Highly hydrophobic, anti-caking starch and process for its preparation

By cross-linking a composite intermediate of plant polyphenol nanoaggregates, soybean polypeptide hydrophobic aggregates, and chitosan, the problem of natural starch easily caking was solved, and highly hydrophobic and anti-caking starch was prepared, improving starch flowability and antioxidant properties, and extending the storage stability of food.

CN122302381APending Publication Date: 2026-06-30QINHUANGDAO JIZHONG FOOD CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
QINHUANGDAO JIZHONG FOOD CO LTD
Filing Date
2026-05-13
Publication Date
2026-06-30

AI Technical Summary

Technical Problem

Natural starch granules contain a large number of hydrophilic hydroxyl groups on their surface, resulting in strong hygroscopicity. They easily absorb moisture from the environment and clump together, affecting the product's flowability, solubility, and ease of use. Existing chemical modification methods involve complex reactions and potential residual reagent problems.

Method used

A composite intermediate was constructed using plant polyphenol nanoaggregates, soybean polypeptide hydrophobic aggregates, and chitosan. Combined with food-grade citric acid crosslinking, a highly hydrophobic and anti-caking starch was prepared through a surface coating process, which enhanced the structural stability of the intermediate and achieved hydrophobic protection of the starch granules.

Benefits of technology

It significantly improves the hydrophobic persistence, anti-caking properties and antioxidant properties of starch, forms a uniform and stable protective layer, and extends the storage stability of food.

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Abstract

This invention discloses a highly hydrophobic and anti-caking starch and its preparation process, belonging to the field of starch preparation technology. It is prepared using the following raw materials in parts by weight: 30-35 parts starch, 11-13.3 parts octenyl succinate starch ester, 2.1-3.5 parts plant polyphenol nanoaggregates, 5.6-7.3 parts plant polypeptide hydrophobic aggregates, 2.2-3.1 parts chitosan, 0.3-1 parts anti-caking agent, and 0.1-0.13 parts food-grade crosslinking agent. Through the above method, this invention constructs a composite intermediate using plant polyphenol nanoaggregates, soybean polypeptide hydrophobic aggregates, and chitosan. The stability of the intermediate structure is increased by crosslinking with food-grade citric acid. A surface coating process is then used to obtain a functional dry powder. This functional dry powder binds to starch particles, achieving hydrophobic protection of the starch particle surface.
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Description

Technical Field

[0001] This invention relates to the field of starch preparation technology, specifically to highly hydrophobic and anti-caking starch and its preparation process. Background Technology

[0002] Starch has a wide range of applications in gummy candy production. It can be used as a mold, such as a cornstarch mold, where starch is used to press the mold cavity, pour in the sugar paste, and then shape and demold the gummy candy. At the same time, starch can also prevent the gummy candy from sticking, provide moderate moisture protection, and isolate oxygen.

[0003] However, natural starch granules contain a large number of hydrophilic hydroxyl groups on their surface, which makes them highly hygroscopic and prone to absorbing moisture from the environment, causing clumping. This seriously affects the product's flowability, solubility, and ease of use.

[0004] In existing technologies, chemical modification is commonly used to hydrophobize starch. However, while chemical grafting modification results in strong bonds, it often involves complex chemical reactions and potential reagent residue issues.

[0005] Based on this, the present invention designs a highly hydrophobic and anti-caking starch and its preparation process to solve the above problems. Summary of the Invention

[0006] In view of the above-mentioned shortcomings of the existing technology, the present invention provides a highly hydrophobic and anti-caking starch and its preparation process.

[0007] To achieve the above objectives, the present invention provides the following technical solution:

[0008] The highly hydrophobic and anti-caking starch is prepared from the following raw materials in parts by weight: 30-35 parts starch, 11-13.3 parts octenyl succinate starch ester, 2.1-3.5 parts plant polyphenol nano-aggregates, 5.6-7.3 parts plant polypeptide hydrophobic aggregates, 2.2-3.1 parts chitosan, 0.3-1 parts anti-caking agent, and 0.1-0.13 parts food-grade crosslinking agent.

[0009] Furthermore, the starch used is corn starch.

[0010] Furthermore, the plant polypeptide hydrophobic aggregate is a soybean polypeptide hydrophobic aggregate.

[0011] Furthermore, the anti-caking agent is made of food-grade silica.

[0012] Furthermore, the food-grade crosslinking agent is food-grade citric acid.

[0013] Furthermore, the preparation method of the plant polyphenol nano-aggregates is as follows: green tea and boiling water are brewed at a mass ratio of 1:50-120, filtered to obtain tea soup, and soda ash and salt are added to the tea soup at a mass ratio of 5:8-11. After dissolving, the tea soup is filtered using a filter membrane with a pore size of 0.22μm. The filter residue is dried and pulverized to obtain tea polyphenol self-assembled nano-aggregates.

[0014] To better achieve the objectives of this invention, the present invention also provides a process for preparing highly hydrophobic and anti-caking starch, comprising the following steps:

[0015] (1) Prepare dispersions of plant polyphenol nano-aggregates, chitosan solution and plant polypeptide hydrophobic aggregates;

[0016] (2) Add the plant polypeptide hydrophobic aggregate dispersion to the plant polyphenol nano-aggregate dispersion and stir evenly to obtain the first mixture for later use;

[0017] (3) Adjust the pH of the first mixture to 4.8-5.5, slowly add the chitosan solution to the first mixture, and stir until homogeneous to obtain the second mixture;

[0018] (4) Add food-grade crosslinking agent to the second mixture, stir and crosslink, and then freeze dry to obtain functional dry powder;

[0019] (5) Take the functional dry powder, octenyl succinic starch ester and anti-caking agent, put them in a high-speed mixer and stir to complete the pre-coating of the powder surface;

[0020] (6) Add starch to the pre-coated functional dry powder and stir; finally, dry, crush and sieve the mixed powder to obtain highly hydrophobic and anti-caking starch.

[0021] Furthermore, step (1) specifically involves:

[0022] Plant polyphenol nanoaggregates were added to deionized water and incubated at 35-40℃ and 500-650 rpm. -1 Stir for 20-30 minutes to prepare a dispersion of plant polyphenol nano-aggregates.

[0023] Take chitosan, add 1-2% (v / v) of food-grade dilute acetic acid solution, stir to dissolve until a transparent solution is obtained, and prepare a chitosan solution with a mass concentration of 2-3%.

[0024] Add hydrophobic aggregates of plant polypeptides to deionized water and incubate at 40-45℃ and 800-950 rpm. -1 Stir for 50-68 minutes to prepare a dispersion of plant polypeptide hydrophobic aggregates.

[0025] Furthermore, in step (2), at 40-43℃ and 700-800 r·min -1 Stir for 15-20 minutes to obtain the first mixture; in step (3), stir at 40-43℃ and 600-750 r·min. -1 Stir for 25-33 minutes to obtain the second mixture; in step (4), stir at 50-55℃ and 200-250 r·min. -1 Stir for 1.5-2 hours; in step (5), the stirring speed is 800-850 r·min. -1 Stir for 15-23 minutes; in step (6), the stirring speed is 600-750 r·min. -1 Stir for 25-30 minutes.

[0026] To better achieve the objectives of this invention, this invention also provides a highly hydrophobic and anti-caking starch, prepared using the aforementioned preparation process.

[0027] Compared to existing technologies, the advantages of this invention are as follows: This invention constructs a composite intermediate using plant polyphenol nanoaggregates, soybean polypeptide hydrophobic aggregates, and chitosan. The stability of the intermediate structure is increased through cross-linking with food-grade citric acid. A surface coating process is then used to obtain a functional dry powder, which binds to starch granules, achieving hydrophobic protection of the starch granules' surface. Specifically, the introduction of a cross-linking agent significantly enhances the structural stability of the intermediate; the introduction of an anti-caking agent further improves the product's flowability; and the introduction of plant polyphenol nanoaggregates further enhances the product's antioxidant properties. The overall solution works synergistically to significantly improve the hydrophobic persistence, anti-caking properties, and antioxidant properties of starch.

[0028] The powder of this invention can be used as a starch mold, and at the same time, it can form a uniform and stable protective layer on the surface of foods such as gummies, effectively locking in the moisture of the gummies, delaying oxidation and deterioration, and helping to extend the storage stability of foods such as gummies. Detailed Implementation

[0029] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0030] Example 1: A method for preparing highly hydrophobic and anti-caking starch, comprising the following steps:

[0031] (1) Preparation of plant polyphenol nano-aggregates: green tea and boiling water were brewed at a mass ratio of 1:50 and filtered to obtain tea soup. Soda ash and salt were added to the tea soup at a mass ratio of 5:8. After dissolving, the tea soup was filtered using a filter membrane with a pore size of 0.22 μm. The filter residue was dried and pulverized to obtain tea polyphenol self-assembled nano-aggregates.

[0032] (2) Raw material pretreatment:

[0033] Take 2.1 parts of plant polyphenol nanoaggregates and add them to 40 parts of deionized water, and incubate at 35℃ and 500 r·min. -1 Stir for 20 minutes to prepare a dispersion of plant polyphenol nano-aggregates;

[0034] Take 2.2 parts of chitosan, add 1% (v / v) of food-grade dilute acetic acid solution, stir to dissolve until a clear solution is obtained, and prepare a chitosan solution with a mass concentration of 2%.

[0035] Take 5.6 parts of soybean polypeptide hydrophobic aggregates and add them to 60 parts of deionized water, and incubate at 40℃ and 800 r·min. -1 Stir for 50 minutes to prepare a dispersion of plant polypeptide hydrophobic aggregates.

[0036] (3) Add the plant polypeptide hydrophobic aggregate dispersion to the plant polyphenol nanoaggregate dispersion and heat at 40℃ and 700 r·min -1 Stir for 15 minutes to obtain the first mixture, set aside.

[0037] (4) Adjust the pH of the first mixture (e.g., food-grade dilute acetic acid) to 4.8, and slowly add the chitosan solution to the first mixture. Then, heat the mixture at 40°C and 600 rpm. -1 Stir for 25 minutes to obtain the second mixture;

[0038] (5) Add 0.1 part of food-grade citric acid to the second mixture and heat at 50°C and 200 r·min. -1 The mixture was stirred for 1.5 hours and then freeze-dried to obtain a functional powder.

[0039] (6) Take functional dry powder, 11 parts of octenyl succinate starch ester and 0.3 parts of food-grade silica, and heat them at room temperature and 800 r·min -1 Stir for 15 minutes to complete the pre-coating of the powder surface;

[0040] (7) Add 30 parts of corn starch to the above pre-coated functional dry powder and heat at room temperature and 600 r·min -1 Stir for 25 minutes; finally, dry the mixed powder to a moisture content of ≤5%, and after drying, crush and sieve to obtain highly hydrophobic and anti-caking starch.

[0041] Example 2: A method for preparing highly hydrophobic and anti-caking starch, comprising the following steps:

[0042] (1) Preparation of plant polyphenol nano-aggregates: green tea and boiling water were brewed and filtered to obtain tea soup. Soda ash and salt were added to the tea soup at a mass ratio of 5:11. After dissolving, the tea soup was filtered using a filter membrane with a pore size of 0.22 μm. The filter residue was dried and pulverized to obtain tea polyphenol self-assembled nano-aggregates.

[0043] (2) Raw material pretreatment:

[0044] Take 3.5 parts of plant polyphenol nanoaggregates and add them to 80 parts of deionized water, and incubate at 40℃ and 650 r·min. -1 Stir for 30 minutes to prepare a dispersion of plant polyphenol nano-aggregates;

[0045] Take 3.1 parts of chitosan, add 2% (v / v) of food-grade dilute acetic acid solution, stir to dissolve until a clear solution is obtained, and prepare a chitosan solution with a mass concentration of 3%.

[0046] Take 7.3 parts of soybean polypeptide hydrophobic aggregates and add them to 120 parts of deionized water, and incubate at 45℃ and 950 r·min. -1 Stir for 68 minutes to prepare a dispersion of plant polypeptide hydrophobic aggregates.

[0047] (3) Add the plant polypeptide hydrophobic aggregate dispersion to the plant polyphenol nanoaggregate dispersion and incubate at 43℃ and 800 r·min -1 Stir for 20 minutes to obtain the first mixture, set aside for later use;

[0048] (4) Adjust the pH of the first mixture to 5.5, and slowly add the chitosan solution to the first mixture. Incubate at 43°C and 750 r·min. -1 Stir for 33 minutes to obtain the second mixture;

[0049] (5) Add 0.13 parts of food-grade citric acid to the second mixture and heat at 55℃ and 250 r·min -1 The mixture was stirred for 2 hours and then freeze-dried to obtain a functional powder.

[0050] (6) Take functional dry powder, 13.3 parts of octenyl succinate starch ester and 1 part of food-grade silica, and heat them at room temperature and 850 r·min -1 Stir for 23 minutes to complete the pre-coating of the powder surface;

[0051] (7) Add 35 parts of corn starch to the above pre-coated functional dry powder and heat at room temperature and 750 r·min -1Stir for 30 minutes; finally, dry the mixed powder to a moisture content of ≤5%, and after drying, crush and sieve to obtain highly hydrophobic and anti-caking starch.

[0052] Example 3: A method for preparing highly hydrophobic and anti-caking starch, comprising the following steps:

[0053] (1) Preparation of plant polyphenol nano-aggregates: green tea and boiling water were brewed and filtered to obtain tea soup. Soda ash and salt were added to the tea soup at a mass ratio of 5:10. After dissolving, the tea soup was filtered using a filter membrane with a pore size of 0.22 μm. The filter residue was dried and pulverized to obtain tea polyphenol self-assembled nano-aggregates.

[0054] (2) Raw material pretreatment:

[0055] Take 2.8 parts of plant polyphenol nanoaggregates and add them to 65 parts of deionized water, and incubate at 38℃ and 550 r·min. -1 Stir for 25 minutes to prepare a dispersion of plant polyphenol nano-aggregates;

[0056] Take 2.6 parts of chitosan, add 1.6% (v / v) of food-grade dilute acetic acid solution, stir to dissolve until a clear solution is obtained, and prepare a chitosan solution with a mass concentration of 2.5%.

[0057] Take 6.6 parts of soybean polypeptide hydrophobic aggregates and add them to 90 parts of deionized water, and incubate at 42℃ and 850 r·min. -1 Stir for 58 minutes to prepare a dispersion of plant polypeptide hydrophobic aggregates.

[0058] (3) Add the plant polypeptide hydrophobic aggregate dispersion to the plant polyphenol nanoaggregate dispersion and heat at 42℃ and 750 r·min -1 Stir for 18 minutes to obtain the first mixture, set aside.

[0059] (4) Adjust the pH of the first mixture to 5.2, and slowly add the chitosan solution to the first mixture. Incubate at 41°C and 650 r·min. -1 Stir for 30 minutes to obtain the second mixture;

[0060] (5) Add 0.11 parts of food-grade citric acid to the second mixture and heat at 52℃ and 220 r·min -1 The mixture was stirred for 1.8 hours and then freeze-dried to obtain a functional powder.

[0061] (6) Take functional dry powder, 12 parts of octenyl succinate starch ester and 0.5 parts of food-grade silica, and heat them at room temperature and 820 r·min -1 Stir for 20 minutes to complete the pre-coating of the powder surface;

[0062] (7) Add 32 parts of corn starch to the above pre-coated functional dry powder and heat at room temperature and 650 r·min -1 Stir for 28 minutes; finally, dry the mixed powder to a moisture content of ≤5%, and after drying, crush and sieve to obtain highly hydrophobic and anti-caking starch.

[0063] Comparative Example 1: The crosslinking treatment step (step 5) is omitted, and the remaining steps are the same as in Example 3.

[0064] Comparative Example 2: Using conventional physical mixing methods, all raw materials were directly mixed and stirred.

[0065] Comparative Example 3: The plant polyphenol nanoaggregates of the present invention were replaced with an equal amount of ordinary refined decolorized apple polyphenols, and the remaining steps were the same as in Example 3.

[0066] Experimental Example: The following performance tests were conducted on the starches of Example 3 and Comparative Examples 1-3:

[0067] Hydrophobicity test: The contact angle of water droplets on the surface of starch tablets was measured using a contact angle meter, and the average value of 5 measurements was taken.

[0068] Anti-caking test: Weigh a certain mass of sample and place it in a constant temperature and humidity chamber (temperature 25℃, relative humidity 75%). After 7 days, determine the proportion of the mass of caking to the total mass (caking rate).

[0069] Antioxidant test: DPPH scavenging rate.

[0070] The results are shown in Table 1.

[0071] Table 1 Performance Test Results

[0072] project Hydrophobic angle clumping rate DPPH removal rate Example 3 132.5° 2.1% 62.6% Comparative Example 1 115.2° 8.5% 54.3% Comparative Example 2 98.6° 15.4% 46.5% Comparative Example 3 120.6° 3.6% 51.8%

[0073] This invention constructs a composite intermediate using plant polyphenol nanoaggregates, soybean polypeptide hydrophobic aggregates, and chitosan. Food-grade citric acid cross-linking enhances the stability of the intermediate structure, and a surface coating process yields a functional dry powder. This functional dry powder binds to starch granules, providing hydrophobic protection to the starch granules. The introduction of a cross-linking agent significantly enhances the structural stability of the intermediate; the introduction of an anti-caking agent further improves the product's flowability; and the introduction of plant polyphenol nanoaggregates further enhances the product's antioxidant properties. The overall solution works synergistically to significantly improve the hydrophobic persistence, anti-caking properties, and antioxidant properties of starch.

[0074] The powder of this invention can be used as a starch mold, and at the same time, it can form a uniform and stable protective layer on the surface of foods such as gummies, effectively locking in the moisture of the gummies, delaying oxidation and deterioration, and helping to extend the storage stability of foods such as gummies.

[0075] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions will not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A highly hydrophobic and anti-caking starch, characterized in that, It is prepared from the following raw materials in parts by weight: 30-35 parts starch, 11-13.3 parts octenyl succinate starch ester, 2.1-3.5 parts plant polyphenol nano-aggregates, 5.6-7.3 parts plant polypeptide hydrophobic aggregates, 2.2-3.1 parts chitosan, 0.3-1 parts anti-caking agent, and 0.1-0.13 parts food-grade crosslinking agent.

2. The highly hydrophobic and anti-caking starch according to claim 1, characterized in that, The starch used is corn starch.

3. The highly hydrophobic and anti-caking starch according to claim 1, characterized in that, The plant polypeptide hydrophobic aggregates used are soybean polypeptide hydrophobic aggregates.

4. The highly hydrophobic and anti-caking starch according to claim 1, characterized in that, The anti-caking agent is made of food-grade silicon dioxide.

5. The highly hydrophobic and anti-caking starch according to claim 1, characterized in that, The food-grade crosslinking agent is food-grade citric acid.

6. The highly hydrophobic and anti-caking starch according to claim 1, characterized in that, The preparation method of the plant polyphenol nanoaggregates is as follows: green tea and boiling water are brewed at a mass ratio of 1:50-120, filtered to obtain tea soup, and soda ash and salt are added to the tea soup at a mass ratio of 5:8-11. After dissolving, the tea soup is filtered using a filter membrane with a pore size of 0.22μm. The filter residue is dried and pulverized to obtain tea polyphenol self-assembled nanoaggregates.

7. The preparation process of highly hydrophobic and anti-caking starch according to any one of claims 1-6, characterized in that, Includes the following steps: (1) Prepare dispersions of plant polyphenol nano-aggregates, chitosan solution and plant polypeptide hydrophobic aggregates; (2) Add the plant polypeptide hydrophobic aggregate dispersion to the plant polyphenol nano-aggregate dispersion and stir evenly to obtain the first mixture for later use; (3) Adjust the pH of the first mixture to 4.8-5.5, slowly add the chitosan solution to the first mixture, and stir until homogeneous to obtain the second mixture; (4) Add food-grade crosslinking agent to the second mixture, stir and crosslink, and then freeze dry to obtain functional dry powder; (5) Take the functional dry powder, octenyl succinic starch ester and anti-caking agent, put them in a high-speed mixer and stir to complete the pre-coating of the powder surface; (6) Add starch to the pre-coated functional dry powder and stir; finally, dry, crush and sieve the mixed powder to obtain highly hydrophobic and anti-caking starch.

8. The preparation process of highly hydrophobic and anti-caking starch according to claim 7, characterized in that, Step (1) is as follows: Plant polyphenol nanoaggregates were added to deionized water and incubated at 35-40℃ and 500-650 rpm. -1 Stir for 20-30 minutes to prepare a dispersion of plant polyphenol nano-aggregates. Take chitosan, add 1-2% (v / v) of food-grade dilute acetic acid solution, stir to dissolve until a transparent solution is obtained, and prepare a chitosan solution with a mass concentration of 2-3%. Add hydrophobic aggregates of plant polypeptides to deionized water and incubate at 40-45℃ and 800-950 rpm. -1 Stir for 50-68 minutes to prepare a dispersion of plant polypeptide hydrophobic aggregates.

9. The preparation process of highly hydrophobic and anti-caking starch according to claim 8, characterized in that, In step (2), at 40-43℃ and 700-800 r·min -1 Stir for 15-20 minutes to obtain the first mixture; in step (3), stir at 40-43℃ and 600-750 r·min. -1 Stir for 25-33 minutes to obtain the second mixture; in step (4), stir at 50-55℃ and 200-250 r·min. -1 Stir for 1.5-2 hours; in step (5), the stirring speed is 800-850 r·min. -1 Stir for 15-23 minutes; in step (6), the stirring speed is 600-750 r·min. -1 Stir for 25-30 minutes.

10. A highly hydrophobic and anti-caking starch, characterized in that, It is prepared using the preparation process described in any one of claims 7-9.