CN105349252A - Method for separating high-purity rice bran crude oil from rice bran - Google Patents
Method for separating high-purity rice bran crude oil from rice bran Download PDFInfo
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- CN105349252A CN105349252A CN201410411625.7A CN201410411625A CN105349252A CN 105349252 A CN105349252 A CN 105349252A CN 201410411625 A CN201410411625 A CN 201410411625A CN 105349252 A CN105349252 A CN 105349252A
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Abstract
The present invention discloses a method for separating high-purity rice bran crude oil from rice bran. The method comprises: weighing 100 g of puffed rice bran, extracting by using n-hexane as a solvent, sequentially carrying out centrifugation and evaporation to obtain primary pure rice bran crude oil, carrying out film distillation on the primary pure rice bran crude oil raw material at a temperature of 120-130 DEG C under an absolute vacuum of 30-50 Pa to remove water and organic small molecule impurities, carrying out distillation twice to obtain fatty acid, and carrying out distillation twice on the remnants of the two distillations to obtain the high-purity rice bran oil. According to the present invention, the method has characteristics of high physiologically active substance content, low wax content, rice bran oil purity improving, physiologically active substance precipitation reducing during the freezing wax treatment, and complete impurity removing.
Description
Technical field
The invention belongs to oil plant deep process technology field, particularly a kind of method of separating high-purity Rice bran crude oil from rice bran.
Background technology
Rice bran accounts for 5% ~ 5.5% of paddy weight, and Rice plumule accounts for about 2.5%, can extract Rice bran crude oil, obtain the edible rice bran oil with nutrient health-care function through refining from this special oils of rice bran; Rice pollard oil is a kind of nutritious vegetables oil, and unsaturated fatty acid content is high, and oleic acid and linolic acid reach the optimum proportioning of 1:1, is rich in the active skull cap components such as thiaminogen, tocopherol and tocotrienols simultaneously, and edible rear specific absorption reaches more than 90%.
Wax approximately containing 2% ~ 5% in Rice pollard oil, chaff wax is water insoluble, ethanol etc., but to some solvent as normal hexane, Virahol, No. six solvents etc. have the character of hot melt cold analysis, when namely heating, chaff wax is all dissolved in grease; But when the temperature decreases, then can partly or entirely separate out; At present, the solvent extraction method liquefaction that suitability for industrialized production adopts, because temperature is too high, can make most wax and pigment be dissolved in the middle of Rice pollard oil, add consumption and the refining difficulty of refining reagent, have a strong impact on Rice pollard oil quality and nutritive value.
Rice pollard oil traditional extraction technique comprise come unstuck, dewax, depickling, decolouring, the step such as deodorization, but each step can not remove the impurity that will remove completely, therefore the Rice pollard oil obtained is still containing impurity, and tradition extraction Rice pollard oil processing step is many, also has certain influence to the composition of Rice pollard oil; With an organic solvent removal of impurities in traditional technology, this impurity-removing method can not remove impurity completely, and the ether of use has hazardness to operator and environment.
Summary of the invention
Technical problem to be solved by this invention is, overcome the shortcoming of prior art, a kind of method of separating high-purity Rice bran crude oil from rice bran is provided, content of physiologically active substance is high, wax content is low, improve the purity of Rice pollard oil, reduce the precipitation of physiologically active substance during freezing Lasaxing Oilfield, decon can be gone out completely simultaneously.
In order to solve above technical problem, the invention provides a kind of method of separating high-purity Rice bran crude oil from rice bran, specifically comprising the following steps:
(1) take the puffed rice bran of 100g, utilize normal hexane for solvent, be that the puffed rice bran suspension liquid of 1:3-1:5 puts into tool plug Erlenmeyer flask by solid-liquid ratio, put into magnetic stirring apparatus, extraction temperature is 10-30 DEG C, and extraction time is 1-3h;
(2) suspension liquid is placed in explosion protected centrifugal machine, under 3000r/min condition, centrifugal 15min, gets supernatant liquid, pours clear liquid into rotatory evaporator, and bath temperature is 60 DEG C, and rotating speed is 100r/min, evaporation 15min, can obtain just pure Rice bran crude oil;
(3) first pure Rice bran crude oil raw material is carried out thin film distillation under the condition of perfect vacuum 30-50Pa and temperature 120-130 DEG C except anhydrating and organic molecule impurity, distillation residue are carried out twice distillation, first, second distillment is merged, obtains lipid acid;
(4) twice distillation residue allowing step (3) obtain carry out third time molecular distillation, overhead product containing Rice pollard oil obtains the 3rd distillment through the condensation of Rice pollard oil trap, its distillation residuum then carries out the 4th molecular distillation, overhead product containing Rice pollard oil obtains the 4th distillment through the condensation of Rice pollard oil trap, 3rd, the 4th distillment is merged, namely obtains high purity Rice pollard oil.
The technical scheme that the present invention limits further is:
Further, the method of aforesaid separating high-purity Rice bran crude oil from rice bran, the solution of 4-8 % by weight methyl alcohol in sodium hydroxide is added in the 4th the molecular distillation resistates that step (4) obtains, alcoholysis 1 hour is carried out under the condition of temperature 60-80 DEG C, adding the vitriol oil again makes its alcoholysis liquid become acid, carry out esterification, and carry out molecular distillation, distill out fatty acid methyl ester; Then distillation residuum is divided into two-layer after leaving standstill, and lower floor is methanol-water phase layer mutually, adopts Distillation recovery methyl alcohol; Second time molecular distillation is carried out mutually in upper strata, and overhead product is mixed methyl aliphatic ester.
The method of aforesaid separating high-purity Rice bran crude oil from rice bran, dissolve obtaining the residue after mixed methyl aliphatic ester in sodium hydroxide solution with methyl alcohol, pH to 7-8 is regulated until completely dissolved with concentrated sulfuric acid solution, the thick thiaminogen of collecting by filtration, filtrate collection carries out Methanol Recovery, repeat aforesaid operations, obtain thiaminogen.
The method of aforesaid separating high-purity Rice bran crude oil from rice bran, gets the thick thiaminogen of 3-5 weight part, 10-15 weight part NaOH, and 10-20 parts by weight of isopropyl alcohol and 75-85 weight parts water react 2h under temperature 110-120 DEG C with the condition of pressure 0.08MP; Boil off Virahol again, filter, collect filtrate and filter cake, filter cake obtains chaff sterol after drying; By the pH regulator to 7 of filtrate, separate out and obtain pure forulic acid after recrystallization.
The invention has the beneficial effects as follows: the method for a kind of separating high-purity Rice bran crude oil from rice bran designed by the present invention, content of physiologically active substance is high, and wax content is low, improves the purity of Rice pollard oil, reduce the precipitation of physiologically active substance during freezing Lasaxing Oilfield, decon can be gone out completely simultaneously.
Embodiment
embodiment 1
The method of a kind of separating high-purity Rice bran crude oil from rice bran that the present embodiment provides, specifically comprises the following steps:
(1) take the puffed rice bran of 100g, utilize normal hexane for solvent, be that the puffed rice bran suspension liquid of 1:3 puts into tool plug Erlenmeyer flask by solid-liquid ratio, put into magnetic stirring apparatus, extraction temperature is 15 DEG C, and extraction time is 1.5h;
(2) suspension liquid is placed in explosion protected centrifugal machine, under 3000r/min condition, centrifugal 15min, gets supernatant liquid, pours clear liquid into rotatory evaporator, and bath temperature is 60 DEG C, and rotating speed is 100r/min, evaporation 15min, can obtain just pure Rice bran crude oil;
(3) first pure Rice bran crude oil raw material is carried out thin film distillation except anhydrating and organic molecule impurity under the condition of perfect vacuum 30Pa and temperature 120 DEG C, distillation residue are carried out twice distillation, first, second distillment is merged, obtains lipid acid;
(4) twice distillation residue allowing step (3) obtain carry out third time molecular distillation, overhead product containing Rice pollard oil obtains the 3rd distillment through the condensation of Rice pollard oil trap, its distillation residuum then carries out the 4th molecular distillation, overhead product containing Rice pollard oil obtains the 4th distillment through the condensation of Rice pollard oil trap, 3rd, the 4th distillment is merged, namely obtains high purity Rice pollard oil.
Further, the solution of 5 % by weight methyl alcohol in sodium hydroxide is added in the 4th the molecular distillation resistates that step (4) obtains, alcoholysis 1 hour is carried out under the condition of temperature 60 C, adding the vitriol oil again makes its alcoholysis liquid become acid, carry out esterification, and carry out molecular distillation, distill out fatty acid methyl ester; Then distillation residuum is divided into two-layer after leaving standstill, and lower floor is methanol-water phase layer mutually, adopts Distillation recovery methyl alcohol; Second time molecular distillation is carried out mutually in upper strata, and overhead product is mixed methyl aliphatic ester;
Dissolve obtaining the residue after mixed methyl aliphatic ester in sodium hydroxide solution with methyl alcohol, regulate pH to 7, the thick thiaminogen of collecting by filtration with concentrated sulfuric acid solution until completely dissolved, filtrate collection carries out Methanol Recovery, repeats aforesaid operations, obtains thiaminogen;
Get the thick thiaminogen of 3-5 weight part, 10 weight part NaOH, 10 parts by weight of isopropyl alcohol and 75 weight parts waters, at temperature 110 DEG C with the condition of pressure 0.08MP, react 2h; Boil off Virahol again, filter, collect filtrate and filter cake, filter cake obtains chaff sterol after drying; By the pH regulator to 7 of filtrate, separate out and obtain pure forulic acid after recrystallization.
embodiment 2
The method of a kind of separating high-purity Rice bran crude oil from rice bran that the present embodiment provides, specifically comprises the following steps:
(1) take the puffed rice bran of 100g, utilize normal hexane for solvent, be that the puffed rice bran suspension liquid of 1:4 puts into tool plug Erlenmeyer flask by solid-liquid ratio, put into magnetic stirring apparatus, extraction temperature is 20 DEG C, and extraction time is 1-3h;
(2) suspension liquid is placed in explosion protected centrifugal machine, under 3000r/min condition, centrifugal 15min, gets supernatant liquid, pours clear liquid into rotatory evaporator, and bath temperature is 60 DEG C, and rotating speed is 100r/min, evaporation 15min, can obtain just pure Rice bran crude oil;
(3) first pure Rice bran crude oil raw material is carried out thin film distillation except anhydrating and organic molecule impurity under the condition of perfect vacuum 35Pa and temperature 125 DEG C, distillation residue are carried out twice distillation, first, second distillment is merged, obtains lipid acid;
(4) twice distillation residue allowing step (3) obtain carry out third time molecular distillation, overhead product containing Rice pollard oil obtains the 3rd distillment through the condensation of Rice pollard oil trap, its distillation residuum then carries out the 4th molecular distillation, overhead product containing Rice pollard oil obtains the 4th distillment through the condensation of Rice pollard oil trap, 3rd, the 4th distillment is merged, namely obtains high purity Rice pollard oil.
Further, the solution of 6 % by weight methyl alcohol in sodium hydroxide is added in the 4th the molecular distillation resistates that step (4) obtains, alcoholysis 1 hour is carried out under the condition of temperature 70 C, adding the vitriol oil again makes its alcoholysis liquid become acid, carry out esterification, and carry out molecular distillation, distill out fatty acid methyl ester; Then distillation residuum is divided into two-layer after leaving standstill, and lower floor is methanol-water phase layer mutually, adopts Distillation recovery methyl alcohol; Second time molecular distillation is carried out mutually in upper strata, and overhead product is mixed methyl aliphatic ester;
Dissolve obtaining the residue after mixed methyl aliphatic ester in sodium hydroxide solution with methyl alcohol, regulate pH to 7.5, the thick thiaminogen of collecting by filtration with concentrated sulfuric acid solution until completely dissolved, filtrate collection carries out Methanol Recovery, repeat aforesaid operations, obtain thiaminogen;
Get the thick thiaminogen of 4 weight parts, 12 weight part NaOH, 18 parts by weight of isopropyl alcohol and 80 weight parts waters, at temperature 115 DEG C with the condition of pressure 0.08MP, react 2h; Boil off Virahol again, filter, collect filtrate and filter cake, filter cake obtains chaff sterol after drying; By the pH regulator to 7 of filtrate, separate out and obtain pure forulic acid after recrystallization.
Above embodiment is only and technological thought of the present invention is described, can not limit protection scope of the present invention with this, and every technological thought proposed according to the present invention, any change that technical scheme basis is done, all falls within scope.
Claims (4)
1. the method for separating high-purity Rice bran crude oil from rice bran, is characterized in that, specifically comprise the following steps:
(1) take the puffed rice bran of 100g, utilize normal hexane for solvent, be that the puffed rice bran suspension liquid of 1:3-1:5 puts into tool plug Erlenmeyer flask by solid-liquid ratio, put into magnetic stirring apparatus, extraction temperature is 10-30 DEG C, and extraction time is 1-3h;
(2) suspension liquid is placed in explosion protected centrifugal machine, under 3000r/min condition, centrifugal 15min, gets supernatant liquid, pours clear liquid into rotatory evaporator, and bath temperature is 60 DEG C, and rotating speed is 100r/min, evaporation 15min, can obtain just pure Rice bran crude oil;
(3) first pure Rice bran crude oil raw material is carried out thin film distillation under the condition of perfect vacuum 30-50Pa and temperature 120-130 DEG C except anhydrating and organic molecule impurity, distillation residue are carried out twice distillation, first, second distillment is merged, obtains lipid acid;
(4) twice distillation residue allowing step (3) obtain carry out third time molecular distillation, overhead product containing Rice pollard oil obtains the 3rd distillment through the condensation of Rice pollard oil trap, its distillation residuum then carries out the 4th molecular distillation, overhead product containing Rice pollard oil obtains the 4th distillment through the condensation of Rice pollard oil trap, 3rd, the 4th distillment is merged, namely obtains high purity Rice pollard oil.
2. the method for separating high-purity Rice bran crude oil from rice bran according to claim 1, it is characterized in that, the solution of 4-8 % by weight methyl alcohol in sodium hydroxide is added in the 4th the molecular distillation resistates that step (4) obtains, alcoholysis 1 hour is carried out under the condition of temperature 60-80 DEG C, adding the vitriol oil again makes its alcoholysis liquid become acid, carry out esterification, and carry out molecular distillation, distill out fatty acid methyl ester; Then distillation residuum is divided into two-layer after leaving standstill, and lower floor is methanol-water phase layer mutually, adopts Distillation recovery methyl alcohol; Second time molecular distillation is carried out mutually in upper strata, and overhead product is mixed methyl aliphatic ester.
3. the method for separating high-purity Rice bran crude oil from rice bran according to claim 2, it is characterized in that, dissolve obtaining the residue after mixed methyl aliphatic ester in sodium hydroxide solution with methyl alcohol, pH to 7-8 is regulated until completely dissolved with concentrated sulfuric acid solution, the thick thiaminogen of collecting by filtration, filtrate collection carries out Methanol Recovery, repeats aforesaid operations, obtains thiaminogen.
4. the method for separating high-purity Rice bran crude oil from rice bran according to claim 3, it is characterized in that, get the thick thiaminogen of 3-5 weight part, 10-15 weight part NaOH, 10-20 parts by weight of isopropyl alcohol and 75-85 weight parts water, react 2h under temperature 110-120 DEG C with the condition of pressure 0.08MP; Boil off Virahol again, filter, collect filtrate and filter cake, filter cake obtains chaff sterol after drying; By the pH regulator to 7 of filtrate, separate out and obtain pure forulic acid after recrystallization.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602713A (en) * | 2016-03-16 | 2016-05-25 | 河北农苍盛生物科技有限公司 | Millet germ oil and preparation method thereof |
| CN106167738A (en) * | 2016-09-21 | 2016-11-30 | 山东健源油脂科技有限公司 | The rice essential smelting method of high plant sterol |
| CN109338720A (en) * | 2018-08-30 | 2019-02-15 | 无锡德冠生物科技有限公司 | A kind of raw matter scouring agent and preparation method thereof |
-
2014
- 2014-08-21 CN CN201410411625.7A patent/CN105349252A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105602713A (en) * | 2016-03-16 | 2016-05-25 | 河北农苍盛生物科技有限公司 | Millet germ oil and preparation method thereof |
| CN106167738A (en) * | 2016-09-21 | 2016-11-30 | 山东健源油脂科技有限公司 | The rice essential smelting method of high plant sterol |
| CN106167738B (en) * | 2016-09-21 | 2019-07-19 | 山东健源油脂科技有限公司 | The rice essential smelting method of high phytosterol |
| CN109338720A (en) * | 2018-08-30 | 2019-02-15 | 无锡德冠生物科技有限公司 | A kind of raw matter scouring agent and preparation method thereof |
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