Low-dust easy-to-disperse xanthan gum and method for preparing the same

Abstract

The application provides a low-dust easy-to-disperse xanthan gum and a preparation method thereof. The application adopts sodium caseinate and polyglycerol fatty acid ester with a specific HLB value to mix with xanthan gum and to perform secondary granulation through a certain means, so that the proportion of fine particle size in the powder can be reduced to reduce the dust amount, the dispersion and solubility of the xanthan gum can be effectively improved, the process and formula are simple and convenient, and the production scale-up is facilitated. The obtained xanthan gum product can be more conveniently applied to commercially available seasoning materials, dairy products, soup materials, beverages, especially solid beverages, meat products, baked products and various food industries. By controlling the particle size within a certain range, the large particles can be returned to be crushed, and the fine particle size byproduct can be subjected to secondary granulation, so that the loss in the preparation process is further reduced, and the production scale-up is facilitated.

Description

Technical Field

[0001] This invention relates to the field of biochemical engineering, and more specifically, to a low-dust, easily dispersible xanthan gum and its preparation method. Background Technology

[0002] Xanthan gum is an ideal thickener, suspending agent, emulsifier, and molding agent in the food industry. Under certain harsh conditions such as high temperature, high salt, and low pH, xanthan gum outperforms existing food additives such as gelatin, CMC (carboxymethyl cellulose), and guar gum. It is widely used in dairy products, beverages, convenience foods, and frozen foods, and the market demand for xanthan gum continues to increase.

[0003] Xanthan gum should be fully hydrated before use; otherwise, its thickening and suspending properties cannot be fully utilized. The dissolution of xanthan gum in water involves two stages: first, swelling, where water molecules penetrate the gum and cause it to expand; and second, the swollen gum evenly distributes in the water until it dissolves completely. Due to its strong hydrophilicity, when xanthan gum enters water, its outermost layer immediately absorbs a large amount of water and swells to form aggregates, preventing other water molecules from entering and creating insoluble "fish-eye" structures that affect the viscosity and rheological properties of the solution. This agglomeration is particularly pronounced when fine powder particles are present in the xanthan gum product. This significantly impacts its practical applications, especially in areas requiring rapid dissolution and thickening, severely limiting its use.

[0004] To address the technical challenge of agglomeration during the dissolution process of xanthan gum, domestic researchers have conducted extensive exploratory studies to improve its practical application performance. Existing techniques are insufficient to further enhance the dispersion and dissolution properties of xanthan gum, and also fail to contribute to improving product viscosity. For example, CN102219912B employs a granulation method that uses a certain proportion of water to re-bind powdered xanthan gum. This method is simple and direct, increasing the specific surface area of ​​the xanthan gum particles and helping to improve dispersion and dissolution. However, this method does not actually change any properties of xanthan gum itself, nor does it add any other auxiliary components; therefore, the improvement effect is limited, and it has no impact on the apparent viscosity of xanthan gum. CN102220393A adds 0.3–0.7% (w / w) of monoglyceride to xanthan gum during pulverization, which is a purely physical mixing method. Monoglycerides contain one lipophilic long-chain alkyl group and two hydrophilic hydroxyl groups, thus exhibiting good surface activity. However, relying solely on dry physical mixing makes it difficult to fully realize their potential. CN113430237A describes the preparation of instant xanthan gum using a large amount (10% by weight) of maltodextrin as a binder. While this improves the dispersion and dissolution speed, it significantly reduces the purity and proportion of xanthan gum in the final product. Furthermore, sucrose fatty acid esters are often used as emulsifiers to improve xanthan gum solubility, but their final dispersion speed is insufficient, and they have no effect on increasing the apparent viscosity of the xanthan gum product itself.

[0005] Sodium caseinate, also known as sodium caseinate, casein sodium, or casein, is the sodium salt of casein, the main protein in cow's milk. It is a safe and harmless thickener and emulsifier. Sodium caseinate has high nutritional value and is therefore often used as a nutritional fortifier. Polyglyceryl ester (PGFE) is a general term for a series of products, also known as polyglycerol ester (PGFE), polyglycerol monopolyglycerol ester, or fatty acid polyglycerol ester. It is characterized by having a large number of hydrophilic hydroxyl groups. Polyglyceryl esters have much better emulsifying properties than monoglycerides because they have more hydrophilic hydroxyl groups. Their hydrophilicity increases with the degree of polymerization of glycerol, while their lipophilicity varies depending on the alkyl group of the fatty acid. By changing the degree of polymerization of polyglycerol, the type of fatty acid, and the degree of esterification, a series of polyglyceryl ester products with different properties (HLB values ​​from 1 to 20) can be obtained, ranging from lipophilic to hydrophilic, to meet various applications. Summary of the Invention

[0006] The purpose of this invention is to provide a low-dust, easily dispersible xanthan gum and its preparation method.

[0007] In actual research, the inventors unexpectedly discovered that sodium caseinate helps to improve the dispersion and solubility of xanthan gum. Specifically, the xanthan gum product obtained by adding a certain amount of sodium caseinate has an increased apparent viscosity, a significantly faster dispersion speed, and a significantly earlier dissolution and tackification time. Moreover, the product obtained by this operation has a faint milky aroma, making it more appealing to consumers in terms of sensory appeal.

[0008] To further improve the dispersion and solubility of xanthan gum, the inventors screened commonly used emulsifiers in the food industry and identified a class of polyglycerol fatty acid esters with specific HLB values. Through exploration and verification of its usage conditions, a xanthan gum product was obtained with faster dispersion and dissolution rates, minimal or no fish-eyes after dissolution, and rapid dissolution with continued stirring. This product has a low emulsifier addition ratio, fast dispersion and dissolution speed, and is easy to use. Compared to ordinary powders, it has increased apparent viscosity, extremely low dust content, and a pleasant sensory taste, making it more appealing to a wider range of users.

[0009] To achieve the objective of this invention, in a first aspect, this invention provides a method for preparing low-dust, easily dispersible xanthan gum, comprising the following steps:

[0010] (1) Weigh sodium caseinate and polyglycerol fatty acid ester by mass (1-5): (3-8), add 60-85% v / v food grade ethanol solution to dissolve them according to the material-liquid ratio (4-13): (10-45), dissolve at 50-75℃, and then process with a colloid mill to obtain a light yellow to white emulsion.

[0011] The polyglycerol fatty acid ester has an HLB value of 2.0 to 11.0, preferably 2.5 to 8.0.

[0012] (2) The xanthan gum powder that has been crushed to a particle size of ≤0.18mm (about 80 mesh) is put into a wet granulator for stirring and shearing;

[0013] (3) Add the emulsion from step (1) into the above wet granulation machine and continue to stir and shear to obtain fine granules; wherein, the amount of emulsion added is calculated based on sodium caseinate and the mass ratio of it to xanthan gum is (1-5):1000.

[0014] (4) The fine granular material from step (3) is transferred to a fluidized bed granulator via negative pressure conveying and dried at 75±5℃ until the moisture content of the material is ≤13%.

[0015] (5) The dried material was separated by two layers of vibrating screens with particle sizes of 40 mesh (0.425 mm) and 80 mesh (0.18 mm) to obtain a low-dust, easily dispersible xanthan gum product with a particle size of 0.180 mm ≤ particle size ≤ 0.425 mm.

[0016] The polyglycerol fatty acid ester may be selected from at least one or a combination of polyglycerol stearate, polyglycerol isostearate, polyglycerol oleate, polyglycerol laurate, polyglycerol palmitate, polyglycerol myristate, polyglycerol caprylate, polyglycerol caprylate, polyglycerol caprylate, polyglycerol ricinoleate, and polyglycerol cocoate.

[0017] Furthermore, the method further includes: mixing the fine powder with a particle size <0.180mm from step (5) and the fine powder with a particle size >0.425mm that has been pulverized twice to ≤0.180mm, and performing secondary wet granulation and sieving to obtain a low-dust, easily dispersible xanthan gum product.

[0018] Secondly, the present invention provides a low-dust, easily dispersible xanthan gum product prepared according to the method described above.

[0019] This invention employs a mixture of ionic surfactant sodium caseinate and nonionic surfactant polyglycerol fatty acid ester as a dispersant and dissolving agent for xanthan gum. Both surfactants possess both hydrophilic and hydrophobic groups. The ratio of hydrophilic to hydrophobic groups determines the hydrophilic-lipophilic balance (HLB) value of the surfactant. Hydrophilic groups exhibit strong affinity for water molecules through hydrogen bonding, while hydrophobic groups bind to water molecules only through van der Waals forces, resulting in weaker affinity. Casein contains a large number of proline residues with pyrrole ring structures, which are concentrated on the peptide chain, thus limiting the formation of ordered structures such as α-helices and S-sheets in the protein's secondary structure, causing casein to randomly coil. Furthermore, the uneven distribution of residual water residues and the aggregation of the first 40-50 amino acids at the N-terminus give it unique amphiphilic properties, exhibiting excellent surfactant characteristics.

[0020] Polyglycerol fatty acid esters have a large number of hydrophilic hydroxyl groups, and their hydrophilicity increases with the degree of polymerization of glycerol, while their lipophilicity varies with the different alkyl groups of fatty acids. Therefore, by changing the degree of polymerization of polyglycerol, the type of fatty acid and the degree of esterification, a series of polyglycerol ester products with different properties from lipophilic to hydrophilic can be obtained to suit various special applications.

[0021] This invention first physically mixes sodium caseinate with a polyglycerol fatty acid ester with a specific HLB value and dissolves them in an ethanol solution of a specific concentration. This approach considers both the role of the numerous hydrophilic and lipophilic groups of both substances in promoting xanthan gum dissolution and the solubility issues of both substances in polar solvents, while also facilitating thorough integration with the xanthan gum product later. The resulting emulsion solution is then thoroughly mixed with xanthan gum during the wet granulation process, allowing some of the xanthan gum product to undergo localized adhesion, forming microparticles with partial pores, thus creating the final product.

[0022] During the dissolution process of the xanthan gum product of this invention, the ionic surfactant sodium caseinate forms a micelle core with hydrophobic groups bonded together. This core can further bind the side chain groups of xanthan gum. Meanwhile, the hydrated polar surfactant groups can form a shell on the micelle surface. To maintain the charge neutrality of the surfactant micelles, a diffuse double layer composed of counterions is also formed on the surface of the micelle shell, which helps to further alter the structure of xanthan gum in aqueous solution. Simultaneously, the large protein molecules of sodium caseinate can adsorb onto the surface of xanthan gum droplets, acting as a steric hindrance. As a nonionic surfactant, polyglycerol fatty acid esters form a micelle shell by binding water through hydroxyl groups. These two surfactants work together to achieve solubilization of xanthan gum through the micelle core during dissolution, and to mitigate the effect of water molecules being prevented from entering the interior and hydrating with xanthan gum during dissolution by competing with xanthan gum molecules for the outer layer of free water.

[0023] Meanwhile, the crystal structure of xanthan gum changes after wet granulation, forming tiny water molecule channels on the crystal surface. This helps water molecules to be released slowly and come into contact with the xanthan gum crystals, thereby improving its dispersion and solubility.

[0024] Furthermore, actual studies have found that when the HLB value of the selected polyglycerol fatty acid ester is greater than 8.0, its effect on improving the dispersion and dissolution performance of xanthan gum decreases. This is especially true when the HLB value is greater than 11.0, where the effect on promoting xanthan gum dispersion and dissolution is even worse, and the effect remains unsatisfactory even when used in combination with sodium caseinate. This may be because the HLB values ​​of sodium caseinate and polyglycerol fatty acid ester follow an additive relationship during the compounding process. When the HLB value of polyglycerol fatty acid ester is greater than 11.0, the additive HLB value approaches or exceeds the corresponding critical point, making the overall surfactant component highly hydrophilic. This causes the surfactant to excessively compete with xanthan gum for water molecules, thus affecting the solubility of xanthan gum itself.

[0025] In summary, the addition of surfactants has no adverse effects on the thickening and stabilizing properties of xanthan gum itself. Furthermore, sodium caseinate itself has a certain viscosity, and its use as a surfactant does, to some extent, enhance the viscosity of xanthan gum products. The combined use of these two surfactants significantly improves the dispersion and solubility properties of xanthan gum.

[0026] By employing the above technical solution, the present invention has at least the following advantages and beneficial effects:

[0027] This invention uses sodium caseinate and polyglycerol fatty acid esters with specific HLB values, mixed with xanthan gum and then subjected to secondary granulation. This reduces the proportion of fine particles in the powder, thereby reducing dust, while effectively improving the dispersion and solubility of xanthan gum. The process and formulation are simple and convenient, facilitating large-scale production. The resulting xanthan gum product can be readily applied to commercially available sauces, dairy products, soup bases, beverages (especially solid beverages), meat products, baked goods, and various food industries. By controlling the particle size within a certain range, large particles can be returned to crushing, and fine particle byproducts can be re-granulated to further reduce losses during preparation, facilitating large-scale production. Attached Figure Description

[0028] Figure 1 These are the dispersion and dissolution curves for all embodiments and comparative samples of this invention.

[0029] Figure 2 This is a comparison of the solution states of some embodiments and comparative samples of the present invention after measurement. Detailed Implementation

[0030] This invention addresses the problems of slow dispersion and dissolution, and the formation of fish-eye patterns in xanthan gum during use, by providing a method for preparing xanthan gum that is easy to disperse and dissolve, quickly forms tack, and has a higher viscosity.

[0031] The present invention also provides a method for effectively reducing dust in xanthan gum products.

[0032] The present invention also provides a xanthan gum product with low dust, high dispersion and solubility and higher viscosity.

[0033] The present invention adopts the following technical solution:

[0034] 1. Weigh sodium caseinate and polyglycerol fatty acid ester (different types, HLB value 2.0-11.0, preferably 2.5-8.0) according to a mass ratio of (1-5):3-8. Add 60-85% (v / v) food-grade ethanol solution to dissolve them according to a material-to-liquid ratio of (4-13):(10-45). The dissolution temperature is 50-75℃. Then, process the solution through a colloid mill to form a homogeneous emulsion that is light yellow to white, and set it aside as an emulsion.

[0035] 2. Add the xanthan gum powder, which has been crushed to a particle size of ≤0.18mm (about 80 mesh), into the wet granulator according to the mass. Then, slowly turn on the main motor stirring and the side shear blade motor, and adjust the frequency converter of the main motor and the frequency converter of the shear blade to the appropriate values.

[0036] 3. The hot ethanol solution containing sodium caseinate and polyglycerol fatty acid esters is pumped into a wet granulator at a uniform flow rate. Under the combined action of the main motor and shear blades of the granulator, stirring continues for 5–15 minutes, ultimately forming uniform, fine granular material. The emulsifier added, calculated based on sodium caseinate, has a mass ratio of (1–5):1000 of xanthan gum dry matter.

[0037] 4. Turn on the air top of the fluidized bed granulation equipment in advance to ensure good airtightness of the equipment. Turn on the top pulse and open the heater steam valve. Set the air inlet temperature to 75±3℃ and turn on the induced draft fan.

[0038] 5. Transfer the wet granulation product obtained in step 3 above to a fluidized bed granulator via negative pressure conveying. Dry the product at 75±5℃. During this process, adjust the frequency converter of the induced draft fan to ensure good fluidization of the material, maintain particle dispersion and fluidization, and prevent agglomeration. Dry the material until the moisture content reaches the value specified in GB1886.41-2015 (≤13%).

[0039] 6. The above materials are separated by two layers of vibrating screens with particle sizes of 40 mesh (0.425 mm) and 80 mesh (0.18 mm) to obtain a product with a particle size of 0.180 mm ≤ particle size ≤ 0.425 mm.

[0040] 7. In step / 6 above, fine powder with a particle size <0.180mm and particles with a particle size >0.425mm that have been pulverized twice to ≤0.180mm are mixed, and then subjected to secondary wet granulation and sieving to obtain a new low-dust, easily dispersible xanthan gum product.

[0041] In this invention, sodium caseinate is a commercially available food additive product, conforming to the national food safety standard GB1886.212-2016, Food Additive, Sodium Caseinate (also known as Sodium Caseinate); polyglycerol fatty acid esters are nonionic surfactants, also commercially available products, conforming to the national food safety standard GB1886.178-2016, Food Additive, Polyglycerol Fatty Acid Ester. Specifically, the polyglycerol fatty acid esters described in this invention have an HLB value of 2.5–8.0, and can be selected from various fatty acid families such as stearic acid, isostearic acid, oleic acid, lauric acid, palmitic acid, caprylic acid, capric acid, caprylic-capric acid, myristic acid, ricinoleic acid, and coconut oil acid.

[0042] To further verify the differences in product dispersion and dissolution properties, we used the following methods to evaluate product performance:

[0043] 1. Instruments and reagents

[0044] Brookfield rheometer and its rotor, φ60×60 round-bottom crystallizer, distilled water, and xanthan gum samples obtained from the experiment.

[0045] 2. Operating Method

[0046] a) Add 100g of distilled water to the crystallizing dish and immerse the rotor in the water until it reaches the required depth.

[0047] b) Weigh 0.50g of xanthan gum sample onto weighing paper for later use;

[0048] c) Set the rheometer shear rate to 100 1 / s, then start stirring and begin timing;

[0049] e) Pour the sample evenly into the crystallization dish within 10 seconds, and measure and record the results while stirring. The total recording time is 1200 min, and the recording interval is 10 seconds.

[0050] e) Based on the viscosity results, plot the curve of solution viscosity over time and evaluate the sample.

[0051] 3. Sample Evaluation

[0052] We analyzed and observed the curves of all samples, recording the product's tack time (the time when the first viscosity data appears) and the viscosity value at the 10th point after tack. Furthermore, we creatively used the 10th point after tack for evaluation. Since 100 seconds have passed from tack to this point, the slope of viscosity / time at that point indicates the product's dissolution rate and viscosity increase rate. The faster the sample disperses, the shorter its tack time; the faster the sample dissolves, the greater the viscosity / time slope at the 10th point after tack. For improved samples, the tack time should not exceed 100 seconds, and the corresponding slope after tack should not be less than 1.5 MPa. The formula for calculating this slope is:

[0053]

[0054] In addition, the number and size of white spots after the sample is dissolved are observed and compared to determine the effect of the sample dissolution.

[0055] The final dust ratio of the product was evaluated using standard sieves of 20 mesh (0.830 mm), 80 mesh (0.180 mm), and 140 mesh (0.109 mm).

[0056] The following examples are used to illustrate the present invention, but are not intended to limit the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are all commercially available products.

[0057] The wet granulator used in the following examples is a ZGH-350, purchased from Changzhou Pinzheng Drying Equipment Co., Ltd.

[0058] The fluidized bed granulator, model GFG-300, was purchased from Changzhou Xinli Drying Equipment Co., Ltd.

[0059] Example 1: Preparation method of low-dust, easily dispersible xanthan gum

[0060] Includes the following steps:

[0061] 1. Weigh sodium caseinate and decaglycerol decaoleate (HLB value approximately 2.5) at a mass ratio of 1:3. Dissolve them in 75.2% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 4:10 at a dissolution temperature of 65°C. Pass the above solution through a colloid mill to form a uniformly dispersed, light yellow emulsion solution for later use.

[0062] 2. Add the xanthan gum powder, which has been pulverized to a particle size of ≤0.18mm (about 80 mesh), into the wet granulator according to the mass. Then, slowly turn on the main motor stirring and the side shear blade motor respectively. Adjust the frequency converter of the main motor and the frequency converter of the shear blade to be able to completely stir the xanthan gum and make it able to pass through the shear blade to achieve the shearing purpose.

[0063] 3. The hot ethanol solution containing sodium caseinate and polyglycerol fatty acid esters is pumped into a wet granulator at a uniform flow rate. Under the combined action of the main motor and shear blade of the granulator, stirring continues for 12 minutes to finally form uniform, small granular wet material. The emulsifier added is calculated based on the mass ratio of sodium caseinate to xanthan gum dry matter of 3:1000.

[0064] 4. Turn on the air top of the fluidized bed granulation equipment in advance and ensure good airtightness of the equipment. Turn on the top pulse and heater steam valves, set the air inlet temperature to 75±3℃, and turn on the induced draft fan.

[0065] 5. Transfer the wet granulation product obtained in step 3 above to a fluidized bed granulator via negative pressure conveying. Dry it at 75±3℃. During this process, adjust the frequency converter of the induced draft fan to ensure good fluidization of the material, maintain particle dispersion and fluidization, and prevent agglomeration. Dry until the moisture content of the material reaches 10.2%, then stop the equipment and unload the material.

[0066] 6. The above material is separated by two layers of vibrating screens with a particle size of 40 mesh (0.425 mm) on the top layer and 80 mesh (0.18 mm) on the bottom layer to obtain a low-dust, easily dispersible xanthan gum product with a particle size of 0.180 mm ≤ particle size ≤ 0.425 mm.

[0067] 7. The particles with a diameter > 0.425 mm from step 6 are crushed a second time to ≤ 0.180 mm, and then mixed with the fine powder under an 80-mesh sieve. The mixture will be fed into the wet granulator for secondary granulation in the next batch.

[0068] Example 2: Preparation method of low-dust, easily dispersible xanthan gum

[0069] Includes the following steps:

[0070] 1. Weigh sodium caseinate and diglycerol distearate (HLB value approximately 3.5) at a mass ratio of 3:5. Dissolve them in 81.3% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 8:25 at a dissolution temperature of 67°C. Disperse the solution in a colloid mill to form a light yellow, uniform emulsion for later use.

[0071] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 9.8% at 73±4℃, stop the equipment, and unload the material.

[0072] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0073] 4. The particles with a diameter > 0.425 mm from step 3 are pulverized a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for use in the next batch of granulation.

[0074] Example 3: Preparation method of low-dust, easily dispersible xanthan gum

[0075] Includes the following steps:

[0076] 1. Weigh sodium caseinate and triglyceride monococarboxylate (HLB value approximately 6.0) at a mass ratio of 3:7. Dissolve them in 70.9% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 10:25 at a dissolution temperature of 65°C. Disperse the solution in a light yellow, uniform emulsion using a colloid mill for later use.

[0077] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, at 75±3℃, dry the product to a final moisture content of 10.2%, stop the equipment, and unload the material.

[0078] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0079] 4. The particles with a diameter > 0.425 mm from step 3 are pulverized a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for use in the next batch of granulation.

[0080] Example 4: Preparation method of low-dust, easily dispersible xanthan gum

[0081] Includes the following steps:

[0082] 1. Weigh sodium caseinate and diglycerol monolaurate (HLB value approximately 7.0) at a mass ratio of 3:8. Dissolve them in 78.4% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 11:30 at a dissolution temperature of 67°C. Disperse the solution in a colloid mill to form a light yellow, uniform emulsion for later use.

[0083] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 8.9% at 77±2℃, stop the equipment, and unload the material.

[0084] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0085] 4. The particles with a diameter > 0.425 mm from step 3 are pulverized a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for use in the next batch of granulation.

[0086] Example 5: Preparation method of low-dust, easily dispersible xanthan gum

[0087] Includes the following steps:

[0088] 1. Weigh sodium caseinate and triglyceride monopalmitate (HLB value approximately 8.0) at a mass ratio of 5:8. Dissolve them in 78.4% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 11:25 at a dissolution temperature of 65°C. Disperse the solution in a light yellow, uniform emulsion using a colloid mill for later use.

[0089] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 9.6% at 73±2℃, stop the equipment, and unload the material.

[0090] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0091] 4. The particles with a diameter > 0.425 mm from step 3 are pulverized a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for use in the next batch of granulation.

[0092] Example 6: Preparation method of low-dust, easily dispersible xanthan gum

[0093] Includes the following steps:

[0094] 1. Weigh sodium caseinate and polyglycerol monolaurate (HLB value approximately 11.0) at a mass ratio of 3:8. Dissolve them in 72.4% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 11:30 at a dissolution temperature of 62℃. Disperse the solution in a light yellow, uniform emulsion using a colloid mill.

[0095] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 10.1% at 73±2℃, stop the equipment, and unload the material.

[0096] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0097] 4. The particles with a diameter > 0.425 mm from step 3 are crushed a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for later use.

[0098] Example 7: Preparation method of low-dust, easily dispersible xanthan gum

[0099] Includes the following steps:

[0100] 1. Weigh sodium caseinate and decaglycerol monomyristate (HLB value approximately 13.5) at a mass ratio of 3:7. Dissolve them in 83.4% (v / v) food-grade ethanol solution at a material-to-liquid ratio of 10:15 at a dissolution temperature of 60°C. Disperse the above solution through a colloid mill to form a light yellow, uniform emulsion solution for later use.

[0101] 2. Following steps 2 to 5 in Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 9.9% at 74±3℃, stop the equipment, and unload the material.

[0102] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0103] 4. The particles with a diameter > 0.425 mm from step 3 are crushed a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for later use.

[0104] Comparative Example 1: A pulverized form of common xanthan gum, specifically:

[0105] Take the above-mentioned xanthan gum powder that has been pulverized to a particle size ≤0.18mm (about 80 mesh) and has a moisture content of 10.8%. Compare this sample directly with other examples or comparative samples.

[0106] Comparative Example 2: A method for preparing low-dust, easily dispersible xanthan gum

[0107] Includes the following steps:

[0108] 1. Weigh out sodium caseinate and ethanol (75.4% v / v food-grade ethanol solution) at a ratio of 5g:100mL and dissolve at 65℃. Disperse the solution using a colloid mill to form a light yellow, uniform emulsion for later use.

[0109] 2. Following steps 2-5 of Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 10.9% at 73±5℃, stop the equipment, and unload the material. In Comparative Example 2, the mass ratio of sodium caseinate to xanthan gum powder is 5:1000.

[0110] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0111] 4. The particles with a diameter > 0.425 mm from step 3 are crushed a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for later use.

[0112] Comparative Example 3: A method for preparing low-dust, easily dispersible xanthan gum

[0113] Includes the following steps:

[0114] 1. Weigh out 8g of triglyceride monococarboxylate (HLB value approximately 6.0) and 120mL of ethanol (81.5% (v / v) food-grade ethanol solution) and dissolve at 65℃. Disperse the solution using a colloid mill to form a light yellow, homogeneous emulsion for later use.

[0115] 2. Following steps 2-5 of Example 1, prepare low-dust, easily dispersible xanthan gum. Then, dry the product to a final moisture content of 9.5% at 73±5℃, stop the equipment, and unload the material. In this example, the mass ratio of polyglycerol ester to xanthan gum dry powder is 8:1000.

[0116] 3. The above materials are sieved according to the method in Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0117] 4. The particles with a diameter > 0.425 mm from step 3 are crushed a second time to ≤ 0.180 mm, and then mixed with the fine powder through an 80-mesh sieve for later use.

[0118] Comparative Example 4: A method for preparing low-dust, easily dispersible xanthan gum

[0119] Includes the following steps:

[0120] 1. Take the dried material before pulverization in the above embodiment, weigh monoglyceride and xanthan gum at a mass ratio of 7:1000, pulverize them together and sieve them to obtain xanthan gum samples with a particle size of 120 mesh ≤ 60 mesh for later use.

[0121] 2. The dispersion and solubility properties of the above samples, along with those of other examples and comparative samples, were determined.

[0122] Comparative Example 5: A method for preparing low-dust, easily dispersible xanthan gum

[0123] Includes the following steps:

[0124] 1. Take the dried material used in the above embodiment before crushing, crush it with a crusher and sieve it to obtain xanthan gum samples with a particle size of 80 mesh ≤ 40 mesh for later use.

[0125] 2. The dispersion and solubility properties of the above samples, along with those of other examples and comparative samples, were determined.

[0126] Comparative Example 6: A method for preparing low-dust, easily dispersible xanthan gum

[0127] 1. Referring to Example 2 of CN102219912B, a fluidized bed granulation device was used to prepare particulate xanthan gum samples, and the obtained materials were sieved according to the method of Example 1 to obtain a low-dust, easily dispersible xanthan gum product.

[0128] 2. The dispersion and solubility properties of the above samples, along with those of other examples and comparative samples, were determined.

[0129] The dissolution curves of all samples obtained from the examples and comparative examples, and the results of the dispersion and dissolution performance tests, are as follows: Figure 1 As shown.

[0130] The tack-forming time and sample dissolution slope of the above embodiments and comparative examples are shown in Table 1:

[0131] Table 1

[0132]

[0133]

[0134] The particle size distribution and dust content of the product were measured, and the results are shown in Table 2.

[0135] Table 2

[0136] Sample Name 20-mesh pass rate % 80 mesh pass rate % 140 mesh pass rate % standard ＞95.0 ≤20.0 ≤5.0 Example 1 99.87±0.13 12.58±0.72 1.88±0.23 Example 2 99.93±0.05 12.87±0.49 1.65±0.43 Example 3 99.89±0.03 11.86±0.82 2.73±0.69 Example 4 99.92±0.02 11.97±0.23 2.47±0.72 Example 5 99.95±0.01 10.92±0.96 1.92±0.46 Example 6 99.92±0.03 12.45±0.27 1.72±0.88 Example 7 99.93±0.01 11.89±1.02 2.23±0.63 Comparative Example 1 100.00±0.00 98.67±0.25 72.77±4.25 Comparative Example 2 99.89±0.05 13.17±0.64 2.31±0.38 Comparative Example 3 99.91±0.03 11.25±1.26 2.17±0.51 Comparative Example 4 99.97±0.01 57.23±0.64 12.97±1.08 Comparative Example 5 99.89±0.03 13.12±0.77 2.90±0.53 Comparative Example 6 99.87±0.02 11.95±0.47 1.94±0.77

[0137] The different dissolution results of some of the above-mentioned embodiments and comparative samples after measurement are shown in the figure. Figure 2 In the figure, No. 1 represents the solution state of Comparative Example 1 after being measured by a rheometer, No. 2 represents the dissolution state of the product of Example 1, No. 3 represents the dissolution state of the product of Example 7, and No. 4 represents the dissolution state of the product of Comparative Example 6.

[0138] The experimental results above show that both sodium caseinate and polyglycerol fatty acid esters with suitable HLB values ​​can improve the dispersion and dissolution rate of xanthan gum products. However, this invention creatively combines the two, resulting in a low-dust, easily dispersible xanthan gum with better dispersion and dissolution performance than products obtained by using a single component alone or by current technologies. This is mainly reflected in: earlier product tackification time, faster tackification speed, fewer fish eyes in the obtained product, and a more homogeneous solution. It also has advantages such as simple production conditions, convenient operation, and low dust content, demonstrating excellent production and application feasibility.

[0139] Although the present invention has been described in detail above with general descriptions and specific embodiments, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention fall within the scope of protection claimed by the present invention.

Claims

1. A method for preparing low-dust, easily dispersible xanthan gum, characterized in that, Includes the following steps: (1) Weigh sodium caseinate and polyglycerol fatty acid ester at a mass ratio of (1~5): (3~8), add 60-85% v / v food grade ethanol solution at a material-liquid ratio of (4~13): (10~45) to dissolve, dissolve at a temperature of 50~75℃, and then process by a colloid mill to form a light yellow to white emulsion. The polyglycerol fatty acid ester has an HLB value of 2.0 to 11.

0. (2) The xanthan gum powder that has been crushed to a particle size ≤0.18mm is fed into a wet granulator for stirring and shearing; (3) Add the emulsion from step (1) into the above wet granulation machine and continue to stir and shear to obtain fine granules; wherein, the amount of emulsion added is calculated based on sodium caseinate and the mass ratio of it to xanthan gum is (1~5):1000. (4) The fine granular material from step (3) is transferred to a fluidized bed granulator via negative pressure conveying and dried at 75±5℃ until the moisture content of the material is ≤13%; (5) The dried material was separated by two layers of vibrating screens with particle sizes of 40 mesh and 80 mesh, respectively, to obtain a low dust and easily dispersible xanthan gum product with a particle size of 0.180 mm ≤ particle size ≤ 0.425 mm.

2. The method according to claim 1, characterized in that, The polyglycerol fatty acid ester has an HLB value of 2.5 to 8.

0.

3. The method according to claim 1, characterized in that, The polyglycerol fatty acid ester is selected from at least one or a combination of polyglycerol stearate, polyglycerol isostearate, polyglycerol oleate, polyglycerol laurate, polyglycerol palmitate, polyglycerol caprylate, polyglycerol decanoate, polyglycerol caprylate-decanoate, polyglycerol ricinoleate, and polyglycerol cocoate.

4. The method according to any one of claims 1-3, characterized in that, The method further includes: mixing the fine powder with a particle size <0.180mm from step (5) and the fine powder with a particle size >0.425mm that has been pulverized twice to ≤0.180mm, and performing secondary wet granulation and sieving to obtain a low-dust, easily dispersible xanthan gum product.

5. A low-dust, easily dispersible xanthan gum product prepared according to any one of claims 1-4.

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