Study On The Synthesis And Characterization Of Vitamin K₃

Vitamin K3 is kind of quinone, known as 2-menadinone, 2-methy-1,4-naphthoquinone. It is a important key intermediate in the preparation of the other vitamins of group K. Vitamin K3 is used as a blood coagulating agent, is also used as a feed suppliment of the animal nutrition. In the traditional process,2-menadinone is produced via stochiometric oxidation of 2-methynaphtalene with chromic acid now. However, a great deal of waste water with chromium will be produced in the process and the final product having small amounts of chromium, which is very serious to environment and make an bad effect on humans. Traditional synthesis methods of menadione sodium bisulfite generally had defects, such as big prodution costs, large consumption of raw material, thus, it is very important to research the synthesis method of 2-menadione.We study a enviromentally benign synthetic route used H2O2 oxidation 2-methynaphtalene for 2-menadinone. Mainly, we discussed catalyst and initiator in the reaction process and the effects of reaction temperature, reaction time, amount of initiator, reactant, solvent material ratio and other factors on 2-methylnaphthoquinone yeild were investigated. First, through single factor experiment search activelly range of reaction conditions and get the highest yield of the synthesis method. Finally, use response surface methodology to optimized reaction conditions.Synthesis of 2-methylnaphthoquinone with ammonium persulfate as initiator in the Acetic-H2O2 system by oxidation of 2-methylnaphthalene was researched. The best performences were achieved. The synthesis conditions of 2-methylnaphthoquinone:reaction time 3 h, reaction temperature 85 ?, molar ratio of 2-methylnaphthalene to acetic acid and hydrogen peroxide 1:15:11.5, amount of initiator is 2% of the total amount of reactant. the yelid of 2-methylnaphthoquinone was 54.3%.Synthesis of 2-methylnaphthoquinone with Fe2+ as initiator in the Acetic-H2O2 system by oxidation of 2-methylnaphthalene was researched. The best performences were achieved. The synthesis conditions of 2-methylnaphthoquinone:reaction time 2.5 h, reaction temperature 60 ?, molar ratio of 2-methylnaphthalene to acetic acid and Hydrogen peroxide 1:11:7, amoout of initiator is 1.8% of the to amount of Hydrogen peroxide. The yelid of 2-methylnaphthoquinone was 50.5%.Synthesis of titanium silicalite-1 molecular sieves with different Si/Ti.Synthesis of 2-methylnaphthoquinone with TS-1 as catalyst in the Acetonitrile-H2O2 system. We use response surface methodology to optimized reaction conditions. The best performences were achieved. The synthesis conditions of 2-methylnaphthoquinone:raw material 2 g, solvent amount 20 mL, oxidant amount 16.97 mL, catalyst amount 140 mg, reaction temperature 121.90 ?, reaction time 5.29 h. The yelid of 2-methylnaphthoquinone was 66.66%.We have been improved methods of synthesis sodium bisulfite menadione. The synthesis conditions of menadione sodium bisulfite reaction time 1 h, reaction temperature 45 ?, molar ratio of 2-methylnaphthoquinone to sodium bisulfite 1:1.5. The yelid of menadione sodium bisulfite was 70%.