Study On Preparation Technology Of High Content Natural ?-Tocopherol

Tocopherol can improve fertility and anti-oxidation and other aspects of significant effect.According to the source of tocopherols,it can be divided into natural tocopherols and synthetic tocopherols.Among them,natural tocopherols are favored by people due to their safe and efficient characteristics.?-tocopherol has the highest biological activity but less content.It can easily be destroyed in the traditional extraction process,therefore the preparation of high purity and high activity of tocopherol has now become the focus of research.In the process of tocopherol extraction,acidic liquid catalysts are widely used.during which there are problems of equipment corrosion,separation difficulties and environmental pollution,which are not in line with the demands of environmental friendly development for society.The solid super acid can effectively solve the problems above.In this paper,a molecular sieve membrane reactor with catalytic function is applied to the tocopherol extraction process,which has the dual function of catalysis and separation,and realizes the coupling between the reaction and the separation process.It improves the efficiency and simplifies the follow-up operation simultaneously which makes contribution to the resources saving.In this paper,the methods of ultrasonic synergy and esterification-saponification combined together are used to remove impurities completely.It's not only easy to operate,but also avoid the use of large-scale expensive equipment.Distillate tocopherols by the use of deodorant while preparing important chemical raw materials---zinc soap.This method achieves the comprehensive utilization of deodorized distillate for broadening the way of the comprehensive utilization of oil which brings new ideas and technical reference for companies.The method of chloromethylation-hydrogenation reduction combined with ion exchange is adopted to convert non-?-tocopherol into ?-tocopherol,increases tocopherol activity the same time increases tocopherol purity and achieves high purity and high activity Preparation of ?-tocopherol.The main conclusions of the method are as follows:(1)Mesoporous molecular sieves MCM-41-1,MCM-41-2,and MCM-41-3 were prepared by two-step synthesis,direct sulfonation and concentrated sulfuric acid impregnation.The BET,XRD,FT-IR and acid strength test were used to characterize and analyze the mesoporous molecular sieve structure parameters.The XRD resultsshowed that the prepared mesoporous molecular sieve possessed the hexagonal pore structure and the structure was stable.The results of FI-IR indicated that not only the typical absorption peak of mesoporous molecular sieve but also the characteristic peak of sulfonic acid group was observed,indicating that the sulfonic acid group was successfully grafted on the surface of mesoporous molecular sieve.Acid strength test results showed that the two-step synthesis of sulfonic acid catalyst MCM-41 belonged to the solid super acid and acid strength is better than the concentrated sulfuric acid impregnation method.(2)The experiment of esterification deodorizer distillate was catalyzed by ultrasonic assisted sulfonic acid type catalyst explored effects of reaction time,material-liquid ratio,reaction temperature,amount of catalyst added and ultrasonic treatment on the esterification reaction rate.The optimal process parameters were as follows: esterification reaction for 2 h,the ratio of material to liquid was 1:3(g / ml),the reaction temperature was 100 ? and the amount of catalyst was 4%.(3)Through esterification control experiment between sulfonic acid type MCM-41 catalyst and liquid catalyst concentrated H2SO4,the sulfonic acid type MCM-41 catalyst is superior to liquid catalyst in terms of catalytic efficiency or considering the loss of tocopherol.The prepared solid catalyst has good stability as well.(4)Through the use of the saponification process to improve the use of ultrasound-assisted extraction of natural mixed tocopherols,while preparing zinc salts.The effects of reaction temperature,amount of alkali,feed ratio,saponification time,alkali addition and ultrasonic power density on the process were investigated experimentally.The best process parameters are listed as follows: The optimal reaction temperature was 75 ?,the excess alkali was 1.02 times of saponification value;the ratio of material to liquid was 1:4(g / ml);the saponification time was 1.5h;the alkali was added in three times;the optimization of response surface showed that the reaction time was 58 min;the ultrasonic power density was 0.93(w / ml)and the ratio of material to liquid was 1:3.8(g / ml).The extraction yield of tocopherol was up to 93.22%;tocopherol purity was 56.32% Zinc soap fatty acid content of 0.37%.which are all in line with the first level standard.(5)The method of chloromethyl-hydrogenation reduction of natural mixed tocopherols in non-?-tocopherol into ?-tocopherol,increases tocopherol activity.The effects of solvent selection,catalyst dosage,solid-liquid ratio,chloromethylation temperature and hydrogenation reduction time on the process were analyzed.Theoptimum experimental conditions were as follows: using ethyl acetate as solvent,the catalyst material was 6% of the material,the ratio of material to liquid was about 1:5,the temperature of chloromethylation was 50 ?,and the hydrogenation reduction time was 4 h.Chloromethyl-reduction method is difficult to control the intermediate products,resulting in ?-tocopherol purity is not high.The use of strong base anion exchange resin ion exchange can effectively achieve the ?-tocopherol purification.Obtained purity of 80.32% ?-tocopherol,extraction rate of 53.28%,realizing the preparation of high purity and high activity ?-tocopherol.