http://rdf.ncbi.nlm.nih.gov/pubchem/patent/RS-51024-B
Outgoing Links
| Predicate | Object |
|---|---|
| assignee | http://rdf.ncbi.nlm.nih.gov/pubchem/patentassignee/MD5_87e95573670a8a797a29aaee8eb0aebd |
| classificationIPCInventive | http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D305-10 http://rdf.ncbi.nlm.nih.gov/pubchem/patentipc/C07D305-12 |
| filingDate | 2001-05-15-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| inventor | http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_60602215afddb3f0da31810c4d308ab3 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_17fe562f223dd88ded905e900d6da117 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_044dcc67255d773178c595d55179665e http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_21de7d6fa8dbc18e5862fd4cc6794b96 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_849e9b4a36efd6930d59f93333ddb728 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_329f94e92b9e8a6299ff31ab622a0ba3 http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_8b002fc72dab6bef675cfd0c6dfab5ff |
| publicationDate | 2010-10-31-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| publicationNumber | RS-51024-B |
| titleOfInvention | SYNTHESIS OF ALKYL KETEN DIMER FROM STEARINE |
| abstract | Synthesis of alkyl ketene dimer from stearin, which in the first phase involves the production of fatty acid chloride from the natural fatty acid mixture (stearin) by the action of thionyl chloride, and then in the second phase the acid chloride mixture is treated with a suitable catalyst to initiate the elimination of hydrogen chloride and the formation of the corresponding ketene. characterized in that a thionyl chloride COCl2 of technical purity up to 96% is poured into the reactor equipped with a stirrer and reflux equipment and heated to 200 ° C; adding 2kg of fatty acid mixture to each kilogram and stirring for 30-45 minutes, stirring the mixture until clear; that the heating is continued to effect reflux and gas evolution, with reflux continuing for another half hour after the gas has ceased; which, after separation of the gases by distillation, removes the excess thionyl chloride used in the next batch; that the heating is interrupted when the distillate temperature exceeds 100Â ° C; which distillation takes about 30 minutes and is done over a regular column with 2-3 practical floors; which after distillation, the apparatus is connected to a gentle vacuum (90kPa) which gradually increases; which, when the pressure in the apparatus drops to about 2 kPa, the mixture is gradually heated to 100 ° C and kept at that temperature for about half an hour to remove the thionyl chloride residues; bringing a mixture of fatty acid chloride from the previous reaction phase into the reactor equipped with a return condenser, a dosing vessel, a thermometer, a cooling liner, a mixer and a vent, and approximately twice the amount of CH 2 Cl 2 methylene chloride; pouring a solution of triethylamine (C2H5) 3N (0,4kg per kilogram of acyl chloride) in methylene chloride into the dosage vessel; the reaction mixture being reacted in the reactor to an internal temperature of 0-5 ° C; adding the solution from the dispensing vessel with stirring slowly over 1 hour; the reaction being exothermic and the temperature of the mixture being maintained below 10Â ° C by regulating the rate of addition of the solution; forming a voluminous white precipitate of triethylammonium hydrochloride (Et3N HC1) during the reaction; which, upon completion of the addition, stops cooling and stirring is continued for another 24 hours at room temperature; which, after verification, the residue of the free base in the reaction mixture is converted to salt by the addition of HCl; that the reaction mixture is passed through a filter press and subjected to current extraction with water; the organic layer being dried over a molecular sieve 3A or 4A and the solvent removed by distillation under gentle vacuum; that the pre-distilled methylene chloride returns to the process and then the white waxy precipitate lags behind |
| priorityDate | 2001-05-15-04:00^^<http://www.w3.org/2001/XMLSchema#date> |
| type | http://data.epo.org/linked-data/def/patent/Publication |
Incoming Links
Total number of triples: 39.