Preparation method of waxy corn starch sodium octenylsuccinate

Abstract

The invention relates to the technical field of modified starch, in particular to a preparation method of waxy corn starch sodium octenyl succinate, which comprises the following steps: step 1, mixing waxy corn starch as a raw material with deionized water to prepare raw starch slurry with the slurry concentration of 35-40wt%; step 2, adding a catalyst into the native starch slurry obtained in the step 1, then adjusting the pH value to 11.0-11.5 by using an alkaline solution, then adding a cross-linking agent, and carrying out cross-linking for 40-90 minutes at the temperature of 20-30 DEG C; step 3, after the reaction in the step 2 is finished, adjusting the pH value to 9.0-9.5 by using an alkaline solution, heating to 35-40 DEG C, then adding an esterifying agent into the reaction system, and reacting for 30-60 minutes; step 4, after the reaction in the step 3 is finished, neutralizing an obtained product with a 10wt% neutralizer hydrochloric acid solution, washing, centrifugally dewatering, and drying to obtain waxy corn starch sodium octenyl succinate subjected to cross-linking esterification compound modification reaction; the transparency and the viscosity of the prepared composite modified starch paste are remarkably improved.

Description

Technical Field

[0001] The invention belongs to the technical field of modified starch, and particularly relates to a method for preparing waxy corn sodium octenylsuccinate starch. Background Art

[0002] As a commonly used emulsifying thickener, sodium starch octenylsuccinate plays an important role in the food industry; however, it still has some limitations in practical applications, such as its performance is easily affected under high salt, high shear force, and excessively strong acid and alkali conditions, its solubility and performance are limited at low temperatures, it is easy to decompose or its performance degrades at high temperatures, and its thickening effect is insufficient when used alone in certain high-viscosity systems; therefore, it is necessary to further modify it to expand its application range and improve its performance. Summary of the invention

[0003] The present invention aims to provide a novel preparation method of waxy corn sodium octenyl succinate starch by cross-linking esterification composite modification reaction, so as to overcome the performance defects of the existing sodium octenyl succinate starch and significantly improve its emulsification performance, gelatinization characteristics, stability and temperature and frost resistance.

[0004] To achieve the above object, the present invention provides the following technical solution: a method for preparing waxy corn starch sodium octenyl succinate, comprising the following steps: Step 1, using waxy corn starch as a raw material and mixing it with deionized water to prepare a raw starch slurry with a slurry concentration of 35-40wt%; Step 2, adding a catalyst to the original starch slurry described in step 1, adjusting the pH to 11.0-11.5 with an alkaline solution, then adding a crosslinking agent, and crosslinking at a temperature of 20-30° C. for 40-90 minutes; After the reaction in step 3 and step 2 is completed, the pH is adjusted to 9.0-9.5 with an alkaline solution, and then the temperature is raised to 35-40° C., and then an esterifying agent is added to the reaction system, and the reaction is carried out for 30-60 minutes; After the reaction in step 4 and step 3 is completed, the obtained product is neutralized with a 10wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain the waxy corn sodium octenyl succinate starch of the cross-linked esterification composite modification reaction.

[0005] Furthermore, the catalyst in step 2 is sodium chloride, and the amount of sodium chloride used is 0.5% to 1.5% of the weight of the starch.

[0006] Furthermore, the alkaline solution described in step 2 is a sodium hydroxide solution, and the concentration of the sodium hydroxide solution is 2wt%~5wt%.

[0007] Furthermore, the cross-linking agent in step 2 is phosphorus oxychloride, and the amount of phosphorus oxychloride used is 0.008% to 0.016% of the weight of the starch.

[0008] Furthermore, the esterifying agent in step 3 is octenyl succinic anhydride, and the amount of octenyl succinic anhydride used is 2% to 4% of the weight of the starch.

[0009] Compared with the prior art, the present invention has the following beneficial effects: 1. Significant performance improvement: (1) The composite modified starch paste prepared by the present invention has significantly improved transparency and viscosity, which enables it to provide better texture and appearance in food applications; for example, it can make the juice beverage clearer and more transparent, and can increase the smoothness of the taste of foods such as rolled noodles.

[0010] (2) Improved stability, including enhanced stability in different acid-base environments, high salt concentrations and high shear conditions; in fruit juice beverages, it can better maintain the emulsified state and prevent emulsion stratification, and its performance can also be kept stable in food systems containing a certain amount of salt.

[0011] (3) Its heat resistance and frost resistance are improved. It is not easy to decompose or its performance degrade during high-temperature processing. It can still maintain good solubility and performance in low-temperature storage or frozen food applications. For example, when used in frozen juice drinks or frozen desserts, it will not lose its emulsification and thickening effects due to the freezing and thawing process.

[0012] 2. Widely used: Due to its excellent performance, it can be widely used in various foods such as fruit juice drinks, flavors and fragrances, alum-free vermicelli, rolled noodles, etc., providing the food industry with an excellent performance additive option; in fruit juice drinks, the improvement of emulsification performance helps to improve the stability and taste of the juice; in flavors and fragrances, it can better encapsulate and release aromatic substances; in alum-free vermicelli and rolled noodles, it can improve their texture and cooking resistance. DETAILED DESCRIPTION

[0013] The present invention is described in detail below in conjunction with specific implementation modes.

[0014] A method for preparing waxy corn starch sodium octenylsuccinate is specifically implemented in the following manner: Step 1 is the preparation of raw starch slurry; waxy corn starch is selected as the raw material, and it is mixed with deionized water in a specific ratio to prepare a raw starch slurry with a slurry concentration of 35-40wt%. This step provides a uniform reaction system basis for subsequent reactions.

[0015] Step 2 is a cross-linking reaction; adding a catalyst sodium chloride to the original starch slurry in step 1, the amount of which is 0.5% - 1.5% (preferably 0.8% - 1.2%) of the weight of the starch, the addition of sodium chloride helps to promote the subsequent reaction; then using a sodium hydroxide solution with a concentration of 2wt% - 5wt% (preferably 3wt% - 4wt%) to adjust the system pH to 11.0 - 11.5, the appropriate pH range can ensure the efficient cross-linking reaction; then adding a cross-linking agent phosphorus oxychloride, the amount of which is 0.008% - 0.016% (preferably 0.010% - 0.014%) of the weight of the starch, and performing a cross-linking reaction at a temperature of 20 - 30°C (preferably 22 -28°C) for 40 - 90min (preferably 50 - 80min), the cross-linking reaction forms chemical bonds between starch molecules, and enhances the structural stability of the starch.

[0016] Step 3 is an esterification reaction. After the cross-linking reaction in step 2 is completed, the pH of the system is adjusted to 9.0-9.5 using sodium hydroxide solution again, and the temperature is raised to 35-40°C. Subsequently, an esterifying agent, octenyl succinic anhydride, is added to the reaction system in an amount of 2%-4% (preferably 2.5%-3.5%) of the weight of the starch, and the reaction is carried out for 30-60 minutes (preferably 40-50 minutes). The esterification reaction introduces octenyl succinic acid groups, which endows the sodium starch with good emulsifying properties.

[0017] Step 4 is post-treatment; after the esterification reaction in step 3 is completed, the reaction system is neutralized with a 10wt% neutralizing agent hydrochloric acid solution to adjust the pH to neutral, and then the product is washed to remove unreacted impurities and by-products, and then the water is further separated by centrifugal dehydration, and finally drying is performed to obtain a finished product of waxy corn sodium octenyl succinate starch of a cross-linked esterification composite modification reaction.

[0018] The technical effects of the present invention are further illustrated by the following examples and comparative examples. Example 1 With waxy corn starch as raw material, 750 kg of waxy corn starch was dissolved in 947.4 kg of deionized water to prepare a slurry with a slurry concentration of 38 wt% of raw starch slurry; then, 6.45 kg (0.86% of the weight of the starch) of sodium chloride catalyst was added, and the pH was adjusted to 11.2 with a sodium hydroxide solution with a concentration of 3 wt%, and then 70.95 g (0.0095% of the weight of the starch) of phosphorus oxychloride crosslinking agent was added, and crosslinked at 25°C for 60 minutes; after the reaction was completed, the pH was adjusted to 9.2 with a sodium hydroxide solution, the temperature was raised to 37°C, and 19.35 kg (2.58% of the weight of the starch) of octenyl succinic anhydride esterifying agent was added, and the reaction was carried out for 40 minutes; after the reaction was completed, the obtained product was neutralized with a 10 wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain waxy corn octenyl succinate sodium starch of crosslinked esterification composite modification reaction.

[0019] Example 2 With waxy corn starch as raw material, 750 kg of waxy corn starch was dissolved in 1092.9 kg of deionized water to prepare a slurry with a slurry concentration of 35 wt% of raw starch slurry; then, 3.23 kg (0.43% of the weight of starch) of sodium chloride catalyst was added, and the pH was adjusted to 11.0 with a sodium hydroxide solution with a concentration of 2 wt%, and then 53.05 g (0.0071% of the weight of starch) of phosphorus oxychloride crosslinking agent was added, and crosslinked at 20°C for 40 minutes; after the reaction, the pH was adjusted to 9.0 with a sodium hydroxide solution, the temperature was raised to 35°C, and 12.9 kg (1.72% of the weight of starch) of octenyl succinic anhydride esterifying agent was added, and the reaction was carried out for 30 minutes; after the reaction, the obtained product was neutralized with a 10 wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain waxy corn octenyl succinate sodium starch of crosslinked esterification composite modification reaction.

[0020] Example 3 With waxy corn starch as raw material, 750 kg of waxy corn starch was dissolved in 862.5 kg of deionized water to prepare a slurry with a concentration of 40 wt% of raw starch slurry; then, 9.68 kg (1.29% of the weight of the starch) of sodium chloride catalyst was added, and the pH was adjusted to 11.5 with a sodium hydroxide solution with a concentration of 5 wt%, and then 106.10 g (0.0141% of the weight of the starch) of phosphorus oxychloride crosslinking agent was added, and crosslinked at 30°C for 90 minutes; after the reaction, the pH was adjusted to 9.5 with a sodium hydroxide solution, the temperature was raised to 40°C, and 25.8 kg (3.44% of the weight of the starch) of octenyl succinic anhydride esterifying agent was added, and the reaction was carried out for 60 minutes; after the reaction, the obtained product was neutralized with a 10 wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain waxy corn octenyl succinate sodium starch with crosslinked esterification composite modification reaction.

[0021] Comparative Example 1 The difference from Example 1 is that the catalyst sodium chloride and the cross-linking agent phosphorus oxychloride are not added in Comparative Example 1, and the other steps are the same as those in Example 1. The details are as follows: With waxy corn starch as raw material, 750 kg of waxy corn starch is dissolved in 947.4 kg of deionized water to prepare a slurry with a concentration of 38 wt% of raw starch slurry, the pH is adjusted to 9.2 with a sodium hydroxide solution, the temperature is raised to 37°C, and then 19.35 kg of esterifying agent octenyl succinic anhydride is added to the reaction system and the reaction is carried out for 40 minutes. After the reaction is completed, the obtained product is neutralized with a 10 wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain waxy corn octenyl succinate sodium starch.

[0022] Comparative Example 2 The difference from Example 1 is that in Comparative Example 2, the esterification agent octenyl succinic anhydride is first used to produce an esterification reaction with the original starch slurry, and then a cross-linking reaction is carried out, and the other steps are the same as those in Example 1. The details are as follows: With waxy corn starch as a raw material, 750 kg of waxy corn starch is dissolved in 947.4 kg of water to prepare a slurry with a slurry concentration of 38 wt% of raw starch, 6.45 kg of catalyst sodium chloride is added, the pH is adjusted to 9.2 with a sodium hydroxide solution with a concentration of 3 wt%, the temperature is raised to 37°C, and then 19.35 kg of octenyl succinic anhydride, an esterifying agent, is added to the reaction system, and the reaction is carried out for 40 minutes; after the reaction is completed, the slurry is cooled to 25°C, the pH is adjusted to 11.2 with a sodium hydroxide solution, and then 70.95 g of phosphorus oxychloride, a cross-linking agent, is added, and cross-linking is carried out for 60 minutes; after the reaction is completed, the obtained product is neutralized with a 10 wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain waxy corn octenyl succinate sodium starch of esterification and cross-linking composite modification reaction.

[0023] The waxy corn starch sodium octenyl succinate prepared in Examples 1 to 3 and Comparative Examples 1 to 2 was measured, and the results are shown in Table 1: Table 1 The following conclusions can be drawn from Table 1: 1. Peak viscosity (BU) determination: The determination was carried out in accordance with GB / T 22427.7-2023 Determination of starch viscosity; the results showed that the peak viscosity of Examples 1 to 3 was significantly higher than that of Comparative Examples 1 to 2 and the unmodified waxy corn starch, indicating that the cross-linked esterification composite modification effectively increased the viscosity of the starch.

[0024] 2. Determination of octenyl succinic acid group (w / %): Determined in accordance with "GB1886.370-2023 Food Additive Octenyl Succinate Starch Sodium"; the octenyl succinic acid group content of Examples 1 to 3 is within a certain range and is different from that of the comparative example, indicating that the modification method has an impact on the introduction of the group.

[0025] 3. Determination of light transmittance: The light transmittance was determined with reference to the "Preparation and Performance Study of Acetate Starch from Different Raw Materials" in "Food Processing" Vol. 38, No. 6, 2013; the light transmittance of Examples 1 to 3 was relatively high, indicating that the transparency of the starch paste was improved.

[0026] Freeze-thaw stability determination: freeze-thaw water separation rate was determined according to "Comparative Study on Properties of Cassava Starch and Modified Cassava Starch" in "Food Industry Science and Technology" No. 6, 2008; the freeze-thaw stability of Examples 1 to 3 was significantly better than that of Comparative Examples 1 to 2 and unmodified waxy corn starch, indicating that the composite modification improved the freeze-thaw resistance of starch.

[0027] In summary, the present invention optimizes the starch modification method by using two chemical denaturation methods, and successively increases the transparency of starch, enhances the emulsification performance, and greatly improves its stability through cross-linking and esterification reactions; the freeze-thaw stability is significantly better than that of acetylated distarch phosphate and acetylated distarch adipate; the performance stability is far better than that of hydroxypropyl starch; and when applied to fruit juice beverages, the emulsification performance is significantly improved.

Claims

1. A method for preparing waxy corn starch sodium octenylsuccinate, characterized in that: The following steps are involved: Step 1, using waxy corn starch as a raw material and mixing it with deionized water to prepare a raw starch slurry with a slurry concentration of 35-40wt%; Step 2, adding a catalyst to the original starch slurry described in step 1, adjusting the pH to 11.0-11.5 with an alkaline solution, then adding a crosslinking agent, and crosslinking at a temperature of 20-30° C. for 40-90 minutes; After the reaction in step 3 and step 2 is completed, the pH is adjusted to 9.0-9.5 with an alkaline solution, and then the temperature is raised to 35-40° C., and then an esterifying agent is added to the reaction system, and the reaction is carried out for 30-60 minutes; After the reaction in step 4 and step 3 is completed, the obtained product is neutralized with a 10wt% neutralizing agent hydrochloric acid solution, washed, centrifuged and dehydrated, and dried to obtain the waxy corn sodium octenyl succinate starch of the cross-linked esterification composite modification reaction.

2. The method for preparing waxy corn starch sodium octenylsuccinate according to claim 1, characterized in that: The catalyst in step 2 is sodium chloride, and the amount of sodium chloride used is 0.5% to 1.5% of the weight of starch.

3. The method for preparing waxy corn starch sodium octenylsuccinate according to claim 1, characterized in that: The alkaline solution described in step 2 is a sodium hydroxide solution, and the concentration of the sodium hydroxide solution is 2wt%~5wt%.

4. The method for preparing waxy corn starch sodium octenylsuccinate according to claim 1, characterized in that: The cross-linking agent in step 2 is phosphorus oxychloride, and the amount of phosphorus oxychloride used is 0.008% to 0.016% of the weight of the starch.

5. The method for preparing waxy corn starch sodium octenylsuccinate according to claim 1, characterized in that: The esterifying agent described in step 3 is octenyl succinic anhydride, and the amount of octenyl succinic anhydride used is 2% to 4% of the weight of the starch.

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