CS221005B1 - Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide - Google Patents
Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide Download PDFInfo
- Publication number
- CS221005B1 CS221005B1 CS701081A CS701081A CS221005B1 CS 221005 B1 CS221005 B1 CS 221005B1 CS 701081 A CS701081 A CS 701081A CS 701081 A CS701081 A CS 701081A CS 221005 B1 CS221005 B1 CS 221005B1
- Authority
- CS
- Czechoslovakia
- Prior art keywords
- cyclohexylamine
- water
- organic
- reaction product
- distillation
- Prior art date
Links
Landscapes
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
Matečné roztoky, získané po oddělení N-cyklohexylbenztiazol-2-sulfénamidu z reakčnej zmesi po oxidačněj kondenzácii cyklohexylamínovej soli 2-merkaptobenztiazolu, pripravovanej zo surověj taveniny 2- -merkaptobenztiazolu a přebytku cyklohexylamínu, roztokom chlornanu sodného, sa pri zvýšenej teplote necliajú; rozdeliť na dve vrstvy. Po ich oddělení sa z každej vrstvy ósobitnou destiláciou regeneruje cyklohexylamín. Dosiahne tým lepšie využitie cyklohexylamínu a podstatné zlepšenie kvality odpadových vod.The mother liquors obtained after separation N-cyclohexylbenzthiazole-2-sulfenamide from the reaction mixtures after oxidative condensation 2-mercaptobenzothiazole cyclohexylamine salt, prepared from the crude melt 2- mercaptobenzothiazole and excess cyclohexylamine, sodium hypochlorite solution is added do not shake at elevated temperature; split into two layers. After separating them from each layer Multiple distillation regenerates cyclohexylamine. This will result in a better utilization of cyclohexylamine and substantial improvement in quality wastewater treatment.
Description
Predmetom vynálezu je spósob spracovania matečných roztokov z filtrácie reakčného produktu pri výrobě N-cyklohexylbenztiazol-2-sulfénamidu.It is an object of the present invention to provide a process for treating mother liquors from the filtration of the reaction product to produce N-cyclohexylbenzothiazole-2-sulfenamide.
N-cyklohexylbenztlazol-2-sulfénamid sa používá ako bezpečný urýchlovač vulkanizácie kaučuku. Spósob jeho přípravy je popísaný v československom patente číslo 114 693, v USA patentoch číslo 2 191 657, 2 268 467, 2 762 814, v německých patentoch číslo 855 564 a DAS číslo 1 940 364.N-cyclohexylbenztlazole-2-sulfenamide is used as a safe rubber vulcanization accelerator. A method for its preparation is described in Czechoslovak patent No. 114 693, in US patents 2 191 657, 2 268 467, 2 762 814, in German patents 855 564 and DAS 1 940 364.
Nový technologický postup výroby N-cyklohexylbenztiazol-2-sulfénamidu, ktorým je možné připravit produkt vysokej čistoty je predmetom AO 215 179.A new technological process for the preparation of N-cyclohexylbenzothiazole-2-sulfenamide, by which a high purity product can be prepared, is the subject of AO 215 179.
Podstatou tohoto vynálezu je oxidačná reakcia cyklohexylamínovej soli 2-merkaptobenztiazolu, ktorá vzniká priamou reakciou surového, nerafinovaného produktu vysokotlakovej reakcie anilínu, sírouhlíka a síry s chlórňánom sodným.The present invention relates to the oxidation reaction of the cyclohexylamine salt of 2-mercaptobenzothiazole, which is formed by direct reaction of the crude, unrefined high pressure reaction product of aniline, carbon disulfide and sulfur with sodium hypochlorite.
Postupy na výrobu N-cyklohexylbenztiazol-2-sulfénamidu používané dnes vo svete neregener.ujú cyklohexylamín. Tento odpadá v matečných roztokoch. Okrem toho, že je stratový v značnej miere, zvyšuje toxicitu odpadových vod.The processes for producing N-cyclohexylbenzothiazole-2-sulfenamide used today in the world do not regenerate cyclohexylamine. This is eliminated in the mother liquors. In addition to being highly loss-making, it increases the toxicity of wastewater.
Aby bolo možné zaručit technologický proces po stránke ekonomickéj a tiež po stránke vplyvu na životné prostredie, je potřebné po separácii flnálneho produktu matečné roztoky podrobit destilácli s cielom získat spát cyklohexylamín.In order to guarantee the technological process in economic and environmental terms, it is necessary after distillation of the mother product to undergo distillation in order to recover cyclohexylamine.
Zlstili sme, že regeneráciu cyklahexylamínu z matečných roztokov odpadajúcich z výroby N-cyklohexylbenztiazol-2-sulfénamidu podTa AO 215 179 je možné uskutočniť vo vysokých výťažkoch na principe předkládaného vynálezu.We have found that the recovery of cyclahexylamine from the mother liquors resulting from the production of N-cyclohexylbenzothiazole-2-sulfenamide according to AO 215 179 can be carried out in high yields on the principle of the present invention.
Podstata vynálezu spočívá v tom, že sa matečné roztoky po filtrácii N-cyklohexylbenztiazol-2-sulfénamidu pri jeho výrobě podl'a AO 215 179 1'ahko rozdeTujú na dve vrstvy. Horná vrstva obsahuje prevážnu váčšinu cyklohexylamínu a v ňom rozpustných vedTajších organických látok, ako aj vodu nasýtenú chloridom sodným. Spodná vrstva obsahuje prevážnu váčšinu vody a chloridu sodného, ako aj malý podřel cyklohexylamínu a v ňom rozpustných smolovitých organických látok. Výhodné je matečné roztoky kontinuálně oddělovat a spracovať separátně na kontinuálně pracujúcich destilačných kolonách.The principle of the invention is that the mother liquors are readily separated into two layers after filtration of the N-cyclohexylbenzothiazole-2-sulfenamide in its preparation according to AO 215 179. The top layer contains the major part of cyclohexylamine and its soluble organic substances, as well as water saturated with sodium chloride. The lower layer contains the bulk of water and sodium chloride, as well as a small proportion of cyclohexylamine and pitch-soluble organic substances soluble therein. It is advantageous to separate the mother liquors continuously and to process them separately on continuously operating distillation columns.
Spósob spracovania matečných lúhov podlá vynálezu ilustrujú, ale neobmedzujú následovně příklady.The process of mother liquor treatment according to the invention is illustrated but not limited by the following examples.
Příklad 1Example 1
790 g matečných lúhov po filtrácii N-cyklohexylbenztiazol-2-sulfénamidu, ktoré obsahujú 103 g cyklohexylamínu (CHA), 608 g vody, 61 g chloridu sodného, 13 g smolovitých látok a 5 g rozpustných neidentifikovaných látok sa nechá 15 minút stát v deliacom lieviku pri teplote 60 °C.790 g of mother liquors after filtration of N-cyclohexylbenzothiazole-2-sulfenamide containing 103 g of cyclohexylamine (CHA), 608 g of water, 61 g of sodium chloride, 13 g of pitch and 5 g of soluble unidentified substances are left in a separatory funnel for 15 min. at 60 ° C.
Oddělená spodná fáza obsahujúca 13 g CHA, 498 g vody, 57 g chloridu sodného a 1,2 g smolovitých látok sa destiluje vo varnej banke opatrenej destilačným nástavcom pri atmosferickom tlaku. Teplota odchádzajúcich pár je 93 až 94 °C. Destiluje sa až po dosiahnutie teploty 105 °C vo varnej banke. Destilát obsahuje 12 g CHA a 15 g vody. Zbytok obsahuje 1 g CHA, 483 g vody, 57 g chloridu sodného a 1,2 g smolovitých látok.The separated bottom phase, containing 13 g of CHA, 498 g of water, 57 g of sodium chloride and 1.2 g of pitch, is distilled in a boiling flask equipped with a distillation head at atmospheric pressure. The temperature of the outgoing vapors is 93-94 ° C. Distil until the temperature reaches 105 ° C in a boiling flask. The distillate contains 12 g CHA and 15 g water. The residue contains 1 g CHA, 483 g water, 57 g sodium chloride and 1.2 g pitch.
Vrchná vrstva obsahujúca 90 g cyklohexylamínu, 110 g vody, 5 g chloridu sodného a 11,8 g smolovitých látok sa destiluje na tom istom zariadení ako spodná vrstva pri atmosferickom tlaku. Teplota odcházajúcich pár je 93 až 94 °C. Destiluje sa po dosahnutie teploty 115 °C, vo varnej banke. Destilát obsahuje 88,0 g CHA a 108 g vody. Zbytok obsahuje 0,5 g CHA, 2,0 g vody, 5 g chloridu sodného a 13,3 g smolóvitýcli látok .The top layer containing 90 g of cyclohexylamine, 110 g of water, 5 g of sodium chloride and 11.8 g of pitch is distilled in the same apparatus as the lower layer at atmospheric pressure. The temperature of the outgoing vapors is 93-94 ° C. Distil when the temperature reached 115 ° C, in a boiling flask. The distillate contains 88.0 g CHA and 108 g water. The residue contains 0.5 g CHA, 2.0 g water, 5 g sodium chloride and 13.3 g pitch.
Příklad 2Example 2
Kontinuálně sa spracováva 4390 kg/h matečných lúhov z filtrácie N-cyklohexylbenztiazol-2-sulfénamidu. Matečné lúhy sa predohrejú v trúbkovom výmenníku na teplotu 60 JC. V kontinuálně pracujúcej dejičke dochádza k fázovému deleniu.4390 kg / h of mother liquors from N-cyclohexylbenzothiazole-2-sulfenamide filtration are continuously processed. The mother liquors are first preheated in a tube heat exchanger to a temperature of 60 C. The J continuously operating dejičke of phase separation.
Vrchom deličky preteká 502 kg/h cyklohexylamínu, 611 kg/h vody, 27,6 kg/h Chloridu sodného a 72 kg/h smól. Táto fázá sa nastrekuje do kontinuitne pracujúcej etážovej kolóny. Vo vařáku kolóny sa udržuje teplota 115 °C, na hlavě kolóny 94 až 95 °C. Hlavou kolóny sa získává 495 kg/h cyklohexylamínu, 605 kg/h vody. Spodom kolóny odchádza 3,5 kg/h CHA, 6 kg/h vody, 27,6 kg/h chloridu sodného a 75,5 kg/h smól.502 kg / h of cyclohexylamine, 611 kg / h of water, 27.6 kg / h of sodium chloride and 72 kg / h of pitch flow through the top of the separator. This phase is injected into a continuously operating tray column. A 115 ° C temperature was maintained in the column digester and 94-95 ° C at the top of the column. 495 kg / h of cyclohexylamine, 605 kg / h of water are obtained at the top of the column. At the bottom of the column, 3.5 kg / h of CHA, 6 kg / h of water, 27.6 kg / h of sodium chloride and 75.5 kg / h of pitch are discharged.
Spodná vodná fáza z deličky s prietokoínBottom aqueous phase of the separator with prietokoin
68,5 kg/h cyklohexylamínu, 2766 kg/h vody, 313 kg/h chloridu sodného sa nastrekuje do kontinuitne pracujúcej etážovej kolóny. Vo vařáku kolóny sa udržuje teplota 105 °C na hlavě kolóny 93 až 94 °G. Hlavou kolóny odchádza 66,5 kg/h cyklohexylamínu a 81 kg/h vody. Spodom kolony odchádza 2,0 kg/h cyklohexylamínu, 2685 kg/h vody a 313 kg/ /h chloridu sodného.68.5 kg / h of cyclohexylamine, 2766 kg / h of water, 313 kg / h of sodium chloride are fed to a continuously operating tray column. A column temperature of 105 ° C at the top of the column is maintained at 93-94 ° C. 66.5 kg / h of cyclohexylamine and 81 kg / h of water were passed through the top of the column. 2.0 kg / h of cyclohexylamine, 2685 kg / h of water and 313 kg / h of sodium chloride were passed through the column.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CS701081A CS221005B1 (en) | 1981-09-23 | 1981-09-23 | Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CS701081A CS221005B1 (en) | 1981-09-23 | 1981-09-23 | Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide |
Publications (1)
Publication Number | Publication Date |
---|---|
CS221005B1 true CS221005B1 (en) | 1983-04-29 |
Family
ID=5418422
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CS701081A CS221005B1 (en) | 1981-09-23 | 1981-09-23 | Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide |
Country Status (1)
Country | Link |
---|---|
CS (1) | CS221005B1 (en) |
-
1981
- 1981-09-23 CS CS701081A patent/CS221005B1/en unknown
Similar Documents
Publication | Publication Date | Title |
---|---|---|
DE69705161T2 (en) | Process for the production of bisphenol | |
US2971010A (en) | Production of dicarboxylic acid anhydrides | |
US4990321A (en) | Method for recovering hydrobromic acid and methanol | |
US10214485B2 (en) | Method of reprocessing alkanesulfonic acid | |
DE2814448C2 (en) | ||
EP0270953B1 (en) | Preparation of anhydrous alkanesulfonic acid | |
JP3340068B2 (en) | Improved method for simultaneous production of propylene oxide and styrene monomer | |
FR2467185A1 (en) | PROCESSES FOR SEPARATION AND PURIFICATION OF RESORCINOL AND HYDROQUINONE | |
TWI593665B (en) | Method for producing bisphenol A. | |
US4559110A (en) | Acetophenone recovery and purification | |
US4016047A (en) | Separation and recovery of polychlorinated phenols | |
US20070093662A1 (en) | Method of obtaining 2-mercaptobenzothiazole | |
US2418047A (en) | Process for the removal of carbon disulphide from a hydrocarbon liquid | |
CS221005B1 (en) | Method of preparation of mother solutions from the filtration of reaction product by making the n-cyclohexylbenzthiazole-2-sulphenamide | |
US4125595A (en) | Process for the production of very pure bromine | |
US4192804A (en) | Process for the purification of mercaptobenzothiazole | |
CN108751229B (en) | Method for recovering dicyclohexyl disulfide mother liquor | |
SU843728A3 (en) | Method of producing chlorocyan and hydrogen chloride | |
JP3917201B2 (en) | Method for producing bisphenol A | |
US4215227A (en) | Recovery of para-nitrosodium phenolate | |
TWI481549B (en) | Method for producing sulfur trioxide from recycled sulfuric acid waste material and apparatus for continuous preparing sulfur trioxide | |
DE2628705A1 (en) | PROCESS FOR THE PRODUCTION OF PARTIALLY HALOGENATED ALCOHOLS | |
JP3901334B2 (en) | How to recover phenol | |
JP3883314B2 (en) | How to recover phenol | |
US3154588A (en) | Recovery of acetaldehyde |