A dispersed xanthan gum and its preparation method

The problem of inaccurate dispersant spraying is solved by heating steam condensation and adhesion, and efficient dispersion performance and low-cost production are achieved, which is suitable for the preparation of food-grade xanthan gum.

CN116041742BActive Publication Date: 2025-08-01RIZHAO HENGTAI ENVIRONMENTAL PROTECTION TECH CO LTD
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Patent Information

Application Number
CN202310088951.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-02-09
Publication Date
2025-08-01
Estimated Expiration
2043-02-09

AI Technical Summary

Technical Problem

In the existing preparation process, the amount of dispersant spraying is difficult to accurately match, resulting in unqualified dispersion or reduced viscosity, and the inability to produce food-grade xanthan gum, which has a large amount of dispersant and high cost.

Method used

The method of generating steam by heating and pressing it into the material through pressure to condense and adhere to it, so that the material and steam can be mixed quickly and evenly, reducing the amount of dispersant used, and improving dispersion performance.

Benefits of technology

It achieves excellent dispersing properties of dispersed xanthan gum, reduces production costs, and can produce food-grade xanthan gum.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The present invention discloses a dispersed xanthan gum and a preparation method thereof. The preparation method comprises the following steps: adding sodium bicarbonate and calcium chloride to xanthan gum and mixing evenly to obtain a mixed material; under stirring conditions, introducing a dispersant vapor into the mixed material by compressed air for condensation and attachment; after the condensation and attachment are completed, sampling and detecting that the salt tolerance value drops by no more than 1 cp and the D value does not exceed 5 agglomerates, then it is determined to be qualified, and then packaging can be carried out. In the preparation method of the present invention, the dispersant is heated to generate vapor, and then the vapor is pressed into the material by pressure and quickly diffuses, condenses and attaches to the material, so that the material and the vapor are quickly and evenly mixed in a short time. Therefore, this method can fully reduce the usage amount of the dispersant, reduce the production cost, cause little damage to the salt tolerance index, and make the prepared dispersed xanthan gum have excellent dispersibility.
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Description

Technical Field

[0001] The present invention relates to the technical field of xanthan gum preparation, and specifically relates to a dispersed xanthan gum and a preparation method thereof. Background Art

[0002] When producing dispersed xanthan gum, xanthan gum manufacturers subject the centrifuged fibrous xanthan gum to pressing, control the material humidity at 40-60%, then crush the material through a crushing device, dissolve the dispersing agent in a solvent, then spray the mixture of the dispersing agent and the solvent into the material, and then obtain the dispersed xanthan gum through drying, pulverizing, and sieving processes.

[0003] However, the existing preparation process has the following problems: 1. In the existing preparation process, the material after pressing is crushed and then sprayed into the dispersing agent solution. It is difficult to accurately match the spraying amount of the dispersing agent solution with the amount of the material. Moreover, after drying and pulverizing, the 200-mesh particles obtained through sieving and crushing are small and difficult to meet the requirements. In addition, too little spraying of the dispersing agent results in unqualified dispersibility, while excessive spraying of the dispersing agent leads to a decrease in viscosity index and pH value, affecting the use effect; 2. The dispersing agent enters the solvent system, resulting in the presence of industrial-grade dispersing agent in the whole system and making it impossible to produce food-grade xanthan gum; 3. When using the original process to produce dispersed xanthan gum, the amount of dispersing agent used is large and the cost is relatively high. Summary of the Invention

[0004] The purpose of the present invention is to provide a dispersed xanthan gum and a preparation method thereof. In this preparation method, the dispersing agent is heated to generate steam, and then the steam is pressed into the material under pressure and quickly diffuses, condenses, and adheres to the material, so that the material and the steam are quickly and evenly mixed in a short time. Therefore, this method can fully reduce the amount of dispersing agent used and make the prepared dispersed xanthan gum have excellent dispersibility.

[0005] In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:

[0006] The first aspect of the present invention provides a preparation method of a dispersed xanthan gum, which is characterized by including the following steps:

[0007] (a) Adding sodium bicarbonate and calcium chloride to xanthan gum and mixing evenly to obtain a mixed material;

[0008] (b) Under stirring conditions, introducing the dispersing agent steam into the mixed material by compressed air for condensation and adhesion;

[0009] (c) After the condensation and adhesion are completed, take a sample for detection. If the decrease in the salt tolerance value does not exceed 1 cp and the D value does not exceed 5 agglomerates, it is determined to be qualified. Then, it can be packaged.

[0010] Preferably, the mass ratio of xanthan gum, sodium bicarbonate and calcium chloride is 1000∶(2 - 4)∶(4 - 6).

[0011] Preferably, the mesh size of the xanthan gum is 40 - 100 mesh.

[0012] Preferably, the mesh sizes of both sodium bicarbonate and calcium chloride are not less than 100 mesh.

[0013] Preferably, the calcium chloride is anhydrous calcium chloride or calcium chloride dihydrate;

[0014] When the calcium chloride is calcium chloride dihydrate, the mass ratio of xanthan gum and calcium chloride is 1000∶(5.2 - 7.8).

[0015] Preferably, the dispersant is a 40% - 50% glyoxal solution.

[0016] Preferably, the pressure of the compressed air is 0.05 - 0.07 Mpa.

[0017] Preferably, the mass ratio of the dispersant to xanthan gum is 4∶(900 - 1100).

[0018] Preferably, the pH value of the xanthan gum is 6 - 8.

[0019] The second aspect of the present invention provides a dispersed xanthan gum prepared by the above preparation method.

[0020] Compared with the prior art, the beneficial effects of the present invention at least include:

[0021] In the preparation method of the present invention, the dispersant generates steam through heating, and then the steam is pressed into the material by pressure and quickly diffuses, condenses and adheres to the material, so that the material and the steam are quickly and uniformly mixed in a short time. Therefore, this method can fully reduce the usage amount of the dispersant, reduce the production cost, and make the prepared dispersed xanthan gum have excellent dispersion performance.

[0022] In the preparation method of the present invention, whether the dispersant is solid or liquid can be used, and it can significantly improve the dispersion effect, making the prepared xanthan gum not only free of agglomeration in the existing brine, but also achieving the effect of no agglomeration in fresh water. Specific Embodiments

[0023] Hereinafter, the embodiments of the technical solution of the present invention will be described in detail. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, so they are only examples and cannot be used to limit the protection scope of the present invention.

[0024] It should be noted that, unless otherwise specified, the technical terms or scientific terms used in this application shall have the ordinary meanings understood by those skilled in the art to which the present invention pertains.

[0025] The raw materials used in the following examples can all be obtained through ordinary commercial channels;

[0026] Xanthan gum: pH value 5.86, salt tolerance value 18 cp, obtained commercially.

[0027] Example 1

[0028] This example is a preparation method of a dispersed xanthan gum, and the preparation method is obtained by including the following steps:

[0029] (a) Convey 2 t of 40-mesh xanthan gum powder into a horizontal mixing tank through a screw conveyor, turn on the main stirrer and side stirrer, add 2 kg of sodium bicarbonate and 4 kg of calcium chloride during the conveying process and mix evenly to obtain a mixed material, wherein the mesh sizes of sodium bicarbonate and calcium chloride are not less than 100 mesh;

[0030] (b) Inject 3 kg of 40% glyoxal solution into a heating tank, turn on the heating rod and heat to 60 °C, then fill 0.05 Mpa of compressed air into the glyoxal container, so that the steam is introduced into the horizontal mixing tank under pressure, and the steam can quickly and widely contact the material, condense and adhere to the surface of the material, and at the same time, mix evenly through the stirring of the plow knife and side stirring blades;

[0031] (c) After the condensation adhesion ends, take a sample to detect that the salt tolerance value drops by no more than 1 cp and the D value does not exceed 5 agglomerations, then it is judged to be qualified, and then it can be packaged.

[0032] Example 2

[0033] This example is a preparation method of a dispersed xanthan gum, and the preparation method is obtained by including the following steps:

[0034] (a) Convey 2 t of 80-mesh xanthan gum powder into a horizontal mixing tank through a screw conveyor, turn on the main stirrer and side stirrer, add 3 kg of sodium bicarbonate and 5 kg of calcium chloride during the conveying process and mix evenly to obtain a mixed material, wherein the mesh sizes of sodium bicarbonate and calcium chloride are not less than 100 mesh;

[0035] (b) Inject 3 kg of 50% glyoxal solution into a heating tank, turn on the heating rod and heat to 50 °C, then fill 0.07 Mpa of compressed air into the glyoxal container, so that the steam is introduced into the horizontal mixing tank under pressure, and the steam can quickly and widely contact the material, condense and adhere to the surface of the material, and at the same time, mix evenly through the stirring of the plow knife and side stirring blades;

[0036] (c) After the condensation and adhesion are completed, take a sample for testing. If the decrease in the salt tolerance value does not exceed 1 cp and the D value does not exceed 5 agglomerates, it is judged as qualified. Then, it can be packaged.

[0037] Example 3

[0038] This example is a preparation method of a dispersed xanthan gum. The preparation method is obtained by including the following steps:

[0039] (a) Convey 2 t of 40-mesh xanthan gum powder into a horizontal mixing tank through a screw conveyor, and turn on the main stirrer and side stirrer. During the conveying process, add 4 kg of sodium bicarbonate and 6 kg of calcium chloride and mix evenly to obtain a mixed material. Among them, the mesh size of sodium bicarbonate and calcium chloride is not less than 100 mesh;

[0040] (b) Inject 3 kg of 45% glyoxal solution into a heating tank, turn on the heating rod to heat to 55 °C, and then fill 0.06 Mpa of compressed air into the glyoxal container, so that the steam is introduced into the horizontal mixing tank under pressure. The steam can quickly and widely contact the material, condense and adhere to the surface of the material, and at the same time, it is evenly mixed through the stirring of the plow knife and the side stirring blade;

[0041] (c) After the condensation and adhesion are completed, take a sample for testing. If the decrease in the salt tolerance value does not exceed 1 cp and the D value does not exceed 5 agglomerates, it is judged as qualified. Then, it can be packaged.

[0042] Comparative Example 1

[0043] This comparative example is a preparation method of a dispersed xanthan gum. The preparation method is obtained by including the following steps:

[0044] (a) Convey 2 t of 40-mesh xanthan gum powder into a horizontal mixing tank through a screw conveyor, and turn on the main stirrer and side stirrer. During the conveying process, add 4 kg of sodium bicarbonate and 6 kg of calcium chloride and mix evenly to obtain a mixed material. Among them, the mesh size of sodium bicarbonate and calcium chloride is not less than 100 mesh;

[0045] (b) Under stirring conditions, spray 3 kg of 45% glyoxal solution on the surface of the mixed material, and at the same time, it is evenly mixed through the stirring of the plow knife and the side stirring blade;

[0046] (c) After the condensation and adhesion are completed, it can be packaged.

[0047] Experimental Example 1

[0048] Comparison between the preparation process of this application and the traditional preparation process: The traditional preparation process is as follows:

[0049] Dissolve the dispersant in ethanol at about 80°C, spray it onto the product at a ratio of 20 kg of 40% dispersant per ton of product, and then obtain the required dispersed xanthan gum after drying, crushing, and sieving.

[0050] The product indexes of the traditional preparation process are shown in Table 1:

[0051] Table 1

[0052]

[0053]

[0054] The product indexes of the preparation method in Example 3 of this application are shown in Table 2:

[0055] Table 2

[0056] [[ID=2�]]

[0057] As can be seen from Table 1 and Table 2:

[0058] For the traditional process, 15 - 25 kg of dispersant is used to process one ton of finished product, while the preparation process of this application uses 4 - 5 kg; the indexes of the traditional process decrease by an average of 1.8 cp, and the indexes of the preparation process of this application decrease by 0.2 cp. The dispersibility qualification rate of the traditional process is 83.3%, and the qualification rate of the preparation process of this application is 100%.

[0059] Experimental Example 2

[0060] Prepare dispersed xanthan gum according to the methods of Example 3 and Comparative Example 1 respectively, and then detect the dissolution of dispersed xanthan gum in sodium chloride and calcium chloride solutions, as well as the solution viscosity of dispersed xanthan gum in seawater solution, respectively, according to the following methods. The detection methods are as follows:

[0061] The detection method for the dissolution of dispersed xanthan gum in sodium chloride and calcium chloride solutions is as follows:

[0062] 1. Weigh 2.00 ± 0.01 g of the sample, 2.00 g of sodium chloride, and 0.2 g of anhydrous calcium chloride separately with a clean and dry weighing paper, mix them evenly and pour them into a reagent bottle, measure 2000 ml of distilled water, and stir evenly;

[0063] 2. Measure 198 ml of the above reagent;

[0064] 3. Place the flask containing the reagent under a stirrer, adjust the paddle to 1.0 - 1.5 cm from the bottom of the cup, install a funnel; the inclination angle is 45 degrees, turn on the stirrer, adjust the rotation speed to 800 rmp / min, add the sample into the reagent within 15 seconds, continue stirring for 30 seconds, then immediately stop stirring, pour the product evenly onto a 20 - mesh sieve, and observe the undissolved product particles.

[0065] The detection method for the dissolution of dispersed xanthan gum in fresh water is as follows:

[0066] 1. Weigh 2.00 ± 0.01 g of the sample separately using a clean and dry weighing paper, pour it into a reagent bottle, measure 2000 ml of distilled water, and stir evenly;

[0067] 2. Measure 198 ml of the above reagent;

[0068] 3. Place the flask containing the reagent under a stirrer, adjust the paddle to 1.0 - 1.5 cm from the bottom of the cup, install a funnel; the inclination angle is 45 degrees, turn on the stirrer, adjust the rotation speed to 800 rmp / min, add the sample into the reagent within 15 seconds, continue stirring for 30 seconds, then immediately stop stirring, pour the sample evenly onto a 20 - mesh sieve, and observe the undissolved product particles.

[0069] The method for measuring the solution viscosity of dispersed xanthan gum in seawater solution:

[0070] 1. Weigh 1 g of the sample using a clean and dry weighing paper, accurate to 0.0001 g;

[0071] 2. Accurately weigh 358 g of synthetic seawater solution into a mixer;

[0072] 3. Turn on the stirrer and increase the stirring speed, which can be controlled to submerge the paddle in water (about 8000 rpm), and slowly add the sample into the water between the stirring blade and the cup wall;

[0073] 4. Stir for 5 ± 0.5 minutes, take out the container and stir, use a spatula to scrape the xanthan gum powder or lumps sticking to the stirring shaft and the inner wall of the stirring cup into the solution;

[0074] 5. Slowly increase the stirring speed when the viscosity increases, and control the speed at 11000 rmp / min ± 200 rpm; stir for 30 minutes, add 1 - 3 drops of defoaming agent and continue stirring for 0.5 minutes;

[0075] 6. Stop stirring, remove the cup, transfer the solution to a 400 - ml beaker, cover the beaker, keep it at a constant temperature of 25 ± 0.5 °C in a water bath, and adjust the temperature within no more than 30 minutes;

[0076] Measurement:

[0077] Use a Fann 35A (f = 0.2) viscometer to measure the viscosity values at a rotation speed of 3 rpm respectively;

[0078] Make 4 replicates respectively, and the test results are shown in Table 3:

[0079] Table 3

[0080]

[0081] As can be seen from Table 3:

[0082] The dispersible xanthan gum prepared by the technical solution of this application has excellent dispersion performance in both brine and fresh water. However, the dispersible xanthan gum prepared by the comparative example also has a certain degree of dispersion, but its dispersion performance is worse than that of the technical solution of this application, especially the dispersion effect in fresh water. In addition, the salt tolerance in the original table refers to the 3-rotation viscosity of 0.285% xanthan gum in seawater brine. As can be seen from the data in Table 3, the technical solution of this application has better salt tolerance than the comparative example.

[0083] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features. And these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be covered within the scope of the claims and the description of the present invention.

Claims

1. A preparation method of a dispersed xanthan gum, characterized in that, It includes the following steps: (a) Add sodium bicarbonate and calcium chloride to xanthan gum and mix evenly to obtain a mixed material; (b) Under stirring conditions, introduce dispersant vapor into the mixed material by compressed air for condensation and adhesion. The dispersant is a 40% - 50% glyoxal solution; (c) After the condensation and adhesion are completed, take a sample for testing. If the salt tolerance value drops by no more than 1 cp and the D value does not exceed 5 agglomerations, it is judged to be qualified. Then, it can be packaged.

2. The preparation method according to claim 1, characterized in that, The mass ratio of the xanthan gum, sodium bicarbonate, and calcium chloride is 1000∶(2 - 4)∶(4 - 6).

3. The preparation method according to claim 1, characterized in that, The mesh size of the xanthan gum is 40 - 100 meshes.

4. The preparation method according to claim 1, characterized in that, The mesh sizes of both the sodium bicarbonate and calcium chloride are not less than 100 meshes.

5. The preparation method according to claim 1, characterized in that, The calcium chloride is anhydrous calcium chloride or calcium chloride dihydrate; When the calcium chloride is calcium chloride dihydrate, the mass ratio of the xanthan gum and calcium chloride is 1000∶(5.2 - 7.8).

6. The preparation method according to claim 1, characterized in that, The pressure of the compressed air is 0.05 - 0.07 Mpa.

7. The preparation method according to claim 1, characterized in that, The mass ratio of the dispersant to the xanthan gum is 4∶(900 - 1100).

8. The preparation method according to claim 1, wherein The pH value of the xanthan gum is 5 - 8.

9. Dispersed xanthan gum prepared by the preparation method according to any one of claims 1 - 8.

Citation Information

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