CN110862872A - Method for preparing MCT oil by using coconut oil - Google Patents
Method for preparing MCT oil by using coconut oil Download PDFInfo
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- CN110862872A CN110862872A CN201911150035.2A CN201911150035A CN110862872A CN 110862872 A CN110862872 A CN 110862872A CN 201911150035 A CN201911150035 A CN 201911150035A CN 110862872 A CN110862872 A CN 110862872A
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- 239000003921 oil Substances 0.000 title claims abstract description 60
- 235000019198 oils Nutrition 0.000 title claims abstract description 60
- 235000019864 coconut oil Nutrition 0.000 title claims abstract description 37
- 239000003240 coconut oil Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 19
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 142
- 235000011187 glycerol Nutrition 0.000 claims abstract description 50
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims abstract description 35
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 claims abstract description 33
- 235000014113 dietary fatty acids Nutrition 0.000 claims abstract description 33
- 239000000194 fatty acid Substances 0.000 claims abstract description 33
- 229930195729 fatty acid Natural products 0.000 claims abstract description 33
- 150000004665 fatty acids Chemical class 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229960002446 octanoic acid Drugs 0.000 claims abstract description 17
- 239000005635 Caprylic acid (CAS 124-07-2) Substances 0.000 claims abstract description 16
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- CMDGQTVYVAKDNA-UHFFFAOYSA-N propane-1,2,3-triol;hydrate Chemical compound O.OCC(O)CO CMDGQTVYVAKDNA-UHFFFAOYSA-N 0.000 claims description 16
- 239000003054 catalyst Substances 0.000 claims description 13
- 238000001816 cooling Methods 0.000 claims description 13
- 238000004821 distillation Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- FBUKVWPVBMHYJY-UHFFFAOYSA-N nonanoic acid Chemical compound CCCCCCCCC(O)=O FBUKVWPVBMHYJY-UHFFFAOYSA-N 0.000 claims description 9
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims description 8
- 238000005886 esterification reaction Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 230000001877 deodorizing effect Effects 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000004042 decolorization Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229940098779 methanesulfonic acid Drugs 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- 229910052725 zinc Inorganic materials 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000004519 grease Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 238000005194 fractionation Methods 0.000 description 9
- 238000001704 evaporation Methods 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 230000008020 evaporation Effects 0.000 description 5
- 230000003301 hydrolyzing effect Effects 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000009874 alkali refining Methods 0.000 description 4
- 239000000706 filtrate Substances 0.000 description 4
- GYSCBCSGKXNZRH-UHFFFAOYSA-N 1-benzothiophene-2-carboxamide Chemical compound C1=CC=C2SC(C(=O)N)=CC2=C1 GYSCBCSGKXNZRH-UHFFFAOYSA-N 0.000 description 3
- -1 C12 carbon fatty acid Chemical class 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000010779 crude oil Substances 0.000 description 2
- 238000004332 deodorization Methods 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000015112 vegetable and seed oil Nutrition 0.000 description 2
- 239000008158 vegetable oil Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 239000005639 Lauric acid Substances 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000011085 pressure filtration Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/02—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils
- C11C1/04—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids from fats or fatty oils by hydrolysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/08—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils with fatty acids
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of special grease synthesis, and particularly relates to a method for preparing MCT oil by using coconut oil. The coconut oil is hydrolyzed to obtain mixed fatty acid and glycerin water, then the mixed fatty acid is treated to obtain caprylic acid and capric acid, the glycerin water is treated to obtain glycerin, and finally the caprylic acid and capric acid are reacted with the glycerin to obtain MCT oil. The invention only takes the coconut oil as the raw material, and synthesizes MCT oil by using the hydrolyzed effective components, and the MCT oil produced by the process has the advantages of lower cost, reasonable yield and guaranteed quality.
Description
Technical Field
The invention belongs to the field of special grease synthesis, and particularly relates to a method for preparing MCT oil by using coconut oil.
Background
MCT oil is medium-chain fatty acid glyceride. MCT oil is colorless transparent liquid at room temperature, slightly has the fragrance of coconut oil, belongs to derivatives of coconut oil or palm oil, has small relative molecular weight and good water solubility due to short carbon chain, is a few oil bodies which can be mutually dissolved with water, has no harm to tissues such as human skin and the like, has low melting point (-15 ℃), high boiling point, small density and low viscosity which is about 50 percent of that of common vegetable oil. The MCT oil has extremely low unsaturated fatty acid content, iodine value of not more than 0.5, excellent physical and chemical properties compared with vegetable oil and animal oil, extremely high antioxidant temperature and extremely low crystallization resistance, excellent carrier for biological preparation and chemical synthetic medicine, small surface tension and easy diffusion of medicine, so that the MCT oil has wide application value. The existing MCT oil production process is mostly controlled by America and European companies, the production process cost is high, the production formula is confidential, and the implementation is difficult.
Disclosure of Invention
The invention aims to provide a method for preparing MCT oil from coconut oil, which has wide raw material source and simple and controllable preparation process.
The technical scheme adopted by the invention is as follows:
a method for preparing MCT oil from coconut oil comprises hydrolyzing coconut oil to obtain mixed fatty acid and glycerol water, treating the mixed fatty acid to obtain caprylic acid and capric acid, treating the glycerol water to obtain glycerol, and reacting caprylic acid, capric acid and glycerol to obtain MCT oil.
When coconut oil is hydrolyzed, methanesulfonic acid with the mass of 5% of coconut oil and concentrated sulfuric acid with the mass of 10% (98 wt%) are added as catalysts, and the mixture is hydrolyzed at the temperature of 80-85 ℃ for 18-20h at the oil-water ratio of 1:1.5 to obtain mixed fatty acid and glycerol water.
Fractionating the mixed fatty acid to obtain caprylic acid and capric acid.
The mixed fatty acid is rich in caprylic acid and capric acid, wherein caprylic acid accounts for about 9.6% of total fatty acids, capric acid accounts for about 6.3% of total fatty acids, and the crude fatty acid can be fractionated to obtain high-quality caprylic acid and capric acid.
Purifying, evaporating and desalting the glycerin water to obtain crude glycerin.
Further, the crude glycerol is treated under the distillation pressure of 360Pa and at the temperature of 161.5 ℃ to obtain pure glycerol with the concentration of 98.5 percent, and then active carbon is added for decolorization to obtain refined glycerol.
Further, crude MCT oil is first obtained by reacting caprylic acid, capric acid and glycerol: mixing glycerol and caprylic-capric acid according to the mass ratio of 1:5.5, carrying out esterification reaction under the action of a catalyst, wherein the initial reaction temperature is 140 ℃, the initial vacuum is 3kPa, slowly heating up to 260 ℃ at the speed of 15 ℃/h during stirring, then adjusting the vacuum to 1kPa, keeping the temperature, continuing to react for 1-1.5h, and cooling to 60-70 ℃ to obtain crude MCT oil.
The catalyst comprises the following components in percentage by mass: 30-40% of zinc chloride, 50-60% of zinc sulfate and 10-12% of zinc; the addition amount of the catalyst is 3-5% of the total mass of the glycerol and the caprylic-capric acid
Preferably, the glycerol is preheated to 120-130 ℃ and then mixed with the caprylic-capric acid.
The crude MCT oil obtained was purified as follows: filtering the crude MCT oil, adding alkali liquor, stirring for 40-50min, centrifuging, washing the collected light liquid with water, decolorizing, and deodorizing to obtain refined MCT oil.
The water washing process comprises the following steps: washing with water for 1-2 times, wherein the water addition amount is 10-15% of MCT oil each time, and stirring for 15-20 min.
Stirring at 95-98 deg.C under vacuum 3kPa for 0.5h before decolorizing, adding 0.3-1% of MCT oil by weight of activated carbon, decolorizing at 115-120 deg.C under vacuum 2660Pa, and stirring for 40 min.
Decolorizing, filtering, separating to remove gas, deodorizing at 240 deg.C under vacuum 800Pa for 90min, and cooling to 40 deg.C to obtain refined MCT oil.
Specifically, the method for preparing MCT oil by using coconut oil comprises the following steps:
1) hydrolysis: using refined coconut oil as a raw material, using methanesulfonic acid with the mass of 5% of oil and concentrated sulfuric acid with the mass of 10% (98%) as a catalyst, and hydrolyzing for 20 hours at 80 ℃ with an oil-water ratio (mass ratio) of 1:1.5 to obtain crude fatty acid and glycerol water;
2) fractionating crude fatty acid to obtain caprylic acid and capric acid: the obtained crude fatty acid is fractionated under negative pressure, the fractionation pressure is 360Pa, and the fractionation temperature is 121.5 ℃ to obtain caprylic acid; the fractionation pressure is 360Pa, and the fractionation temperature is 143.3 ℃ to obtain the decanoic acid;
3) obtaining glycerol from glycerol water: purifying, evaporating and desalting the glycerol water obtained in the step 1) to obtain crude glycerol with the mass content of 80%, distilling the crude glycerol at the distillation pressure of 360Pa and the temperature of 161.5 ℃ to obtain pure glycerol with the mass content of 98.5wt%, and adding activated carbon for decoloring to obtain refined glycerol;
4) mixing glycerol and caprylic-capric acid at a ratio of 1:5.5, carrying out esterification reaction, wherein the initial reaction temperature is 140 ℃, the initial vacuum is 3kPa, slowly heating up to 260 ℃ at a speed of 15 ℃/h during stirring, then regulating the vacuum to 1kPa, keeping the temperature, continuing to react for 1-1.5h, and cooling to 60-70 ℃ to obtain the crude MCT oil. And refining the crude MCT oil by alkali refining, decoloring by active carbon, deodorizing, cooling and finely filtering to obtain refined MCT oil.
Has the advantages that:
the method comprises the steps of obtaining caprylic acid and capric acid by using mixed fatty acid obtained by hydrolyzing coconut oil through a fractionation process, obtaining crude glycerol by using glycerol water obtained by hydrolyzing coconut oil through purification, evaporation and desalination, heating the crude glycerol and caprylic/capric acid for esterification reaction by using the refined glycerol, adding a catalyst to obtain crude MCT oil, refining the crude MCT oil through alkali refining, decoloring the activated carbon, deodorizing, cooling and fine filtering to obtain the refined MCT oil. The method has the innovation that only the coconut oil is taken as the raw material, and the MCT oil is synthesized by the hydrolyzed effective components, so that the MCT oil produced by the process has the advantages of low cost and reasonable yield, the yield of the MCT oil is 13-14% of that of the coconut oil, and the quality is ensured.
Detailed Description
The technical solution of the present invention is illustrated by the following specific examples, but the scope of the present invention is not limited thereto:
example 1
1) Coconut oil hydrolysis: adding soft water into refined coconut oil (the temperature is preheated to 90-95 ℃), wherein the mass ratio of oil to water is 1:1.5, and adding methanesulfonic acid, wherein the adding amount is 5% of the weight of the coconut oil; then adding 98wt% of concentrated sulfuric acid, wherein the adding amount is 10% of the weight of the coconut oil. Controlling the hydrolysis temperature at 80-85 deg.C, stopping heating when the hydrolysis time reaches 10h, standing for 40min, and placing glycerol water into water distribution tank. Then the processes of adding water, adding acid, adding catalyst and secondary hydrolysis are repeated, and the operation is the same as that of the primary hydrolysis. Then washing the fatty acid twice with soft water (preheated to 80-85 deg.C) with the water amount of 30-40% of the oil amount. Degassing the fatty acid, and placing the fatty acid into a crude fatty acid tank for fractionation; the hydrolysis rate after the secondary hydrolysis is not less than 92 percent.
2) Fatty acid fractionation: heating the crude fatty acid, raising the temperature to 95 ℃, then carrying out gas evolution, cooling the gas evolved, and discharging the gas into a light fraction tank (first fraction), wherein the gas evolution pressure is 360 Pa. Heating the temperature of the crude fatty acid after gas separation to 160.2 ℃ for first fractionation, and obtaining light fraction fatty acid, cooling and temporarily storing the light fraction fatty acid at the fractionation pressure of 360 Pa. Heating the light fraction (C8/C10/C12 carbon fatty acid), heating to 143.3 deg.C, fractionating at 360Pa, cooling the light fraction fatty acid (C8/C10 carbon fatty acid), and storing temporarily. The heavy fraction C12 fatty acid is recovered after cooling. Heating light fraction fatty acid (C8/C10 carbon fatty acid) to 121.2 deg.C, fractionating at 360Pa to obtain light fraction C8 fatty acid; and (4) performing heat exchange and cooling on the heavy fraction C10 fatty acid to obtain the finished product decanoic acid. By fractional distillation, octanoic acid (C8 acid), decanoic acid (C10 acid) and lauric acid (C12 acid) are obtained.
3) Preparing refined glycerol from glycerol water: hydrolyzing glycerol water generated from coconut oil, keeping the temperature of the solution at 80-85 deg.C, adding lime milk to adjust the pH value of the solution to 7.5-8, stirring with steam for 30min, and press filtering to obtain clear filtrate; FeCl is added3Adding the solution, maintaining the temperature at 50-60 deg.C, adjusting pH to 3.8-4.2, and stirring with air for 20-30 min. And (3) performing pressure filtration, and performing alkali washing on the obtained filtrate: adding sodium carbonate (5%) solution under vacuum to adjust pH to 9-9.5, maintaining the solution at 78-82 deg.C, steam stirring for 30min, and stopping heating. And (5) performing filter pressing, wherein the clear filtrate is the purified glycerol water. Testing the PH value of the purified glycerol water to be between 9 and 9.5, heating the glycerol water to about 100 ℃, performing normal pressure evaporation to obtain the glycerol with the concentration of about 75 to 80 percent, and then sequentially performing vacuum evaporation (double-effect evaporation) and triple-effect evaporation to obtain crude glycerol with the concentration of more than 92 percent, wherein salt is added during the double-effect and triple-effect evaporation. Heating the crude glycerol to 75-80 ℃, continuing to heat to 105-115 ℃, carrying out gas evolution, continuing to heat to 170 ℃, and entering the first distillation tower. The distillation vapor rises to the top of the tower and enters a cooler, the distillation vapor is condensed into glycerol liquid, the glycerol liquid flows back to the lower part of the second distillation tower and is circularly heated and fractionated at the temperature of 170 ℃; the distillation steam rises to the top of the tower and enters a cooler, the distillation steam is condensed into glycerol liquid, the glycerol liquid flows back to the upper part of the distillation tower and overflows to a glycerol temporary storage tank from an overflow port above an upper partition plate. Pumping glycerol liquid into heater, heating to 80-90 deg.C, adding into decolorizing tank, stirring for 90min, adding decolorizing agent active carbon 0.3% of glycerol weight, pumping into filter press, and separating to obtain filtrate as essenceGlycerin with a glycerin content of more than 95%.
4) Preparing MCT through esterification: after the glycerol is preheated to about 120 ℃, the glycerol and the caprylic-capric acid are efficiently mixed according to the proportion and are subjected to esterification reaction to prepare MCT crude oil, the initial reaction temperature is 140 ℃, the initial vacuum is 3kPa, the stirring and the slow temperature rise are carried out, the temperature rises to 260 ℃ (the speed of 15 ℃/h) after the reaction is carried out for 8 hours, the vacuum is adjusted to 1kPa, the heating is stopped, the stirring is carried out for 1 hour, then the cooling is carried out to 60-70 ℃, and the MCT crude oil enters a crude MCT tank. The mass percentage of the catalyst added in the esterification reaction is as follows: 35% of zinc chloride, 55% of zinc sulfate and 10% of zinc; the addition amount of the catalyst is 4 percent of the total mass of the glycerol and the caprylic-capric acid, and the esterification rate is more than 90 percent.
5) And (3) MCT refining: filtering crude MCT, alkali refining in refining pot (adding NaOH solution), stirring for 45min, separating MCT oil with tubular centrifuge, adding fructus Gleditsiae Abnormalis in fructus Gleditsiae Abnormalis tank, and returning light liquid to refining tank. After alkali refining, washing twice with water, wherein the water addition amount is 10% of MCT each time, and stirring time is 20 min. After washing, pumping MCT oil into a decolorizing tank, heating and drying at 95-98 deg.C under vacuum of 3kPa for about 0.5 h. Then adding activated carbon which is 0.5 percent of the weight of the MCT oil, decoloring at the temperature of 115 ℃ and 120 ℃, and stirring and decoloring for 40min under the vacuum of 2660 Pa. And pumping the mixed liquor into a leaf filter, performing fine filtration on the filtered clear liquor, then feeding the filtered clear liquor into a gas separator, pumping the filtered clear liquor into a heater, heating the filtered clear liquor, and feeding the heated clear liquor into a deodorization tower. Deodorizing at 240 deg.C under vacuum of 800Pa for 90 min. After the deodorization is finished, the mixture is pumped into a cooler to be cooled to 40 ℃, and the refining yield of the MCT oil is 96%. The detection shows that the melting point of the product is-15 ℃, and the acid value is 0.2 mgKOH/g.
Claims (9)
1. A method for preparing MCT oil by using coconut oil is characterized in that coconut oil is hydrolyzed to obtain mixed fatty acid and glycerol water, then the mixed fatty acid is treated to obtain caprylic acid and capric acid, the glycerol water is treated to obtain glycerol, and finally the caprylic acid, capric acid and glycerol are reacted to obtain the MCT oil.
2. A process for the preparation of MCT oil from coconut oil as claimed in claim 1 wherein crude MCT oil is obtained by reacting caprylic acid, capric acid and glycerol: mixing glycerol and caprylic-capric acid according to the mass ratio of 1:5.5, carrying out esterification reaction under the action of a catalyst, wherein the initial reaction temperature is 140 ℃, the initial vacuum is 3kPa, slowly heating up to 260 ℃ at the speed of 15 ℃/h during stirring, then adjusting the vacuum to 1kPa, keeping the temperature, continuing to react for 1-1.5h, and then cooling to 60-70 ℃ to obtain crude MCT oil; the catalyst comprises the following components in percentage by mass: 30-40% of zinc chloride, 50-60% of zinc sulfate and 10-12% of zinc; the addition amount of the catalyst is 3-5% of the total mass of the glycerol and the caprylic-capric acid.
3. A process for the preparation of MCT oil from coconut oil as claimed in claim 2 where the glycerin is preheated to 120-130 ℃ before being mixed with caprylic acid and capric acid.
4. A process for the preparation of MCT oil from coconut oil as claimed in claim 2, wherein the crude MCT oil obtained is purified as follows: filtering the crude MCT oil, adding alkali liquor, stirring for 40-50min, centrifuging, washing the collected light liquid with water, decolorizing, and deodorizing to obtain refined MCT oil.
5. The method for preparing MCT oil by using coconut oil as claimed in claim 4, wherein the water is added for 1-2 times, the amount of water added for each time is 10-15% of the MCT oil, and the stirring time is 15-20 min.
6. The method for preparing MCT oil from coconut oil as claimed in claim 4, wherein the MCT oil is stirred for 0.5h at 95-98 ℃ and under vacuum 3kPa before decolorization, and then activated carbon with the weight of 0.3-1% of that of the MCT oil is added, the decolorization temperature is 115-120 ℃, the decolorization vacuum is 2660Pa, and the stirring decolorization is 40 min.
7. The process for preparing MCT oil using coconut oil as claimed in claim 4, wherein refined MCT oil is obtained by filtering and separating to remove gas after decolorizing, deodorizing at 240 ℃ under vacuum 800Pa for 90min, and cooling to 40 ℃.
8. A process for preparing MCT oil from coconut oil as claimed in any one of claims 1-7, wherein during the hydrolysis of coconut oil, methanesulfonic acid 5% by mass of coconut oil and concentrated sulfuric acid 10% by mass of coconut oil at 98% concentration are added as catalysts, and the mixture is hydrolyzed at 80-85 ℃ for 18-20h at an oil-water ratio of 1:1.5 to obtain crude fatty acid and glycerol water.
9. The process for preparing MCT oil from coconut oil as claimed in claim 8, wherein the glycerol is purified, evaporated, desalted to obtain crude glycerol, the crude glycerol is treated at distillation pressure of 360Pa and temperature of 161.5 ℃ to obtain pure glycerol, and then activated carbon is added to decolorize to obtain refined glycerol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911150035.2A CN110862872A (en) | 2019-11-21 | 2019-11-21 | Method for preparing MCT oil by using coconut oil |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050208179A1 (en) * | 2004-03-18 | 2005-09-22 | Albrecht Daniel S | Nutritional formula containing select carotenoid combinations |
| CN102559390A (en) * | 2011-12-21 | 2012-07-11 | 南昌大学 | Preparation method of medium-chain polyglycerol fatty acid ester |
| CN108383722A (en) * | 2018-03-14 | 2018-08-10 | 河南工业大学 | A kind of method of preparation of industrialization middle chain triglyceride |
| CN109836328A (en) * | 2019-03-16 | 2019-06-04 | 广州隽沐生物科技股份有限公司 | The synthetic method of median chain triglyceride oil |
-
2019
- 2019-11-21 CN CN201911150035.2A patent/CN110862872A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050208179A1 (en) * | 2004-03-18 | 2005-09-22 | Albrecht Daniel S | Nutritional formula containing select carotenoid combinations |
| CN102559390A (en) * | 2011-12-21 | 2012-07-11 | 南昌大学 | Preparation method of medium-chain polyglycerol fatty acid ester |
| CN108383722A (en) * | 2018-03-14 | 2018-08-10 | 河南工业大学 | A kind of method of preparation of industrialization middle chain triglyceride |
| CN109836328A (en) * | 2019-03-16 | 2019-06-04 | 广州隽沐生物科技股份有限公司 | The synthetic method of median chain triglyceride oil |
Non-Patent Citations (2)
| Title |
|---|
| FEREIDOON SHAHIDI主编，王兴国等主译: "《贝雷油脂化学与工艺学 第6卷 油脂的工业产品与非食用产品 第6版》", 中国轻工业出版社, pages: 210 - 213 * |
| 夏秋瑜等: "中碳链脂肪酸甘油三酯的研究进展", 《食品研究与开发》, no. 07, 5 July 2007 (2007-07-05), pages 150 - 153 * |
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