CN111875657A - Deodorized distillate suitable for biological enzyme esterification reaction and preparation method thereof - Google Patents
Deodorized distillate suitable for biological enzyme esterification reaction and preparation method thereof Download PDFInfo
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- CN111875657A CN111875657A CN202010759361.XA CN202010759361A CN111875657A CN 111875657 A CN111875657 A CN 111875657A CN 202010759361 A CN202010759361 A CN 202010759361A CN 111875657 A CN111875657 A CN 111875657A
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Abstract
The invention relates to the technical field of biochemical engineering, in particular to deodorized distillate suitable for biological enzyme esterification reaction and a preparation method thereof, wherein the acid value of the deodorized distillate is below 120mg/g, the saponification value is below 160mg/g, the VE content is below 10%, and the sterol content is below 12%; according to the invention, by mixing and compounding the DD oil raw materials with different physical and chemical parameters, the acid value, saponification value, VE content and sterol content of the DD oil meet the actual application requirements of extracting sterol by biological enzyme esterification, the esterification time is shortened, the sterol extraction rate is improved, the production cost is saved, and the method is suitable for further popularization and application.
Description
Technical Field
The invention relates to the technical field of biochemical engineering, in particular to deodorized distillate suitable for biological enzyme esterification reaction and a preparation method thereof.
Background
The vegetable oil deodorized distillate (DD oil) is rich in natural vitamin E and phytosterol, and is an excellent raw material for preparing the natural vitamin E and the phytosterol. The method for extracting the phytosterol from the vegetable oil deodorized distillate (DD oil) through biological enzyme esterification has the advantages of mild operation conditions, strong selectivity, small damage to active substances, environmental friendliness and the like, and is a development direction for resource high-value utilization of the vegetable oil deodorized distillate. However, not all DD oils are suitable for bio-enzymatic esterification to extract phytosterols. The acid value, saponification value, VE content and sterol content in the DD oil raw material have great influence on the extraction of sterol by biological enzyme esterification. If the DD oil raw material is not blended, the effect of extracting sterol by biological enzyme esterification is influenced, the methanol dosage is increased, the extraction rate of phytosterol is reduced, the product quality is reduced, and the production cost is increased.
Disclosure of Invention
In view of the above problems, the present invention provides a deodorized distillate suitable for biological enzyme esterification reaction.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a deodorized distillate suitable for biological enzyme esterification reaction, wherein the acid value of the deodorized distillate is below 120 mg/g.
Further, the saponification value of the deodorized distillate is 160mg/g or less.
Further, the VE content of the deodorized distillate is below 10%.
Further, the sterol content of the deodorized distillate is below 12%.
The invention further provides a preparation method of the deodorized distillate suitable for the biological enzyme esterification reaction, which comprises the following steps:
s1: detecting physical and chemical parameters of different types of deodorized distillate raw materials;
s2: mixing different kinds of deodorized distillate raw materials according to a certain proportion, and making the physicochemical parameters of the mixed deodorized distillate meet the requirements that the acid value is below 120mg/g, the saponification value is below 160mg/g, the VE content is below 10% and the sterol content is below 12%.
Further, the physicochemical parameters to be detected for the different types of deodorized distillates in S1 include acid value, saponification value, VE content and sterol content.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, by mixing and compounding the DD oil raw materials with different physical and chemical parameters, the acid value, saponification value, VE content and sterol content of the DD oil meet the actual application requirements of extracting sterol by biological enzyme esterification, the esterification time is shortened, the sterol extraction rate is improved, and the production cost is saved. The acid value of the DD oil raw material is prepared to be below 120mg/g, so that the esterification time can be shortened, the methanol dosage can be reduced, and the cost can be saved; the saponification value of the blended DD oil raw material is below 160mg/g, the VE content is below 10%, and the sterol content is below 12%, so that the extracted crude sterol content can be improved; in addition, the blending method of the invention has convenient operation and wide application, and is suitable for further popularization and application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the acid value of the deodorized distillate in the embodiment is below 120 mg/g; more preferably, the acid value is between 60 and 100 mg/g.
The preparation method of the deodorized distillate comprises the following steps:
s1: detecting physicochemical parameters such as acid value, saponification value, VE content and sterol content of different types of deodorized distillate (DD oil) raw materials; wherein the deodorized distillate is preferably deodorized distillate of vegetable oil such as soybean oil, oleum Rapae, oleum Arachidis Hypogaeae, oleum Helianthi, and palm oil.
S2: mixing different types of deodorized distillate raw materials according to a certain proportion, and making the physicochemical parameters of the mixed deodorized distillate meet the requirement that the acid value is below 120 mg/g. (the main principle is that the acid value of the mixed DD oil reaches the requirement below 120mg/g by mixing different DD oil according to different physical and chemical parameters)
The process for extracting the sterol by using the deodorized distillate (DD oil) comprises the following steps:
adding 3% of water into DD oil, adding alkali liquor to adjust the pH to about 7, adding a proper amount of methanol (the methanol is added according to the content of fatty acid) and biological enzyme (model Lipozyme TL IM), stirring at normal temperature, carrying out biological enzyme esterification reaction, and stopping the reaction when the acid value in the system is measured to be less than 5; and (3) carrying out cold precipitation on the mixed solution at a low temperature (15 ℃) for 24 hours, and filtering to obtain the sterol.
The methanol dosage and the reaction time of the DD oil with different acid values are shown in the following table:
as can be seen from the table above, when the acid value of DD oil is 80mg/g and 100mg/g, the esterification reaction time is substantially consistent with the methanol dosage, and when the acid value is more than 120mg/g, the esterification reaction time and the methanol dosage are both obviously increased, and the production cost is increased. Specifically, when the acid value is 83.5mg/g, the esterification time is 24 hours, the acid value is reduced to 4.78mg/g, and the dosage of methanol is 53 g. The acid value is 98.7mg/g, the esterification time is 24 hours, the acid value is reduced to 4.49mg/g, and the dosage of methanol is 55 g. When the acid value is 121.5mg/g, the esterification time is 26 hours, the acid value is reduced to 4.74mg/g, and the dosage of the methanol is 70 g. (acid value refers to the number of milligrams of potassium hydroxide required for neutralizing free fatty acid in 1g of grease, reflecting the content of the free fatty acid.methanol is a reaction substrate and reacts with the fatty acid to generate methyl ester of the fatty acid and reduce the acid value under the action of a catalyst.)
Example 2:
the deodorized distillate of this example was substantially the same as example 1 except that the saponification value of the deodorized distillate was 160mg/g or less; more preferably, the saponification number is between 100 and 160 mg/g.
The method for preparing deodorized distillate is the same as that in example 1, and the saponification value of the DD oil is below 160 mg/g.
The process for extracting sterols from deodorized distillate (DD oil) was the same as in example 1.
The crude sterol content of the different saponification values DD oil extractions is shown in the table below:
as can be seen from the above table, when the saponification value of DD oil is more than 160mg/g, the extraction rate of phytosterol is reduced. Specifically, when the saponification value is 143.5mg/g, the content of crude sterol extracted is 62.4%. When the saponification value is 161.8mg/g, the content of the extracted crude sterol is 67.8%. When the saponification value is 184.7mg/g, the extracted crude sterol content is 47.1%, and the sterol content in the filtrate is 2.65% and the extraction is incomplete. (the saponification number is the number of milligrams of potassium hydroxide required to saponify 1g of oil under the prescribed conditions, and is the determination of the free fatty acid and glyceride content in the oil and fat.)
Example 3:
the deodorized distillate in this example was essentially the same as in example 2, except that the VE content of the deodorized distillate was below 10%; more preferably, the VE content is between 2 and 10%.
The preparation method of the deodorized distillate is the same as that of example 2, and the VE content of the prepared DD oil is below 10%.
The process for extracting sterols from deodorized distillate (DD oil) was the same as in example 1.
The crude sterol content extracted from DD oil with different VE contents and the VE content in crude sterol are shown in the following table:
from the above table, it can be seen that the content of VE in the DD oil is greater than 10%, VE is adhered to sterol, and the extraction rate of phytosterol is reduced. Specifically, when the VE content is 7.98%, the content of the extracted crude sterol is 65.5%. When the VE content is 10.12%, the content of the extracted crude sterol is 66.7%. When the VE content is 11.88%, the content of extracted crude sterol is 45.8%, and the sterol content in the filtrate is 2.44%.
Example 4:
the deodorized distillate in this example was essentially the same as in example 3, except that the sterol content of the deodorized distillate was below 12%; more preferably, the sterol content is between 2-10%.
The preparation method of the deodorized distillate is the same as that of example 3, and the sterol content of the prepared DD oil is below 12%.
The process for extracting sterols from deodorized distillate (DD oil) was the same as in example 1.
The crude sterol content of the DD oil extracts with different sterol contents is shown in the following table:
as can be seen from the above table, when the content of the sterol in the DD oil is more than 12%, the extraction rate of the sterol is reduced. Specifically, when the sterol content is 10.14%, the extracted crude sterol content is 67.4%. When the sterol content is 12.12%, the extracted crude sterol content is 67.2%. When the sterol content is 15.26%, the extracted crude sterol content is 48.3%, and the sterol content in the filtrate is 2.54%, which is not completely extracted.
From the above results, it was confirmed that the deodorized distillate to be used in the bio-enzyme esterification reaction was required to have an acid value of not more than 120mg/g, a saponification value of not more than 160mg/g, a VE content of not more than 10%, and a sterol content of not more than 12%.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. A deodorized distillate suitable for bio-enzyme esterification reaction, characterized in that the acid value of the deodorized distillate is below 120 mg/g.
2. The deodorized distillate for use in biological enzymatic esterification reaction according to claim 2, wherein the deodorized distillate has a saponification number of 160mg/g or less.
3. The deodorized distillate according to claim 3, characterized in that it has a VE content of less than 10%.
4. The deodorized distillate according to claim 4, wherein the deodorized distillate has a sterol content of 12% or less.
5. A process for the preparation of deodorized distillates suitable for use in the esterification reaction of biological enzymes, according to claim 4, characterized by comprising the following steps:
s1: detecting physical and chemical parameters of different types of deodorized distillate raw materials;
s2: mixing different kinds of deodorized distillate raw materials according to a certain proportion, and making the physicochemical parameters of the mixed deodorized distillate meet the requirements that the acid value is below 120mg/g, the saponification value is below 160mg/g, the VE content is below 10% and the sterol content is below 12%.
6. The method of claim 5, wherein the physicochemical parameters to be tested for the different types of deodorized distillates in S1 include acid value, saponification value, VE content and sterol content.
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