CN107513112A - A kind of preparation method for being esterified maltodextrin - Google Patents
A kind of preparation method for being esterified maltodextrin Download PDFInfo
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Abstract
The invention belongs to maltodextrin technical field, and in particular to a kind of preparation method for being esterified maltodextrin, acidulant ultrasonic disperse will be added after maltodextrin dispersing and dissolving using ethanol water and reacts to obtain acidifying maltodextrin；Then pH adjusting agent and modifying agent are added to acidifying maltodextrin, and ultrasonic reaction is esterified, circulation carries out secondary esterification in heated sealed pressurization after addition inorganic initiator, is filtrated to get and is esterified maltodextrin highly finished product；Esterification maltodextrin highly finished product are finally put into water-bath micro-boiling back flow reaction in glycerol-alcohol solvent, ethanol washs to obtain the esterification maltodextrin of high-quality after filtering.The preparation method of the present invention simply controls, and esterifying efficiency is fast, and yield is high, solves the problem of prior art low yield, refining step complexity.
Description
Technical field
The invention belongs to maltodextrin technical field, and in particular to a kind of preparation method for being esterified maltodextrin.
Background technology
The maltodextrin in the 1950s, people just begin one's study.Maltodextrin (C6H10O5)n·H2O, also referred to as water solubility
Dextrin is a kind of through acid system, enzyme process or acid --- the linear straight chain starch of enzyme collaboration method control and the amylopectin with branch
Low degree catabolite, range of molecular weight distributions is very big, and molal weight is between starch and starch sugar.It is generally acknowledged that malt
Dextrin is the polymer of a kind of D-Glucose, the linear long formed containing α-Isosorbide-5-Nitrae glucosides key connection α-D- glucopyranose residues
Chain, while also have the side chain being connected to form a little by branch point α -1,6 glycosidic bonds.Because reducing end increases in process of starch degradation
Add, its palliating degradation degree can be represented with DE values, and wherein maltodextrin DE values are less than 20.Maltodextrin is a kind of carbohydrate admixture,
Its sugar composition can use gel filtration or high performance liquid chromatography to be measured, and Main Ingredients and Appearance is dextrin, polysaccharide, tetrose
Or oligosaccharide more than tetrose, also containing a small amount of maltose and glucose.The DE values of maltodextrin not only represent its hydrolysis degree,
It is food production and for describing the most frequently used parameter of its molecular weight distribution, its theoretical value is inversely proportional with mean molecule quantity
The theoretical foundation that relevant important physical property provides, such as hygroscopicity, glass transition temperature, colligative property.Because of maltodextrin
DE values are corresponding with its sugared composition, and sugared composition directly affects its sugariness, viscosity, hygroscopicity, dissolubility and coloring, leads
Cause the maltodextrin property of different DE values different.With the increase of the intensification of maltodextrin hydrolysis degree, i.e. DE values, maltodextrin point
The linear degree of son gradually reduces, and branch degree gradually increases, and molecular weight distribution tends to be uniform, and molecular structure tends to be simple, always
Change degree, adhesive power and anti-crystallization gradually reduce, while the sugariness of product, dissolubility, hygroscopicity gradually increase, easily hair
Raw brown stain etc..
Maltodextrin is boundless because of its excellent functional characteristic, market prospects.However, the production of maltodextrin at present is still
With certain empirical, product quality is not sufficiently stable, and DE values and the component distribution of precisely control product still has certain tired
It is difficult.For common low DE value maltodextrin, many macromolecule polyalcohols are contained in molecule, linear dextrin content is also relatively more,
And molecular weight distribution is also uneven, easily cause its intermolecular association, easily flocculated after standing a period of time in the solution,
Precipitation.Polymerizeing again or bringing back to life for dextrin can influence the rate of filtration of syrup, influence being smoothed out for processing technology, while also influence
The qualities of maltodexLtrin products, eventually limit the application field of maltodexLtrin products.The limitation applied to maltodextrin,
In order to obtain more preferable feature, the application of maltodextrin is widened, it is necessary to further pay close attention to and discuss that maltodextrin uses
During the problem of existing, strengthen the research in terms of maltodextrin modification.
In the molecular structure of maltodextrin, in addition to easily cleavage reaction occurs for glycosidic bond, glucose unit C2、C3、
C6Alcoholic extract hydroxyl group reactivity it is very high, the hydroxyl in maltodextrin parent can be substituted using the functional group of some materials, from
And introduce different chemical groups or the reaction such as oxidation, rearrangement, molecular replacement occurs, to improve the physicochemical property of maltodextrin.
The modification common method of maltodextrin is directly to act on obtaining finished product with chemical reagent using maltodextrin.Method reaction is easy
Control, product color is white, is not easy to turn to be yellow during high temperature, prevented from caking, but yield is more relatively low, and refining step is relative complex.
The content of the invention
For the problems of the prior art, the present invention provides a kind of preparation method for being esterified maltodextrin, the preparation method
Simple control, esterifying efficiency is fast, and yield is high, solves the problem of prior art low yield, refining step complexity.
To realize above technical purpose, the technical scheme is that：A kind of preparation method for being esterified maltodextrin, it is special
Sign is：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 20-30min, it is acidified
Maltodextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 2-4h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 30- in heated sealed pressurization
50min, it is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 50-80min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 75-80%, and the concentration of the maltodextrin is 20-
30%.
Pharmaceutical grade dispersant in the step 1 uses polyvinylpyrrolidone or polyethylene glycol, the medical fraction
The addition of powder is maltodextrin quality 8-16%, and the stirring uses mechanical agitation, mixing speed 1500-3000r/
min。
As an improvement, the feed postition of the pharmaceutical grade dispersant adds for gradation formula, each addition is 1-2g/ times,
Interval time is 10-20min.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 1-5% of maltodextrin quality,
The addition speed of the acidulant is 2-5mL/min, and the frequency of the ultrasonic reaction is 1.5-5.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH in 5.5-6.5, the modification
Agent uses stearic acid, and the stearic addition is the 10-15% of maltodextrin quality, and the pH adjusting agent and modifying agent are same
When add, the rate of addition is 3-5g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency
25-35kHz, temperature are 60-70 DEG C, and inner recirculation flow speed is 10-20mL/min.
As an improvement, the response procedures of circular response are as follows in the water bath sonicator：
| Supersonic frequency kHz | Temperature DEG C | Back-flow velocity mL/min | Time min |
| 10-20 | Room temperature -50 | 0-10 | 10-20 |
| 25-30 | 60-70 | 10-20 | 20-30 |
| 35 | 70 | 20 | Remaining time |
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
1-4%, the temperature of circular response is 70-80 DEG C, pressure 0.3-0.8MPa in heated sealed pressurization, inner recirculation flow speed
For 30-50mL/min.
The concentration of esterification maltodextrin highly finished product in the step 5 is 30-60g/L, the water-bath micro-boiling back flow reaction
Temperature be 70-80 DEG C, the volume of glycerine and ethanol is 0.8-1.4 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 50-60 DEG C.
Step 1 adds maltodextrin into ethanol water, can half dissolubility turbid solution, maltodextrin can be dissolved in
In water, insoluble in ethanol, therefore the mixed liquor of suspended state is formed, add dispersant and stir to form the good suspended shape of dispersion
The maltodextrin solution of state.
Acidulant is dispersed in maltodextrin solution by step 2 under ultrasonic state, ensures acidulant fine dispersion effect
While, it is in acidity to keep solution, improves the stability of hydroxyl on maltodextrin.
Step 3 by add pH adjusting agent you, keep the pH stability of reaction solution, the addition of modifying agent can be with acetic acid shape
Into bisgallic acid structure, during ultrasonic reaction, the clutch that ultrasound is brought can improve the activity of hydroxyl on maltodextrin, cause hydroxyl
Base is broken, while modifying agent carries out esterification with acetic acid in the presence of ultrasonic clutch energy；The mode of interior circulation can be by height
The acidifying maltodextrin very first time of concentration and modifying agent, quick esterification, increases modifying agent under ultrasound condition
Reaction efficiency；The speed of reaction, moment can be adjusted according to reaction density using the temperature ultrasound back flow reaction of Gradient methods
Ensure the high efficiency of esterification.
Step 4 adds inorganic initiator into esterification maltodextrin crude product, in heated sealed pressurization under cycling condition,
Inorganic initiator acts on the acidulant of residual and modifying agent to the residual hydroxyl of esterification maltodextrin, forms secondary esterification,
Obtain degree of esterification and be deeper esterified maltodextrin, that is, be esterified maltodextrin highly finished product.
Step 5 is put into maltodextrin highly finished product are esterified in glycerine-ethanol solution, and inorganic initiator is produced by glycerine
Sodium sulphate dissolving, deimpurity purpose can be reached；The modifying agent of low content can dissolve in ethanol with acidulant,
Being esterified maltodextrin does not dissolve in ethanol and glycerine simultaneously；By micro-boiling reaction system, hot ethanol can not only remove impurity, together
When can it is deep enough esterification maltodextrin inside, internal layer impurity is removed；Washed after finally filtering using ethanol by the glycerine of residual
Remove, the esterification maltodextrin of high-quality is obtained after drying.
The present invention will add acidulant ultrasonic disperse using ethanol water and react to obtain acid after maltodextrin dispersing and dissolving
Change maltodextrin；Then pH adjusting agent and modifying agent are added to acidifying maltodextrin, and ultrasonic reaction is esterified, and adds nothing
Circulation carries out secondary esterification in heated sealed pressurization after machine initiator, is filtrated to get esterification maltodextrin highly finished product；Finally
Esterification maltodextrin highly finished product are put into water-bath micro-boiling back flow reaction in glycerine-alcohol solvent, ethanol washs to obtain height after filtering
The esterification maltodextrin of quality.
From the above, it can be seen that the present invention possesses advantages below：
1. the preparation method of the present invention simply controls, esterifying efficiency is fast, and yield is high, solves prior art low yield, essence
The problem of complex procedures processed.
2. the preparation method of the present invention reduces the difficulty of esterification, esterifying efficiency and esterification depth are improved.
3. product prepared by the present invention substantially increases the performance of product, the defects of overcoming existing dextrin product, improve attached
It is value added, expand the application field of dextrin.
4. the present invention can not only provide acidity environment using acetic acid as acidulant, ensure hydroxyl stability early stage, together
When can be used as being modified, form double modified systems with stearic acid, substantially increase the substitution value of maltodextrin.
5. the present invention uses double esterification method, the esterification depth of maltodextrin is deepened, while inorganic initiator can not only
Promotion esterification is played, while also can all be removed in the later stage, does not influence product quality.
6. the present invention uses glycerine-ethanol as solvent, by caused impurity removal in reaction, while by ethanol to sweet
The dissolubility of oil solves the residue problem of glycerine, ensure that the quality of product.
Embodiment
Describe the present invention in detail in conjunction with the embodiments, but any restriction is not done to the claim of the present invention.
Embodiment 1
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 20min, obtain being acidified malt
Dextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 2h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 30min in heated sealed pressurization,
It is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 50min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 75%, and the concentration of the maltodextrin is 20%.
Pharmaceutical grade dispersant in the step 1 uses polyvinylpyrrolidone, the addition of the pharmaceutical grade dispersant
It is maltodextrin quality 8%, the stirring uses mechanical agitation, mixing speed 1500r/min.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 1% of maltodextrin quality, institute
The addition speed for stating acidulant is 2mL/min, and the frequency of the ultrasonic reaction is 1.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 5.5, and the modifying agent is adopted
With stearic acid, the stearic addition is the 10% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent,
The rate of addition is 3g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 25kHz, temperature
For 60 DEG C, inner recirculation flow speed is 10mL/min.
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
1%, the temperature of circular response is 70 DEG C, pressure 0.3MPa in heated sealed pressurization, and inner recirculation flow speed is 30mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 30g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 70 DEG C, the volume of glycerine and ethanol is 0.8 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 50 DEG C.
Embodiment 2
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 30min, obtain being acidified malt
Dextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 4h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 50min in heated sealed pressurization,
It is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 80min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 80%, and the concentration of the maltodextrin is 30%.
Pharmaceutical grade dispersant in the step 1 uses polyethylene glycol, and the addition of the pharmaceutical grade dispersant is malt
Dextrin quality 16%, the stirring use mechanical agitation, mixing speed 3000r/min.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 5% of maltodextrin quality, institute
The addition speed for stating acidulant is 5mL/min, and the frequency of the ultrasonic reaction is 5.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 6.5, and the modifying agent is adopted
With stearic acid, the stearic addition is the 15% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent,
The rate of addition is 5g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 35kHz, temperature
For 70 DEG C, inner recirculation flow speed is 20mL/min.
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
4%, the temperature of circular response is 80 DEG C, pressure 0.8MPa in heated sealed pressurization, and inner recirculation flow speed is 50mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 60g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 80 DEG C, the volume of glycerine and ethanol is 1.4 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 60 DEG C.
Embodiment 3
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 25n, obtain being acidified malt paste
Smart solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 3 simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 30- in heated sealed pressurization
50min, it is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 7min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 78, and the concentration of the maltodextrin is 25.
Pharmaceutical grade dispersant in the step 1 uses polyethylene glycol, and the addition of the pharmaceutical grade dispersant is malt
Stirring uses mechanical agitation, mixing speed 2500min described in dextrin quality 12.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 3 of maltodextrin quality, described
The addition speed of acidulant is 3L/min, and the frequency of the ultrasonic reaction is 35kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 6, and the modifying agent uses
Stearic acid, the stearic addition are the 13% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent, institute
It is 4g/min to state rate of addition, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 30kHz, temperature
65 DEG C, inner recirculation flow speed is 15mL/min.
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
3%, the temperature of circular response is 75 DEG C, pressure 0.5MPa in heated sealed pressurization, and inner recirculation flow speed is 40mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 45g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 75 DEG C, the volume of glycerine and ethanol is 1.2 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 55 DEG C.
Embodiment 4
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 25min, obtain being acidified malt
Dextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 4h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 50min in heated sealed pressurization,
It is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 80min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 80%, and the concentration of the maltodextrin is 25%.
Pharmaceutical grade dispersant in the step 1 uses polyethylene glycol, and the addition of the pharmaceutical grade dispersant is malt
Dextrin quality 13%, the stirring use mechanical agitation, mixing speed 2500r/min；The addition of the pharmaceutical grade dispersant
Mode adds for gradation formula, and each addition is 1g/ times, interval time 10min.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 2% of maltodextrin quality, institute
The addition speed for stating acidulant is 4mL/min, and the frequency of the ultrasonic reaction is 2.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 6.5, and the modifying agent is adopted
With stearic acid, the stearic addition is the 13% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent,
The rate of addition is 4g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 35kHz, temperature
For 70 DEG C, inner recirculation flow speed is 20mL/min；The response procedures of circular response are as follows in the water bath sonicator：
| Supersonic frequency kHz | Temperature DEG C | Back-flow velocity mL/min | Time min |
| 10 | Room temperature | 10 | 10 |
| 25 | 60 | 10 | 20 |
| 35 | 70 | 20 | Remaining time |
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
3%, the temperature of circular response is 75 DEG C, pressure 0.7MPa in heated sealed pressurization, and inner recirculation flow speed is 40mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 40g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 75 DEG C, the volume of glycerine and ethanol is 1 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 55 DEG C.
Embodiment 5
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 25min, obtain being acidified malt
Dextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 4h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 50min in heated sealed pressurization,
It is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 80min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in 5 steps 1 is 75%, and the concentration of the maltodextrin is 20%.
Pharmaceutical grade dispersant in the step 1 uses polyvinylpyrrolidone, the addition of the pharmaceutical grade dispersant
It is maltodextrin quality 14%, the stirring uses mechanical agitation, mixing speed 2000r/min；The pharmaceutical grade dispersant
Feed postition be gradation formula add, each addition be 2g/ times, interval time 20min.
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 2% of maltodextrin quality, institute
The addition speed for stating acidulant is 4mL/min, and the frequency of the ultrasonic reaction is 4.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 5.5, and the modifying agent is adopted
With stearic acid, the stearic addition is the 12% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent,
The rate of addition is 4g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 35kHz, temperature
For 70 DEG C, inner recirculation flow speed is 20mL/min；The response procedures of circular response are as follows in the water bath sonicator：
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
2%, the temperature of circular response is 75 DEG C, pressure 0.4MPa in heated sealed pressurization, and inner recirculation flow speed is 35mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 40g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 75 DEG C, the volume of glycerine and ethanol is 1.3 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 55 DEG C.
Embodiment 6
A kind of preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：
Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form wheat
Bud dextrin solution；
Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 25min, obtain being acidified malt
Dextrin solution；
Step 3, acidifying maltodextrin solution is put into interior circular response kettle, pH adjusting agent and modifying agent is slowly added dropwise
Ultrasonic reaction 4h simultaneously, obtain being esterified maltodextrin crude product；
Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 50min in heated sealed pressurization,
It is filtrated to get esterification maltodextrin highly finished product；
Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, water-bath micro-boiling
Back flow reaction 80min, drying obtains being esterified maltodextrin after ethanol washs after filtering.
The concentration of alcohol of ethanol water in the step 1 is 80%, and the concentration of the maltodextrin is 30%.
Pharmaceutical grade dispersant in the step 1 uses polyethylene glycol, and the addition of the pharmaceutical grade dispersant is malt
Dextrin quality 14%, the stirring use mechanical agitation, mixing speed 2500r/min.
The feed postition of the pharmaceutical grade dispersant is that gradation formula adds, and each addition is 2g/ times, and interval time is
15min。
Acidulant in the step 2 uses acetic acid, and the addition of the acidulant is the 3% of maltodextrin quality, institute
The addition speed for stating acidulant is 4mL/min, and the frequency of the ultrasonic reaction is 2.5kHz.
PH adjusting agent in the step 3 uses sodium hydroxide, and pH adjusting agent controls pH 5.5, and the modifying agent is adopted
With stearic acid, the stearic addition is the 13% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent,
The rate of addition is 4g/min, and the ultrasonic reaction is using circular response in water bath sonicator, supersonic frequency 35kHz, temperature
For 70 DEG C, inner recirculation flow speed is 20mL/min；The response procedures of circular response are as follows in the water bath sonicator：
| Supersonic frequency kHz | Temperature DEG C | Back-flow velocity mL/min | Time min |
| 15 | 50 | 5 | 15 |
| 30 | 65 | 15 | 25 |
| 35 | 70 | 20 | Remaining time |
Inorganic initiator in the step 4 uses sodium peroxydisulfate, and the addition of inorganic initiator is maltodextrin quality
4%, the temperature of circular response is 70 DEG C, pressure 0.6MPa in heated sealed pressurization, and inner recirculation flow speed is 45mL/
min。
The concentration of esterification maltodextrin highly finished product in the step 5 is 45g/L, the temperature of the water-bath micro-boiling back flow reaction
Spend for 70 DEG C, the volume of glycerine and ethanol is 0.9 in the glycerine-alcohol mixed solvent:1.
Ethanol washing in the step 5 is washed using heating stirring, and heating-up temperature is 5 DEG C.
Performance test：
In summary, the present invention has advantages below：
1. the preparation method of the present invention simply controls, esterifying efficiency is fast, and yield is high, solves prior art low yield, essence
The problem of complex procedures processed.
2. the preparation method of the present invention reduces the difficulty of esterification, esterifying efficiency and esterification depth are improved.
3. product prepared by the present invention substantially increases the performance of product, the defects of overcoming existing dextrin product, improve attached
It is value added, expand the application field of dextrin.
4. the present invention can not only provide acidity environment using acetic acid as acidulant, ensure hydroxyl stability early stage, together
When can be used as being modified, form double modified systems with stearic acid, substantially increase the substitution value of maltodextrin.
5. the present invention uses double esterification method, the esterification depth of maltodextrin is deepened, while inorganic initiator can not only
Promotion esterification is played, while also can all be removed in the later stage, does not influence product quality.
6. the present invention uses glycerine-ethanol as solvent, by caused impurity removal in reaction, while by ethanol to sweet
The dissolubility of oil solves the residue problem of glycerine, ensure that the quality of product.
It is understood that above with respect to the specific descriptions of the present invention, it is merely to illustrate the present invention and is not limited to this
Technical scheme described by inventive embodiments.It will be understood by those within the art that still the present invention can be carried out
Modification or equivalent substitution, to reach identical technique effect；As long as meet use needs, all protection scope of the present invention it
It is interior.
Claims (10)
- A kind of 1. preparation method for being esterified maltodextrin, it is characterised in that：Its preparation process is as follows：Step 1, maltodextrin is added into ethanol water, adds pharmaceutical grade dispersant, be mixing uniformly to form malt paste Smart solution；Step 2, acidulant is slowly added dropwise into maltodextrin solution, while ultrasonic reaction 20-30min, obtain being acidified malt Dextrin solution；Step 3, acidifying maltodextrin solution is put into interior circular response kettle, while pH adjusting agent and modifying agent is slowly added dropwise Ultrasonic reaction 2-4h, obtain being esterified maltodextrin crude product；Step 4, inorganic initiator is added in esterification maltodextrin crude product, circular response 30-50min in heated sealed pressurization, It is filtrated to get esterification maltodextrin highly finished product；Step 5, esterification maltodextrin highly finished product are put into reactor, add glycerine-alcohol mixed solvent, the backflow of water-bath micro-boiling 50-80min is reacted, drying obtains being esterified maltodextrin after ethanol washs after filtering.
- A kind of 2. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 1 The concentration of alcohol of ethanol water is 75-80%, and the concentration of the maltodextrin is 20-30%.
- A kind of 3. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 1 Pharmaceutical grade dispersant uses polyvinylpyrrolidone or polyethylene glycol, and the addition of the pharmaceutical grade dispersant is maltodextrin Quality 8-16%, the stirring use mechanical agitation, mixing speed 1500-3000r/min.
- A kind of 4. preparation method for being esterified maltodextrin according to claim 3, it is characterised in that：The pharmaceutical grade is disperseed The feed postition of agent adds for gradation formula, and each addition is 1-2g/ times, interval time 10-20min.
- A kind of 5. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 2 Acidulant uses acetic acid, and the addition of the acidulant is the 1-5% of maltodextrin quality, and the addition speed of the acidulant is 2-5mL/min, the frequency of the ultrasonic reaction is 1.5-5.5kHz.
- A kind of 6. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 3 PH adjusting agent uses sodium hydroxide, and pH is controlled and used stearic acid, the tristearin in 5.5-6.5, the modifying agent by pH adjusting agent The addition of acid is the 10-15% of maltodextrin quality, and the pH adjusting agent adds simultaneously with modifying agent, and the rate of addition is 3-5g/min, the ultrasonic reaction are 60-70 DEG C using circular response in water bath sonicator, supersonic frequency 25-35kHz, temperature, Inner recirculation flow speed is 10-20mL/min.
- A kind of 7. preparation method for being esterified maltodextrin according to claim 6, it is characterised in that：In the water bath sonicator The response procedures of circular response are as follows：
Supersonic frequency kHz Temperature DEG C Back-flow velocity mL/min Time min 10-20 Room temperature -50 0-10 10-20 25-30 60-70 10-20 20-30 35 70 20 Remaining time - A kind of 8. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 4 Inorganic initiator uses sodium peroxydisulfate, and the addition of inorganic initiator is the 1-4% of maltodextrin quality, and the heated sealed adds The temperature of circular response is 70-80 DEG C, pressure 0.3-0.8MPa in pressure, and inner recirculation flow speed is 30-50mL/min.
- A kind of 9. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 5 The concentration of esterification maltodextrin highly finished product is 30-60g/L, and the temperature of the water-bath micro-boiling back flow reaction is 70-80 DEG C, described sweet The volume of glycerine and ethanol is 0.8-1.4 in oil-alcohol mixed solvent:1.
- A kind of 10. preparation method for being esterified maltodextrin according to claim 1, it is characterised in that：In the step 5 Ethanol washing is washed using heating stirring, and heating-up temperature is 50-60 DEG C.
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| CN113598363A (en) * | 2021-08-12 | 2021-11-05 | 海南天壮营养工程有限公司 | Special medical-purpose total-nutrient formula food for cancer-related fatigue |
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