A process for the preparation of phytosteryl esters

Abstract

The application discloses a preparation method of phytosterol ester, and relates to the technical field of food engineering, and comprises the following steps: loading a catalyst and active ingredients, wherein the active ingredients comprise stannous oxide, and the loading material comprises one or more combinations of kaolin, activated clay and diatomite; a phytosterol mixture and oleic acid with a preset concentration are added into a reaction kettle according to a first preset mass ratio, and are uniformly mixed; the loaded catalyst is further added into the reaction kettle, and the mass ratio of the loaded catalyst to the phytosterol mixture is a second preset mass ratio; the reaction kettle is controlled to reach a preset vacuum pressure, and a phytosterol ester is obtained by reacting at a first preset temperature and a preset stirring speed for a first preset time; and the application can solve the technical problems of complex process and catalyst residue in the prior art.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of food engineering, and in particular to a preparation method of phytosterol ester. BACKGROUND

[0002] Phytosterol ester can inhibit the absorption of cholesterol and promote its metabolism and excretion, inhibit cholesterol biosynthesis, promote cholesterol catabolism, and reduce cholesterol levels, thereby achieving the effect of reducing blood lipids; phytosterol ester can inhibit platelet aggregation and thrombus formation, effectively preventing cardiovascular diseases. Phytosterol ester is widely used and can be applied to dairy products, functional foods, medicines, oils and cosmetics, reducing the use of emulsifiers. As a new resource food, the quality requirement of phytosterol ester is light yellow viscous oil paste, phytosterol ester and phytosterol (free) is greater than or equal to 97%, phytosterol ester is greater than or equal to 90%, free phytosterol is less than or equal to 6%, and acid value is less than or equal to 1mg KOH / g.

[0003] The current common preparation methods of phytosterol ester are chemical catalysis and enzyme catalysis. The enzyme catalysis has relatively mild reaction conditions, less by-products and high product safety, but the stability and reusability of the enzyme preparation are difficult to meet the requirements of industrial production. Subsequently, the immobilized lipase is removed by filtration, the organic solvent and the alkaline ionic liquid are recovered by extraction, then the neutralizing agent is added to remove the unreacted fatty acid, and finally the phytosterol ester is obtained. This process is complex, there is a risk of residual organic solvent, the reusability of the enzyme is not high, and it is not suitable for industrial production. The chemical catalysis has short reaction time, high yield and easy industrialization. The commonly used catalysts p-toluenesulfonic acid and SnO both have good catalytic activity, and the acid values are both less than 0.2mg KOH / g; the activity of p-toluenesulfonic acid is the best, the reaction time is short, and the catalyst dosage is small, but the S element is residual, and when the reaction temperature exceeds 185℃, the reverse reaction is obvious; ZnO, MgO, SnO and SnO@Al2O3 also have metal residues. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application aims to provide a preparation method of phytosterol ester, which solves the technical problems of complex process and catalyst residue in the traditional preparation of phytosterol ester in the prior art.

[0005] The present application provides a preparation method of phytosterol ester, which comprises:

[0006] The active ingredient includes stannous oxide, and the support includes one or more combinations of kaolin, activated clay and diatomite;

[0007] A phytosterol mixture and oleic acid with a preset concentration are added to a reaction kettle according to a first preset mass ratio and uniformly mixed.

[0008] A supported catalyst is further added into the reaction kettle, and the mass ratio of the supported catalyst to the phytosterol mixture is a second preset mass ratio;

[0009] The reaction kettle is controlled to reach a preset vacuum pressure, and the phytosterol ester is obtained by reacting for a first preset time at a preset stirring speed and a first preset temperature.

[0010] The reaction route is as follows:

[0011]

[0012] wherein,

[0013] R2 = 8-Heptadecenyl.

[0014] Compared with the prior art, the method for preparing the phytosterol ester can effectively improve the yield and purity and reduce the catalyst residue.

[0015] Further, the step of preparing the supported catalyst from the support and the active ingredient includes:

[0016] The support is soaked in a second preset concentration of hydrochloric acid solution for a second preset time for pretreatment.

[0017] The active ingredient stannous oxide is dissolved in a second preset concentration of hydrochloric acid solution to prepare an impregnation solution.

[0018] The pretreated support is added into the impregnation solution and reacted for a third preset time, and then sodium hydroxide solution is slowly added to adjust the pH value to a preset value.

[0019] The reacted support is calcined at a second preset temperature for a fourth preset time to be activated to obtain the supported catalyst.

[0020] Further, the mass ratio of the support to the active ingredient is (3-5) : 1.

[0021] Further, the second preset concentration is 36% to 38%, the second preset time is 5 min to 15 min, the third preset time is 25 min to 45 min, and the preset pH value is 7 to 8.

[0022] Further, the second preset temperature is 150 DEG C to 180 DEG C, and the fourth preset time is 2 h to 5 h.

[0023] Further, the first preset concentration of the phytosterol mixture is W, the mass of the phytosterol mixture is M, the mass of the oleic acid is m, the first preset mass ratio is MW / m, and the first preset mass ratio is 1:(0.5 to 1.5).

[0024] Further, the mass of the active ingredient is Z, the second preset mass ratio is Z / MW, and the second preset mass ratio is (0.001 to 0.005):1.

[0025] Further, the preset vacuum pressure is 80 Pa to 150 Pa, the preset stirring speed is 100 r / min to 500 r / min, the first preset temperature is 160 DEG C to 180 DEG C, and the first preset time is 4 h to 6 h.

[0026] Further, when the load is any two combinations, the mass ratio of the two loads is 1:1, and when the load is three combinations, the mass ratio of the kaolin, the activated white clay, and the diatomite is 3:4:3.

[0027] Further, the method further comprises:

[0028] When the reaction of the reaction kettle is completed, an equal amount of petroleum ether is added and stirred, activated carbon and activated white clay are added for decolorization, and suction filtration is performed to obtain a filtrate;

[0029] The filtrate is subjected to rotary evaporation to remove petroleum ether, water, and excess oleic acid;

[0030] Ethanol is added for washing and extraction, and the ethanol is removed by rotary evaporation to obtain phytosterol esters. BRIEF DESCRIPTION OF DRAWINGS

[0031] The above and / or additional aspects and advantages of the present application will become apparent and more readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings, in which:

[0032] Figure 1 A flowchart of the method for preparing phytosterol esters in the present application; DETAILED DESCRIPTION

[0033] In order to make the objects, characteristics and advantages of the present application more apparent, the specific embodiments of the present application will be described in detail below with reference to the accompanying drawings. The present application is shown in several embodiments in the drawings. However, the present application can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the disclosure of the present application more thorough and comprehensive.

[0034] It should be noted that when an element is referred to as being "fixed" to another element, it can be directly on the other element or there can be an intervening element. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or there can be an intervening element. The terms "vertical", "horizontal", "left", "right", "upper", "lower", and similar expressions as used herein are for illustrative purposes only and are not intended to indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the present application.

[0035] In the present application, unless otherwise explicitly specified and limited, the terms "mounting", "connection", "connecting", "fixing" and the like should be interpreted broadly, for example, it can be fixedly connected, or it can be detachably connected, or it can be integrally connected; it can be mechanically connected, or it can be electrically connected; it can be directly connected, or it can be indirectly connected through an intermediate medium; it can be the internal communication of two elements. For those skilled in the art, the specific meaning of the above terms in the present application can be understood according to the specific circumstances. The term "and / or" used herein includes any and all combinations of one or more related listed items.

[0036] Please refer to Figure 1 , which shows a method for preparing phytosterol esters provided by the present application, the method comprising steps S10-S13:

[0037] Step S10, the active ingredient including stannous oxide is prepared into a supported catalyst with a support including one or more combinations of kaolin, activated clay and diatomite;

[0038] Specifically, the support is soaked in a second pre-set concentration of hydrochloric acid solution for a second pre-set time for pretreatment;

[0039] When the support is any two combinations, the mass ratio of the two supports is 1:1, and when the support is three combinations, the mass ratio of the kaolin, the activated clay and the diatomite is 3:4:3.

[0040] Preferably, the second preset concentration is 36% to 38%, for example, it can be 36%, 37% or 38%, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0041] Preferably, the second preset time is 5 min to 15 min, for example, it can be 5 min, 8 min, 10 min, 12 min or 15 min, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0042] It should be noted that the load is pretreated with a hydrochloric acid solution to remove heavy metals in the load. In addition, the pretreatment of the hydrochloric acid solution can make the surface of the load carry acidic groups, improve the adsorption capacity, and be beneficial to the subsequent loading of active ingredients.

[0043] The active ingredient stannous oxide is added to the second preset concentration of the hydrochloric acid solution for dissolution to configure an impregnation solution;

[0044] The pretreated load is added to the impregnation solution for reaction for a third preset time, and then sodium hydroxide solution is slowly added to adjust to a preset pH value.

[0045] Preferably, the third preset time is 25 min to 45 min, for example, it can be 25 min, 30 min, 35 min, 40 min or 45 min, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0046] Preferably, the preset pH value is 7 to 8.

[0047] The mass ratio of the load to the active ingredient is (3-5):1.

[0048] It should be noted that the active ingredient stannous oxide is loaded on the load to effectively improve the activity of the loaded catalyst. The active ingredient includes stannous oxide, and the load includes one or more combinations of kaolin, activated clay and diatomite. When the stannous oxide is loaded on the load, it can have the characteristics of high catalytic activity and reduced catalyst element residues.

[0049] The reacted load is calcined at a second preset temperature for a fourth preset time to be activated to obtain a loaded catalyst.

[0050] Preferably, the second preset temperature is 150°C to 180°C, for example, it can be 150°C, 155°C, 160°C, 165°C, 170°C, 175°C or 180°C, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0051] Preferably, the fourth preset time is 2h-5h, for example, it can be 2h, 3h, 4h or 5h, but is not limited to the listed values, and other values not listed in the value range are also applicable.

[0052] It should be noted that calcination at the second preset temperature can effectively remove the solvent, increase the specific surface area of the support, and improve the uniformity of the distribution of the active ingredient on the support.

[0053] Step S11, a plant sterol mixture and oleic acid of a preset concentration are added to the reaction kettle according to a first preset mass ratio, and are uniformly mixed;

[0054] Further, the plant sterol mixture is derived from soybean oil, rapeseed oil, corn oil and the like, and the oleic acid is derived from sunflower seed oil.

[0055] The first preset concentration of the plant sterol pure substance in the plant sterol mixture is W, the mass of the plant sterol mixture is M, the mass of the oleic acid is m, and the first preset mass ratio of the plant sterol pure substance is MW / m, and the value range of the first preset mass ratio is 1:(0.5-1.5).

[0056] It should be noted that under the setting of the first preset mass ratio, the reaction of the plant sterol and the oleic acid to generate the plant sterol ester can be effectively improved.

[0057] Step S12, a supported catalyst is further added to the reaction kettle, and the mass ratio of the supported catalyst to the plant sterol mixture is a second preset mass ratio;

[0058] The supported catalyst is Z, the second preset mass ratio is Z / MW, and the value range of the second preset mass ratio is (0.001-0.005):1.

[0059] Step S13, the reaction kettle is controlled to reach a preset vacuum pressure, and is reacted at a preset stirring speed and a first preset temperature for a first preset time to obtain a plant sterol ester;

[0060] The reaction route is as follows:

[0061]

[0062] wherein,

[0063] R2=8-Heptadecenyl.

[0064] The preset vacuum pressure is 80Pa-150Pa, the preset stirring speed is 100r / min-500r / min, the first preset temperature is 160℃-180℃, and the first preset time is 4h-6h.

[0065] By setting the preset vacuum pressure, the preset stirring speed, and the first preset temperature, the yield and purity of the reaction can be effectively improved, the reaction time can be reduced, and the energy consumption can be reduced.

[0066] The method further comprises:

[0067] When the reaction in the reaction kettle is completed, an equal amount of petroleum ether is added and stirred, activated carbon and activated clay are added for decolorization, and filtration is performed to obtain a filtrate;

[0068] The filtrate is subjected to rotary evaporation to remove the petroleum ether and moisture, and distillation is performed to remove excess oleic acid.

[0069] Ethanol is added for washing and extraction, and rotary evaporation is performed to remove the ethanol to obtain the phytosterol ester.

[0070] The application is further described below with reference to specific examples:

[0071] Example 1

[0072] The method provided by the first embodiment of the application provides a method for preparing a phytosterol ester, and the method comprises steps S10-S13:

[0073] In step S10, a support and an active ingredient are prepared into a supported catalyst, the active ingredient comprises stannous oxide, and the support comprises one or more combinations of kaolin, activated clay, and diatomite.

[0074] Specifically, the support is soaked in a second preset concentration of a hydrochloric acid solution for a second preset time for pretreatment.

[0075] The support is activated clay.

[0076] The second preset concentration is 36% to 38%, and the second preset time is 10 minutes.

[0077] The catalyst is dissolved in a second preset concentration of a hydrochloric acid solution to prepare an impregnation solution.

[0078] The pretreated support is added to the impregnation solution and reacted for a third preset time, and then sodium hydroxide solution is slowly added to adjust the pH value to a preset value.

[0079] The third preset time is 30 minutes, and the preset pH value is 7 to 8.

[0080] The mass ratio of the support to the active ingredient is 4:1.

[0081] The reacted support is calcined at a second preset temperature for a fourth preset time to be activated to obtain the supported catalyst.

[0082] The second preset temperature is 160 DEG C, and the fourth preset time is 3h.

[0083] In step S11, a plant sterol mixture and oleic acid with a first preset concentration are added into a reaction kettle according to a first preset mass ratio, and are uniformly mixed.

[0084] The first preset concentration of the plant sterol mixture is 97.3%, the plant sterol mixture is derived from soybean oil with a mass of 50.0g, the oleic acid is sunflower oil acid with a mass of 50.0g, and the first preset mass ratio is 1:1.028.

[0085] It should be noted that the step of uniform mixing is that the oil bath is heated to 110 DEG C, and stirring dehydration is performed for 1h.

[0086] In step S12, a supported catalyst is further added into the reaction kettle, and the mass ratio of the supported catalyst to the plant sterol mixture is a second preset mass ratio.

[0087] The supported catalyst is Z=0.10g, the second preset mass ratio is Z / MW, and the second preset mass ratio is in a range of 0.002:1.

[0088] In step S13, the reaction kettle is controlled to reach a preset vacuum pressure, and is reacted at a preset stirring speed and a first preset temperature for a first preset time to obtain a plant sterol ester.

[0089] The preset vacuum pressure is 100Pa, the preset stirring speed is 200r / min, the first preset temperature is 160 DEG C, and the first preset time is 6h.

[0090] The method further comprises:

[0091] When the reaction of the reaction kettle is completed, an equal amount of petroleum ether is added and stirred, activated carbon and activated clay are further added for decolorization, and suction filtration is performed to obtain a filtrate.

[0092] The activated carbon is 1%, the activated clay is 2%, and the decolorization is performed for 0.5h.

[0093] The filtrate is subjected to rotary evaporation to remove petroleum ether, water, and excess oleic acid.

[0094] Ethanol is added for washing and extraction, and the ethanol is removed by rotary evaporation to obtain a plant sterol ester.

[0095] A yellowish viscous plant sterol ester with a lipid aroma is obtained, with a yield of 75.6g, a yield of 92.2%, a content of 97.6%, free sterols of 0.6%, an acid value of 0.11mg KOH / g, and a tin residual amount of 24ppm.

[0096] It should be noted that the free sterol content of the phytosterol ester product is determined according to the gas chromatography method of GB / T25223-2010 of the People's Republic of China for determination of sterol composition and total sterol content of animal and vegetable oils.

[0097] The total phytosterol content of the phytosterol ester product is determined according to the standard method, and then the method of GB / T25223-2010 is used to determine the total phytosterol content after saponification of the phytosterol ester.

[0098] The content of the phytosterol ester product is calculated from the determined free sterol content and total phytosterol content according to the quantitative relationship.

[0099] The acid value of the phytosterol ester product is determined according to GB / T5530-2005 for determination of acid value and acidity of animal and vegetable oils.

[0100] Example 2

[0101] The second embodiment of the present application provides a method for preparing phytosterol ester, which is different from the method for preparing phytosterol ester in the first embodiment in that:

[0102] The support is active clay and kaolin with a mass ratio of 1:1.

[0103] The first preset concentration of the phytosterol mixture is 97.3%, the phytosterol mixture is derived from soybean oil with a mass of 50.0g, the oleic acid is sunflower oil acid with a mass of 50.0g, and the first preset mass ratio is 1:1.028.

[0104] A light yellow thick phytosterol ester with a lipid aroma is obtained, with a yield of 91.5%, a content of 97.5%, a free sterol content of 0.8%, an acid value of 0.12mg KOH / g, and a tin residual amount of 16ppm.

[0105] Example 3

[0106] The third embodiment of the present application provides a method for preparing phytosterol ester, which is different from the method for preparing phytosterol ester in the first embodiment in that:

[0107] The support is diatomite, and the catalyst is proportionally increased, with a first preset temperature of 170℃ and a first preset time of 5h.

[0108] The first preset concentration of the phytosterol mixture is 99.0%, the phytosterol mixture is derived from rapeseed oil with a mass of 200.0g, the oleic acid is sunflower oil acid with a mass of 203.3g, and the first preset mass ratio is 1:1.027.

[0109] A pale yellow thick phytosterol ester with a lipid aroma of 299.2 g was obtained, the yield was 91.2%, the content was 98.0%, the free sterol was 0.3%, the acid value was 0.10 mg KOH / g, and the tin residual amount was 42 ppm.

[0110] Example Four

[0111] The plant sterol ester preparation method provided in the fourth embodiment of the present application is different from the plant sterol ester preparation method in the first embodiment in that:

[0112] The support is diatomite and activated clay with a mass ratio of 1:1, the supported catalyst is increased in proportion, the first preset temperature is 170 DEG C, and the first preset time is 5 h.

[0113] The first preset concentration of the plant sterol mixture is 99.0%, the plant sterol mixture is derived from rapeseed oil, the mass is 200.0 g, the oleic acid is sunflower oil acid, the mass is 203.3 g, and the first preset mass ratio is 1:1.027.

[0114] A pale yellow thick phytosterol ester with a lipid aroma of 302.1 g was obtained, the yield was 92.1%, the content was 98.2%, the free sterol was 0.2%, the acid value was 0.08 mg KOH / g, and the tin residual amount was 11 ppm.

[0115] Example Five

[0116] The plant sterol ester preparation method provided in the fifth embodiment of the present application is different from the plant sterol ester preparation method in the first embodiment in that:

[0117] The support is kaolin, the supported catalyst is increased in proportion, the first preset temperature is 180 DEG C, and the first preset time is 4 h.

[0118] The first preset concentration of the plant sterol mixture is 95.6%, the plant sterol mixture is derived from mixed vegetable oil, the mass is 500.0 g, the oleic acid is sunflower oil acid, the mass is 490.7 g, and the first preset mass ratio is 1:1.027.

[0119] A pale yellow thick phytosterol ester with a lipid aroma of 766.5 g was obtained, the yield was 93.4%, the content was 97.7%, the free sterol was 0.7%, the acid value was 0.11 mg KOH / g, and the tin residual amount was 48 ppm.

[0120] Example Six

[0121] The sixth embodiment of the present application provides a preparation method of phytosterol ester, and the difference between the preparation method of phytosterol ester in the embodiment and the preparation method of phytosterol ester in the first embodiment is that:

[0122] The support is kaolin and activated white clay with a mass ratio of 1:1, the supported catalyst is increased in proportion, the first preset temperature is 180 DEG C, and the first preset time is 4h.

[0123] The first preset concentration of the phytosterol mixture is 95.6%, the phytosterol mixture is derived from mixed vegetable oil with a mass of 500.0g, the oleic acid is sunflower oil acid with a mass of 490.7g, and the first preset mass ratio is 1:1.027.

[0124] The phytosterol ester with a light yellow color, a thick and greasy smell, a mass of 764.8g, a yield of 93.2%, a content of 97.3%, free sterols of 0.8%, an acid value of 0.13mg KOH / g, and a tin residue of 16ppm is obtained.

[0125] Comparative example one

[0126] The first comparative example of the present application provides a preparation method of phytosterol ester, and the difference between the preparation method of phytosterol ester in the comparative example and the preparation method of phytosterol ester in the first embodiment is that:

[0127] The catalyst is stannous oxide, and no loading treatment is performed.

[0128] The first preset concentration of the phytosterol mixture is 97.3%, the phytosterol mixture is derived from soybean oil with a mass of 50.0g, the oleic acid is sunflower oil acid with a mass of 50.0g, and the first preset mass ratio is 1:1.028.

[0129] The phytosterol ester with a dark and light yellow color, a thick and greasy smell, a mass of 70.3g, a yield of 85.7%, a content of 86.4%, free sterols of 5.4%, an acid value of 0.85mg KOH / g, and a tin residue of 1284ppm is obtained.

[0130] Comparative example two

[0131] The second comparative example of the present application provides a preparation method of phytosterol ester, and the difference between the preparation method of phytosterol ester in the comparative example and the preparation method of phytosterol ester in the fifth embodiment is that:

[0132] The catalyst is stannous oxide, and no loading treatment is performed.

[0133] The first preset concentration of the phytosterol mixture is 96.5%, the phytosterol mixture is derived from mixed vegetable oil, the mass is 500.0 g, the oleic acid is sunflower oil acid, the mass is 490.7 g, and the first preset mass ratio is 1:1.027.

[0134] A dark and light yellow thick phytosterol ester 726.9 g with a lipid aroma is obtained, the yield is 88.6%, the content is 87.5%, the free sterol is 4.7%, the acid value is 0.78 mg KOH / g, and the tin residual amount is 1053 ppm.

[0135] In combination with the data of Examples 1 to 6 and Comparative Examples 1 and 2, it can be seen that the yield and purity of the phytosterol ester can be effectively improved by the preparation method of the phytosterol ester, and the residual amount of the catalyst is reduced.

[0136] In the description of the present specification, the description of the terms "one embodiment", "some embodiments", "an example", "a specific example", or "some examples" and the like means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0137] The above-described embodiments only express several embodiments of the present application, which are described in a more specific and detailed manner, but should not be understood as limiting the scope of the patent of the present application. It should be noted that for ordinary skilled persons in the art, several modifications and improvements can be made without departing from the concept of the present application, which are all within the protection scope of the present application. Therefore, the protection scope of the patent of the present application should be subject to the appended claims.

Claims

1. A method for preparing phytosterol esters, characterized in that: The method comprises: The supported material and the active ingredient stannous oxide are prepared into a supported catalyst, wherein the supported material is one or more combinations of kaolin, activated clay, and diatomaceous earth, including: The load is placed in a hydrochloric acid solution of a second preset concentration and immersed for a second preset time for pretreatment. The active ingredient stannous oxide is added to a hydrochloric acid solution of a second preset concentration for dissolution to prepare an impregnation solution. The pretreated load is added to the impregnation solution to react for a third preset time, and then sodium hydroxide solution is slowly added to adjust to a preset pH value. Calcinate the supported material after the reaction at a second preset temperature for a fourth preset time to activate it, thereby obtaining a supported catalyst, wherein the second preset concentration is 36% to 38%, the second preset time is 5 minutes to 15 minutes, the third preset time is 25 minutes to 45 minutes, the preset pH value is 7 to 8, the second preset temperature is 150° C. to 180° C., and the fourth preset time is 2 hours to 5 hours; Adding a plant sterol mixture of a preset concentration and oleic acid into the reactor according to a first preset mass ratio and mixing them evenly; Then, adding a supported catalyst to the reactor, wherein the mass ratio of the supported catalyst to the phytosterol mixture is a second preset mass ratio; Controlling the reactor to reach a preset vacuum pressure, reacting for a first preset time at a preset stirring speed and a first preset temperature to obtain phytosterol esters, wherein the preset vacuum pressure is 80 Pa to 150 Pa, the preset stirring speed is 100 r / min to 500 r / min, the first preset temperature is 160° C. to 180° C., and the first preset time is 4 h to 6 h; The reaction route is as follows: Where R1= , , , .

2. The method for preparing phytosterol esters according to claim 1, wherein The mass ratio of the support to the active ingredient stannous oxide is (3-5):

1.

3. The method for preparing phytosterol ester according to claim 1, wherein The first preset concentration of the plant sterol mixture is W, the mass of the plant sterol mixture is M, the mass of the oleic acid is m, the first preset mass ratio is MW / m, and the value range of the first preset mass ratio is 1: (0.5~1.5).

4. The method for preparing phytosterol esters according to claim 3, wherein The mass of the supported catalyst is Z, the second preset mass ratio is Z / MW, and the value range of the second preset mass ratio is (0.001~0.005):

1.

5. The method for preparing phytosterol esters according to claim 1, wherein When the loads are any two combinations, the mass ratio of the two loads is 1:

1. When the loads are three combinations, the mass ratio of the kaolin, the activated clay, and the diatomaceous earth is 3:4:

3.

6. The method for preparing phytosterol esters according to claim 1, wherein The method further comprises: After the reaction in the reactor is completed, an equal amount of petroleum ether is added and stirred, and then activated carbon and activated clay are added for decolorization, and the mixture is filtered to obtain a filtrate; The filtrate is subjected to rotary evaporation to remove petroleum ether and water, and excess oleic acid is removed by distillation; Ethanol is added for washing and extraction, and the ethanol is removed by rotary evaporation to obtain phytosterol esters.

Images