené podfa ČSN 666 301, čl. 13).In 200 ml of ethanol-benzene (1: 3 in parts by weight), 30 g of technical 2-MBT containing 96% of the active substance was dissolved by boiling. The solution was filtered hot and allowed to crystallize at + 5 ° C for 12 hours, stirring occasionally. After filtration and drying, 19.3 g (64.3%] 2-mercaptobenzothiazole with a purity of 99.96%! (Determined according to DIN 666 301, Art. 13).
P r í k 1 a d 2Example 1 a d 2
V 100 ml zmesi etanol-benzén (1:1) sa za varu rozpustilo 20 g technického 2-MBT. Roztok sa za horúca přefiltroval a nechal vykrystalizovat. Po kryštalizácii isa získalo20 g of technical 2-MBT was dissolved in 100 ml of ethanol-benzene (1: 1) at boiling point. The solution was filtered hot and allowed to crystallize. After crystallization, isa was obtained
12,4 g (62,0 %) 2-merkaptobenztiazolu o čistotě 99,61 % hmot. (stanovené metodikou ako v příklade č. 1).12.4 g (62.0%) of 2-mercaptobenzothiazole having a purity of 99.61% by weight. (determined by the methodology as in Example 1).
P r í k 1 a d 3 g technického 2-MBT obsahujúceho 94 percent účinnej látky sa za varu rozpustilo v 300 ml zmesi etanol-benzén (1:2 V hmot. dieloch). Po přefiltrovaní horúceho roztoku, jeho ochladení a kryštalizácii sa 'získalo 32,0 g (64,0 %) 2-merkaptobenztiazolu o čistotě 99,72 %.EXAMPLE 3 3 g of technical 2-MBT containing 94 percent of the active compound were dissolved in 300 ml of ethanol-benzene (1: 2 in parts by weight) at boiling point. After filtering the hot solution, cooling and crystallizing, 32.0 g (64.0%) of 2-mercaptobenzothiazole were obtained with a purity of 99.72%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS174482A CS221042B1 (en) | 1982-03-15 | 1982-03-15 | Method of cleaning the 2-mercaptobenzthiazole |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS174482A CS221042B1 (en) | 1982-03-15 | 1982-03-15 | Method of cleaning the 2-mercaptobenzthiazole |
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| CS221042B1 true CS221042B1 (en) | 1983-04-29 |
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| CS174482A CS221042B1 (en) | 1982-03-15 | 1982-03-15 | Method of cleaning the 2-mercaptobenzthiazole |
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1982
- 1982-03-15 CS CS174482A patent/CS221042B1/en unknown
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