A composite emulsifier and its preparation method and application

Abstract

The invention discloses a composite emulsifier and a preparation method and application thereof, belonging to the technical field of emulsifiers. The cationic starch-sodium cholate composite emulsifier is prepared by the following method: sodium cholate and cationic starch are mixed, distilled water is added, and the mixture is heated and stirred at 50-60 DEG C in an oil bath for 0.5-2h to obtain the cationic starch-sodium cholate composite emulsifier solution, and then the obtained cationic starch-sodium cholate composite emulsifier solution is sealed and stored at 4 DEG C for 3-5h, and then vacuum freeze-dried at -30 DEG C for 24-36h to obtain the cationic starch-sodium cholate composite emulsifier. The preparation process of the invention is simple, the raw material source is abundant, the cost is low, and the use of industrial production is easy; the composite emulsifier provided by the invention has stable properties and strong emulsification ability; the invention uses cationic starch and sodium cholate as raw materials, is safe and non-toxic, has no problems such as phytotoxicity and pollution, and is green and environmentally friendly.

Description

Technical Field

[0001] The invention relates to the technical field of emulsifiers, and in particular to a compound formed by cationic starch and sodium cholate as a vegetable oil emulsifier, and a preparation method and application thereof. Background Art

[0002] Emulsifier is a kind of surfactant with both lipophilic and hydrophilic groups. Its molecules can be arranged in a directional manner to reduce the interfacial energy of the water phase and the oil phase in the mixed system, making the system relatively stable and uniform. It is an organic compound that can make immiscible liquids form stable emulsions. Emulsifier is a surfactant with both hydrophilic and lipophilic groups in its molecules. It gathers at the oil / water interface, which can reduce the interfacial tension and the energy required to form an emulsion, thereby increasing the energy of the emulsion. According to the HLB value, emulsifiers are divided into two categories: oil-in-water type (W / O type, i.e. lipophilic type) and water-in-oil type (O / W type, i.e. hydrophilic type). There are many types of emulsifiers, which can be used in cleaning, petroleum, food, pharmaceuticals, cosmetics, daily chemical industries and other industries.

[0003] Cationic starch is a starch ether with amino groups generated by the reaction of amine compounds and starch molecule hydroxyl groups. It belongs to chemically modified starch. Since cationic starch introduces cationic groups into starch macromolecules, it carries positive charge and is easy to combine with negatively charged matrix. It can also adsorb and retain other negatively charged additives on the matrix, thus giving starch cationic properties and becoming an important starch derivative. Due to its excellent properties, it has a wide range of uses abroad, mainly in papermaking, textile, food, adhesive, cosmetics, medicine and mining industries. At present, other industries in my country except papermaking are in the stage of promotion and application.

[0004] Sodium cholate is a mixture of bile acid salts extracted from cattle or pig bile. It is used as a choleretic in clinic for bile deficiency and cholecystitis. It can also be used for biochemical research, preparation of bacterial culture medium, anti-inflammatory, non-denaturing detergent for extracting membrane proteins, etc. The stereo conformation of sodium cholate molecules has two sides, hydrophilic and hydrophobic, which can reduce the surface tension between oil / water phases. It is an emulsifier, but its emulsification effect is poor when used alone.

[0005] Vegetable oil is a compound formed by the reaction of higher fatty acids and glycerol. It is widely distributed in nature and has a wide range of uses. It is the main raw material for industrial products such as soap, paint, ink, rubber, leather, textiles, candles, lubricants, synthetic resins, cosmetics and medicines. It is also used in large quantities in many industries such as food. Summary of the invention

[0006] The present invention provides a composite emulsifier and a preparation method and application thereof, which has excellent emulsification performance and good stability, and has the advantages of abundant raw material sources, low price, green environmental protection, etc. The preparation method of the composite is simple and easy, and it is easy to use in industrial production.

[0007] The composite emulsifier provided by the present invention is composed of cationic starch and sodium cholate and is prepared according to the following method:

[0008] Step 1: After mixing sodium cholate and cationic starch, add distilled water, heat and stir in an oil bath at 50-60° C. for 0.5-2 hours to obtain the cationic starch-sodium cholate complex emulsifier solution; the mass ratio of the cationic starch to the sodium cholate is 1:1-3;

[0009] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4° C. for 3 to 5 hours, and then vacuum freeze-dried at -30° C. for 24 to 36 hours to obtain a cationic starch-sodium cholate complex emulsifier.

[0010] Furthermore, the mass ratio of the cationic starch to sodium cholate is 1:1 to 3, preferably 1:2.

[0011] Furthermore, the oil bath temperature is 50-60° C., and the magnetic stirring time is 0.5-2 h, preferably 1.5-2 h.

[0012] Furthermore, the amount of distilled water added is 15-40 mL / g based on the total mass of the cationic starch and sodium cholate mixed.

[0013] Furthermore, the degree of substitution of the cationic starch is 0.08 to 0.12.

[0014] The present invention also provides an application of a cationic starch-sodium cholate compound emulsifier solution as an emulsifier for vegetable oil.

[0015] Furthermore, the application is: mixing the vegetable oil with the cationic starch-sodium cholate complex emulsifier solution, the volume ratio of the cationic starch-sodium cholate emulsifier to the vegetable oil is 50-60%:40-50% (preferably 60%:40%).

[0016] Furthermore, the vegetable oil is peanut oil, soybean oil, linseed oil, castor oil, rapeseed oil, valerian oil, or sunflower seed oil.

[0017] Compared with the prior art, the beneficial effects of the present invention are mainly reflected in:

[0018] (1) The preparation process is simple, the raw materials are abundant and low in cost, and it is easy to use in industrial production.

[0019] (2) The composite emulsifier provided by the present invention has stable properties and strong emulsifying ability.

[0020] (3) The present invention uses cationic starch and sodium cholate as raw materials, which are safe and non-toxic, have no problems such as phytotoxicity and pollution, and are green and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Instructions attached Figure 1 It is the structural formula of cationic starch.

[0022] Instructions attached Figure 2 It is the structural formula of sodium cholate. DETAILED DESCRIPTION

[0023] 1. Preparation of compound emulsifier

[0024] Example 1

[0025] A composite emulsifier, the preparation method of which comprises the following steps:

[0026] Step 1: Mix 1 g of sodium cholate and 1 g of cationic starch with a degree of substitution of 0.1, add 30 mL of distilled water, heat in an oil bath at 50° C., and stir for 1 hour to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0027] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 3 hours, and then vacuum freeze-dried at -30°C for 24 hours to obtain 2 g of cationic starch-sodium cholate complex emulsifier.

[0028] Example 2

[0029] A composite emulsifier, the preparation method of which comprises the following steps:

[0030] Step 1: Mix 2g of sodium cholate and 1g of cationic starch with a degree of substitution of 0.1, add 70mL of distilled water, heat in an oil bath at 55°C, and stir for 1.5h to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0031] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 4 hours, and then vacuum freeze-dried at -30°C for 30 hours to obtain 3 g of cationic starch-sodium cholate complex emulsifier.

[0032] Example 3

[0033] A composite emulsifier, the preparation method of which comprises the following steps:

[0034] Step 1: Mix 3 g of sodium cholate and 1 g of cationic starch with a degree of substitution of 0.09, add 150 mL of distilled water, heat in an oil bath at 60° C., and stir for 2 h to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0035] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 5 hours, and then vacuum freeze-dried at -30°C for 36 hours to obtain 4 g of cationic starch-sodium cholate complex emulsifier.

[0036] Example 4

[0037] A composite emulsifier, the preparation method of which comprises the following steps:

[0038] Step 1: Mix 1.5 g sodium cholate and 1 g cationic starch with a degree of substitution of 0.1, add 60 mL of distilled water, heat in an oil bath at 55°C, and stir for 1.5 hours to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0039] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 4 hours, and then vacuum freeze-dried at -30°C for 24 hours to obtain 2.5 g of cationic starch-sodium cholate complex emulsifier.

[0040] Example 5

[0041] A composite emulsifier, the preparation method of which comprises the following steps:

[0042] Step 1: Mix 2.5 g of sodium cholate and 2 g of cationic starch with a degree of substitution of 0.11, add 90 mL of distilled water, heat in an oil bath at 50°C, and stir for 0.5 h to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0043] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 5 hours, and then vacuum freeze-dried at -30°C for 30 hours to obtain 4.5 g of cationic starch-sodium cholate complex emulsifier.

[0044] Example 6

[0045] A composite emulsifier, the preparation method of which comprises the following steps:

[0046] Step 1: Mix 3.5 g of sodium cholate and 2 g of cationic starch with a degree of substitution of 0.1, add 160 mL of distilled water, heat in an oil bath at 60° C., and stir for 2 h to obtain a cationic starch-sodium cholate complex emulsifier solution.

[0047] Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4°C for 5 hours, and then vacuum freeze-dried at -30°C for 36 hours to obtain 5.5 g of cationic starch-sodium cholate complex emulsifier.

[0048] Comparative Example 1

[0049] Preparation method of single component emulsifier:

[0050] Take 0.6g, 1.5g, 2.4g, and 3.6g of sodium cholate respectively and add them into 29.4mL, 28.5mL, 27.6mL, and 26.4mL of distilled water respectively, heat in an oil bath at 50°C, and stir for 1h to obtain sodium cholate emulsifier solutions with mass fractions of 2%, 5%, 8%, and 12%, respectively.

[0051] Comparative Example 2

[0052] Preparation method of single component emulsifier:

[0053] Take 0.6g, 1.5g, 2.4g, and 3.6g of cationic starch with a substitution degree of 0.1 and add them to 29.4mL, 28.5mL, 27.6mL, and 26.4mL of distilled water respectively, heat in an oil bath at 50°C, and stir for 1h to obtain cationic starch emulsifier solutions with mass fractions of 2%, 5%, 8%, and 12%, respectively.

[0054] 2. Evaluation of emulsifying properties of emulsifiers

[0055] Evaluation method: The emulsification and emulsification stability of the composite system were determined by centrifugation. Equal volumes of water phase and oil phase were emulsified and the stratification was observed after centrifugation. The freeze-dried preparations of the above-mentioned composite emulsifiers were dissolved in distilled water and prepared into emulsifier solutions with a total mass fraction of 2%, 5%, 8%, and 12%, respectively. 10 mL of emulsifier solution and 10 mL of valerian oil were mixed evenly and emulsified. The height of the emulsion layer was measured after centrifugation, and the emulsification and emulsification stability were calculated according to the following formula.

[0056]

[0057] Table 1 Emulsification performance of different emulsifiers in Examples 1-6 and Comparative Examples 1-2

[0058]

[0059] 3. Emulsification effect of compound on vegetable oil emulsification

[0060] The emulsifying properties of the compound were evaluated by centrifugation. 6 g of sodium cholate and 3 g of cationic starch with a degree of substitution of 0.1 were dissolved in 150 mL of distilled water, heated in an oil bath at 50 ° C, and stirred for 2 hours to obtain the cationic starch-sodium cholate compound emulsifier solution. 10 mL of the emulsifier solution was mixed with 10 mL of peanut oil, soybean oil, linseed oil, castor oil, rapeseed oil, valerian oil, and sunflower oil, respectively, and emulsified after mixing evenly. The volume of the emulsion layer was measured after centrifugation. The emulsifying performance score was defined as:

[0061] Table 2 Emulsification effect of sodium cholate: cationic starch = 2:1 on different vegetable oils

[0062]

[0063]

[0064] The above table shows that the cationic starch-sodium cholate complex emulsifier has different emulsifying effects on different vegetable oils. This may be due to the different components of different vegetable oils. The complex has a strong emulsifying ability for the three essential oils of sunflower oil, peanut oil and rapeseed oil.

Claims

1. A composite emulsifier, characterized in that: The composite emulsifier is prepared according to the following method: Step 1: After mixing sodium cholate and cationic starch, add distilled water, heat and stir in an oil bath at 50-60° C. for 0.5-2 h to obtain the cationic starch-sodium cholate complex emulsifier solution; the mass ratio of the cationic starch to the sodium cholate is 1:1-3; Step 2: The cationic starch-sodium cholate complex emulsifier solution obtained in step 1 is sealed and stored at 4° C. for 3 to 5 hours, and then vacuum freeze-dried at -30° C. for 24 to 36 hours to obtain a cationic starch-sodium cholate complex emulsifier; The degree of substitution of the cationic starch is 0.08-0.

12.

2. The emulsifier of a composite compound according to claim 1, characterized in that The mass ratio of the cationic starch to sodium cholate is 1:1-3.

3. The emulsifier of a composite compound according to claim 1, characterized in that The oil bath temperature is 50-60°C, and the magnetic stirring time is 0.5-2h.

4. The emulsifier of a composite compound according to claim 1, characterized in that The amount of distilled water added is 15-40 mL / g based on the total mass of the cationic starch and sodium cholate mixed.

5. Use of the cationic starch-sodium cholate complex emulsifier as claimed in any one of claims 1 to 4 as an emulsifier for vegetable oil.

6. The use according to claim 5, characterized in that The application is: mixing the vegetable oil with the cationic starch-sodium cholate compound emulsifier solution, wherein the volume ratio of the cationic starch-sodium cholate emulsifier solution to the vegetable oil is 50-60%:40-50%.

7. The use according to claim 5, characterized in that The vegetable oil is peanut oil, soybean oil, linseed oil, castor oil, rapeseed oil, valerian oil and sunflower seed oil.

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