CN113087812A - Preparation method of high-fluidity starch - Google Patents

Preparation method of high-fluidity starch Download PDF

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CN113087812A
CN113087812A CN202110440903.1A CN202110440903A CN113087812A CN 113087812 A CN113087812 A CN 113087812A CN 202110440903 A CN202110440903 A CN 202110440903A CN 113087812 A CN113087812 A CN 113087812A
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starch
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fluidity
alcohol
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CN113087812B (en
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王亚娟
仇丹
李亚
孔祥礼
王灵辉
姚利辉
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Ningbo University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00—Preparation of derivatives of starch
    • C08B31/003—Crosslinking of starch
    • C08B31/006—Crosslinking of derivatives of starch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00—Preparation of derivatives of starch
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00—Preparation of derivatives of starch
    • C08B31/02—Esters
    • C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention discloses a preparation method of high-fluidity starch, which is characterized by comprising the following steps: (1) adding deionized water into starch, then dropwise adding a mixed solution of octenyl succinic anhydride and alcohol, and finally filtering, washing and drying; (2) adding deionized water into a dry sample, adding 5-10 parts by mass of plant tannin extract for reaction, and finally cooling to room temperature; (3) dropwise adding acid liquor into the solution, passing through a metal screen, heating the solution after passing through the screen to 30-40 ℃, reacting for 30-120 min, adding alkali liquor, adjusting the pH to 3.5-4.5, heating to 45-50 ℃, continuing to react for 30-60 min, centrifuging after the reaction is finished, washing and drying to obtain the required high-fluidity starch. Compared with the prior art, the preparation method has simple operation, can obtain metal ions in situ, has uniform reaction, and can prepare the high-fluidity starch with uniform particle size.

Description

Preparation method of high-fluidity starch
Technical Field
The invention relates to the technical field of starch modification, in particular to a preparation method of high-fluidity starch.
Background
Natural starch widely exists in roots, stems and seeds of plants, is a polysaccharide substance which is generated by the plants after photosynthesis and is mainly used for energy storage, and natural starch and modified products thereof are widely applied to the fields of food, medicine, papermaking, chemical industry, cosmetics and the like due to the characteristics of wide sources, reproducibility, biodegradability and the like.
Since native starch contains a large number of hydroxyl groups in its molecule and is liable to form intramolecular hydrogen bonds, native starch granules tend to aggregate and cohere with each other and have poor flowability even in a dry state, thereby limiting its applicability. Hydrophilic groups in the starch molecule are responsible for its poor flowability, and thus the increase in flowability can be achieved by introducing hydrophobic groups in its molecule or shielding the hydrophilicity of the surface.
For example, patent application No. CN200710304696.7 (publication No. CN101230151A) discloses a high-fluidity and strong-hydrophobicity starch and a preparation method thereof, which comprises coating an aluminate coupling agent and a silane coupling agent on the surface of starch particles by a dry method, and coating the outermost layer with a fluidity improver of a silicon dioxide or aluminum oxide layer to obtain better fluidity. However, the method mainly depends on physical mixing and coating, and if the method is not uniform, the flowing effect is influenced; patent application No. CN201210141066.3 (publication No. CN102702368A) invention patent "a fluidity starch and its dry preparation method" discloses a method for preparing fluidity starch by dry method, the method needs a dry reactor, the experimental condition requirement is higher, after the first stage octenyl succinic acid esterification, unreacted octenyl succinic acid is not removed, the later stage to inject a little solution of high valence metal ion salt into the reactor, therefore the reaction uniformity with starch is worse, and after the metal ion reacts with starch, its anion group can react with sodium ion in starch ester, thus other inorganic salt components are introduced.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of high-fluidity starch, which is simple to operate, can obtain metal ions in situ and has uniform reaction, aiming at the current situation of the prior art, and the method can be used for preparing the high-fluidity starch with uniform particle size.
The technical scheme adopted by the invention for solving the technical problem is as follows: a preparation method of high-fluidity starch is characterized by comprising the following steps:
(1) adding deionized water into 100 parts by mass of starch to prepare 20-40 wt% starch milk, dropwise adding alkali liquor to control the pH to 7.5-9.0, dropwise adding 1-3 parts by mass of a mixed solution of octenyl succinic anhydride and alcohol, reacting for 30-240 min, adjusting the pH to be neutral by using acid liquor, and finally filtering, washing and drying;
wherein the volume ratio of octenyl succinic anhydride to alcohol in the mixed solution of octenyl succinic anhydride and alcohol is 1: 4-6;
(2) adding deionized water into 100 parts by mass of the dried sample obtained in the step (1) to prepare starch paste with the concentration of 10-40 wt%, placing the starch paste into an ultrasonic reactor, dropwise adding acid liquor, controlling the pH value to 4.5-6.5, externally adding mechanical stirring for 20-40 min, then adding 5-10 parts by mass of plant tannin extract, heating to 30-40 ℃ for reaction for 30-240 min, then adjusting the pH value to 3.8-4.0 by using the acid liquor, heating to 45-50 ℃ for continuous reaction for 30-60 min, and finally cooling to room temperature;
(3) and (3) dropwise adding acid liquor into the solution obtained in the step (2) to adjust the pH value to 2.5-3.0, passing through a metal screen, heating the solution passing through the screen to 30-40 ℃, reacting for 30-120 min, adding alkali liquor to adjust the pH value to 3.5-4.5, heating to 45-50 ℃, continuing to react for 30-60 min, centrifuging after the reaction is finished, and washing and drying to obtain the required high-fluidity starch.
Preferably, the starch in step (1) is at least one of waxy corn starch, waxy sorghum starch, waxy rice starch and wheat starch.
Preferably, the alcohol in the mixed solution of octenyl succinic anhydride and alcohol in step (1) is one of methanol, ethanol and isopropanol.
Preferably, the alkali solution in the step (1) is a NaOH solution, and the acid solution is dilute hydrochloric acid.
Preferably, the power of the ultrasonic reactor in the step (2) is 300-1000W, and the frequency is 28-40 kHz.
Preferably, the rotation speed of the mechanical stirring in the step (2) is 200-400 rpm.
Preferably, the acid solution in the step (2) is dilute hydrochloric acid and formic acid in sequence.
Preferably, the plant tannin extract in step (2) is at least one of catechin, Galla chinensis, oak cup, chestnut, and wattle bark plant tannin extract.
Preferably, the metal screen in step (3) is at least one of a wire mesh, an aluminum wire mesh and a stainless steel mesh.
Preferably, the metal screen mesh in the step (3) is a metal screen mesh gradually passing through 24 meshes, 40 meshes, 80 meshes and 120 meshes.
Preferably, the acid solution in step (3) is dilute sulfuric acid, and the alkali solution is sodium bicarbonate solution.
The working principle of the invention is as follows: hydrophobic groups (octenyl succinic acid) are connected to starch molecules through an aqueous phase method, then cross-linking agents (tannin extracts and metal ion cross-linking agents) are combined to shield hydroxyl groups on the surface of OS-starch, so that the hydrophobicity of the OS-starch is increased, wherein metal ions are obtained in situ by filtering acidic starch milk combined with tannin extracts through a metal screen, and the uniformity of the particle size of the prepared high-fluidity starch can be ensured.
Compared with the prior art, the invention has the advantages that:
(1) octenyl succinic acid is grafted to starch molecules in a water phase, so that the requirement on reaction equipment is not high, and unreacted octenyl succinic anhydride is removed through alcohol washing and water washing;
(2) the ultrasonic generator is introduced into the reaction process of the plant tannin extract, the metal ions and the starch, so that the reaction efficiency is increased, and the reaction is more uniform;
(3) the starch ester crosslinked with the tannin extract is adjusted to be acidic, and is filtered by metal screens with different meshes, the metal screens can prepare metal ions in situ while playing a filtering role, the operation is simple, other inorganic salt components can not be introduced, and the metal ions can be further complexed with the starch and the tannin extract by changing the environment, so that the modified starch with uniform particle size and high fluidity can be obtained.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) adding a proper amount of deionized water into 100 parts of waxy corn starch in parts by mass to prepare starch milk with the concentration of 30 wt%, dropwise adding NaOH solution to control the pH to 8.5, dropwise adding 3 parts of OSA/ethanol solution (namely mixed solution of octenyl succinic anhydride and ethanol, the volume ratio of the octenyl succinic anhydride to the ethanol is 1:5), reacting at 30 ℃ for 60min, adjusting the pH to be neutral by using dilute hydrochloric acid, filtering, washing with alcohol for 3 times, washing with water for 3 times, and freeze-drying;
(2) taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 20 wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 5.0, applying mechanical stirring for 30min, setting the parameters of an ultrasonic reaction field to be 35kHz and 600W, setting the stirring parameters to be 300rmp, adding 8 parts of Galla Turcica tannin extract, heating to 35 ℃, reacting for 120min, adjusting the pH value to 3.9 with formic acid, heating to 45 ℃, continuing mechanical stirring for 40min, and then cooling to room temperature;
(3) adjusting reaction pH to 2.8 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh wire mesh sieves, heating the obtained filtrate to 35 deg.C, reacting for 60min, and adding NaHCO3Adjusting the pH value of the solution to 4.0, heating to 48 ℃, continuing to react for 40min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
Example 2:
(1) adding a proper amount of deionized water into 100 parts of glutinous rice starch by mass to prepare 20 wt% starch milk, dropwise adding NaOH solution to control the pH to 7.5, dropwise adding 1 part of OSA/isopropanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1:4), reacting at 30 ℃ for 30min, adjusting the pH to be neutral by using dilute hydrochloric acid, filtering, washing with alcohol for 3 times, washing with water for 3 times, and freeze-drying;
(2) taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 10 wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 4.5, mechanically stirring for 20min, setting the parameters of an ultrasonic reaction field to be 28kHz and 300W, setting the stirring parameters to be 200rmp, adding 5 parts of castanea mollissima extract, heating to 30 ℃, reacting for 30min, adjusting the pH value to be 3.8 by using formic acid, heating to 45 ℃, continuously mechanically stirring for 40min, and cooling to room temperature;
(3) adjusting reaction pH to 2.5 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh aluminum wire mesh sieves, heating the obtained filtrate to 30 deg.C, reacting for 30min, and adding NaHCO3Adjusting the pH value of the solution to 3.5, heating to 45 ℃, continuing to react for 30min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
Example 3:
(1) adding a proper amount of deionized water into 100 parts of wheat starch in parts by mass to prepare starch milk with the concentration of 40 wt%, dropwise adding NaOH solution to control the pH to 9.0, dropwise adding 2 parts of OSA/ethanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1:6), reacting at 30 ℃ for 240min, adjusting the pH to be neutral by using dilute hydrochloric acid, filtering, washing with alcohol for 3 times, washing with water for 3 times, and freeze-drying;
(2) taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 40 wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 6.5, mechanically stirring for 40min, setting the parameters of an ultrasonic reaction field to be 40kHz and 1000W, setting the stirring parameters to be 400rmp, adding 10 parts of oak cup tannin extract, heating to 40 ℃, reacting for 240min, adjusting the pH value to 4.0 by using formic acid, heating to 50 ℃, continuously mechanically stirring for 60min, and then cooling to room temperature;
(3) adjusting reaction pH to 3.0 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh stainless steel sieve, heating the obtained filtrate to 40 deg.C, reacting for 120min, and adding NaHCO3Adjusting the pH value of the solution to 4.5, heating to 45 ℃, continuing to react for 60min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
Example 4:
(1) adding a proper amount of deionized water into 100 parts of waxy sorghum starch in parts by mass to prepare starch milk with the concentration of 40 wt%, dropwise adding NaOH solution to control the pH to 7.5, dropwise adding 3 parts of OSA/ethanol solution (the volume ratio of octenyl succinic anhydride to ethanol is 1:6), reacting at 30 ℃ for 240min, adjusting the pH to be neutral by using dilute hydrochloric acid, filtering, washing with alcohol for 3 times, washing with water for 3 times, and freeze-drying;
(2) taking 100 parts of freeze-dried sample, adding a proper amount of deionized water to prepare starch paste with the concentration of 25 wt%, placing the starch paste into an ultrasonic reactor, dropwise adding dilute hydrochloric acid to control the pH value to be 4.5, mechanically stirring for 40min, setting the parameters of an ultrasonic reaction field to be 40kHz and 300W, setting the stirring parameters to be 400rmp, adding 8 parts of wattle bark tannin extract, heating to 40 ℃, reacting for 240min, adjusting the pH value to 4.0 by using formic acid, heating to 50 ℃, continuously mechanically stirring for 45min, and then cooling to room temperature;
(3) adjusting reaction pH to 3.0 with dilute sulfuric acid, gradually sieving with 24 mesh, 40 mesh, 80 mesh and 120 mesh sieve, heating the obtained filtrate to 40 deg.C, reacting for 90min, and adding NaHCO3Adjusting the pH value of the solution to 4.5, heating to 45 ℃, continuing to react for 60min, centrifuging after the reaction is finished, washing with water for 3 times, washing with alcohol for 3 times, and drying to obtain a sample.
The flowability of the powder sample can be characterized by the angle of repose, and the smaller the angle of repose, the better the flowability.
The angle of repose of waxy corn starch and the high fluidity starch obtained in example 1 was determined using a powder comprehensive property tester, and the specific test method was: the damping table is arranged in a positioning hole in the center of the instrument, a material receiving disc and an angle of repose sample table are arranged on the damping table, and the upper plane of the angle of repose sample table can be ensured to be in a horizontal state by adjusting screws below the damping table. Closing the front door of the instrument, preparing a sample, adjusting the timer to 3min, opening a vibrating screen cover and a vibrating screen switch, slowly feeding materials at a feeding port by using a small spoon, spraying the materials onto a sample table through a screen and a discharging port to form a cone, stopping feeding after a symmetrical cone is formed, closing the vibrating screen, placing a goniometer at the left side of a sample tray and close to a material pile, measuring from three different positions when measuring the angle of repose, calculating the average value as one measurement, and measuring each sample for 3 times.
Table 1 lists the angle of repose for the different samples, and it can be seen that the fluidity of the waxy corn starch obtained by the present method is significantly increased.
Table 1:
sample (I) Angle of repose
Waxy corn starch 56.07±0.73
Example 1 14.48±0.53

Claims (10)

1.一种高流动性淀粉的制备方法，其特征在于包括有以下步骤：1. a preparation method of high fluidity starch is characterized in that comprising the following steps: (1)在100质量份淀粉中加入去离子水，配置成浓度为20～40wt％的淀粉乳，滴加碱液控制pH至7.5～9.0，而后滴加1～3质量份辛烯基琥珀酸酐和醇的混合溶液，反应30～240min后，使用酸液调节pH至中性，最后过滤洗涤干燥；(1) Add deionized water to 100 parts by mass of starch, configure into starch milk with a concentration of 20 to 40 wt %, add lye dropwise to control pH to 7.5 to 9.0, and then dropwise add 1 to 3 parts by mass of octenyl succinic anhydride Mixed solution with alcohol, after 30-240min reaction, use acid solution to adjust pH to neutrality, and finally filter, wash and dry; 其中，所述辛烯基琥珀酸酐和醇的混合溶液中辛烯基琥珀酸酐和醇的体积比为1:4～6；Wherein, the volume ratio of octenyl succinic anhydride and alcohol in the mixed solution of octenyl succinic anhydride and alcohol is 1:4～6; (2)在100质量份步骤(1)得到的干燥样品中加入去离子水，配置成浓度为10～40wt％的淀粉糊，将其置于超声波反应器中，然后滴加酸液，控制pH至4.5～6.5，外加机械搅拌20～40min，接着加入5～10质量份的植物栲胶并升温至30～40℃反应30～240min，然后使用酸液调节pH至3.8～4.0并升温至45～50℃继续反应30～60min，最后冷却至室温；(2) adding deionized water to 100 parts by mass of the dry sample obtained in step (1), and configuring a starch paste with a concentration of 10 to 40 wt %, placing it in an ultrasonic reactor, and then adding acid solution dropwise to control pH To 4.5～6.5, add mechanical stirring for 20～40min, then add 5～10 parts by mass of vegetable tannin extract and be warmed up to 30～40 ℃ and react for 30～240min, then use acid solution to adjust pH to 3.8～4.0 and be warmed up to 45～ Continue the reaction at 50°C for 30-60min, and finally cool to room temperature; (3)在步骤(2)得到的溶液中滴加酸液调节pH至2.5～3.0，过金属筛网，而后将过网后的溶液升温至30～40℃反应30～120min，后加入碱液调节pH至3.5～4.5并升温至45～50℃继续反应30～60min，结束后离心，洗涤干燥后得到所需的高流动性淀粉。(3) in the solution obtained in step (2), add acid solution dropwise to adjust pH to 2.5～3.0, pass through a metal mesh, and then heat the solution after passing through the mesh to 30～40°C for 30～120min, and then add lye The pH is adjusted to 3.5-4.5, and the temperature is raised to 45-50° C. to continue the reaction for 30-60 minutes, centrifugation after completion, washing and drying to obtain the desired high-fluidity starch. 2.根据权利要求1所述的高流动性淀粉的制备方法，其特征在于：步骤(1)中所述的淀粉为糯玉米淀粉、糯高粱淀粉、糯米淀粉、小麦淀粉中的至少一种。2. the preparation method of high fluidity starch according to claim 1 is characterized in that: the starch described in step (1) is at least one in waxy corn starch, waxy sorghum starch, glutinous rice starch, wheat starch. 3.根据权利要求1所述的高流动性淀粉的制备方法，其特征在于：步骤(1)中所述辛烯基琥珀酸酐和醇的混合溶液中的醇为甲醇、乙醇、异丙醇中的一种。3. the preparation method of high-fluidity starch according to claim 1 is characterized in that: the alcohol in the mixed solution of octenyl succinic anhydride and alcohol described in step (1) is in methyl alcohol, ethanol, isopropanol a kind of. 4.根据权利要求1所述的高流动性淀粉的制备方法，其特征在于：步骤(1)中所述的碱液为NaOH溶液，所述的酸液为稀盐酸。4. The preparation method of high-fluidity starch according to claim 1, is characterized in that: the lye solution described in the step (1) is NaOH solution, and the described acid solution is dilute hydrochloric acid. 5.根据权利要求1所述的高流动性淀粉的制备方法，其特征在于：步骤(2)中所述超声波反应器的功率为300～1000W，频率为28～40kHz；5. The preparation method of high-fluidity starch according to claim 1, characterized in that: the power of the ultrasonic reactor described in step (2) is 300-1000W, and the frequency is 28-40kHz; 步骤(2)中所述机械搅拌的转速为200～400rpm。The rotational speed of the mechanical stirring in step (2) is 200-400 rpm. 6.根据权利要求1所述的高流动性淀粉的制备方法，其特征在于：步骤(2)中所述的酸液依次为稀盐酸和甲酸。6. The preparation method of high fluidity starch according to claim 1, is characterized in that: the acid solution described in step (2) is dilute hydrochloric acid and formic acid successively. 7.根据权利要求1所述的的高流动性淀粉的制备方法，其特征在于：步骤(2)中所述的植物栲胶为儿茶素、五棓子、橡碗、栗木、荆树皮植物栲胶中的至少一种。7. the preparation method of high-fluidity starch according to claim 1, is characterized in that: the plant tannin extract described in step (2) is catechin, quinquefolium, rubber bowl, chestnut, wattle bark At least one of plant tannin extracts. 8.根据权利要求1所述的的高流动性淀粉的制备方法，其特征在于：步骤(3)中所述的金属筛网为铁丝网、铝丝网、不锈钢网中的至少一种。8. The preparation method of high-fluidity starch according to claim 1, characterized in that: the metal screen described in the step (3) is at least one of a wire mesh, an aluminum wire mesh, and a stainless steel mesh. 9.根据权利要求1所述的的高流动性淀粉的制备方法，其特征在于：步骤(3)中所述的过金属筛网具体为逐步过24目、40目、80目和120目的金属筛网。9. the preparation method of high-fluidity starch according to claim 1, is characterized in that: the metal screen described in step (3) is specifically to gradually pass 24 orders, 40 orders, 80 orders and 120 orders of metal sieve. 10.根据权利要求1至9中任一权利要求所述的的高流动性淀粉的制备方法，其特征在于：步骤(3)中所述的酸液为稀硫酸，所述的碱液为碳酸氢钠。10. according to the preparation method of the high fluidity starch described in any one of claim 1 to 9, it is characterized in that: the acid solution described in the step (3) is dilute sulfuric acid, and described alkali solution is carbonic acid Sodium hydrogen.
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