CN109678976A - A kind of preparation process of the double starch adipates of acetylation - Google Patents
A kind of preparation process of the double starch adipates of acetylation Download PDFInfo
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- CN109678976A CN109678976A CN201811607167.9A CN201811607167A CN109678976A CN 109678976 A CN109678976 A CN 109678976A CN 201811607167 A CN201811607167 A CN 201811607167A CN 109678976 A CN109678976 A CN 109678976A
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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
- C08B31/02—Esters
- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/04—Starch derivatives
- C08J2303/06—Esters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/06—Pectin; Derivatives thereof
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- Polymers & Plastics (AREA)
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- Engineering & Computer Science (AREA)
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- Materials Engineering (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a kind of preparation processes of the double starch adipates of acetylation; the following steps are included: step 1; starch is added in rice bran oil and reacts 20-30min at 100-110 DEG C; speed of agitator is 300-400r/min; mixing time is 35-45min, and then washing, centrifugation, drying, are then fed into filling pocket; it adds water and is configured to starch emulsion, then add pectin.Rice bran oil of the present invention has a variety of fatty acid isoreactivity ingredients, a large amount of hydroxyl is generated at 100-110 DEG C, it is combined with starch, it improves starch and acetic anhydride is esterified and adipic acid cross-linking efficiency, the pectin of addition can be improved the viscosity of starch emulsion simultaneously, improve starch cross-linking efficiency in subsequent cross-linking process.
Description
Technical field
The present invention relates to converted starch preparation technical fields, and in particular to a kind of preparation of the double starch adipates of acetylation
Technique.
Background technique
The double starch adipates of acetylation are also known as dual denaturation glutinous rice flour, for a kind of white to similar white powder, odorless,
It is tasteless, cold water, ethyl alcohol are not dissolved in, iodine is met and reddens the compound of brown, be a kind of widely used chemically modified starch, product is not
The only characteristic intrinsic with glutinous rice, such as faint scent, waxy, stickiness etc., also have good anti-aging, mouldability of converted starch etc.
Characteristic can be to utilize the mixed of adipic acid and acetic anhydride using the processing of the cakes such as Deep-Fried Glutinous Rice Cake Stuffed with Bean Paste, green group, the double starch adipates of acetylation
It closes acid anhydrides starch is crosslinked and is esterified, the composite modified starch that dual denaturation obtains, modified starch is carried out to starch
Aqueous, good transparency, low-temperature stability and acid resistance with splendid anti-folding introduce acetyl group, have starch lower
Gelatinization point, higher hot viscosity and good film forming and ageing resistance, the Hu that cross-bond can then increase starch it is glutinous
Degree improves heat paste stability and freeze-thaw stability.
Starch gelatinization: the phenomenon that starch with translucent colloid is become after water heat together under certain condition.Starch milk is heated
Afterwards, in certain temperature range, amylum body beginning is destroyed, and crystal structure disappears, and enlarged volume, viscosity steeply rises, in sticky
Paste, become noncrystalline starch.The gelatinization point of various starch with the difference of raw material type, amylum body size etc. and
It is different.The essence of gelatinization is that the hydrogen bond in starch granules orderly and between the starch molecule of disordered state disconnects, and being dispersed in water becomes
Colloidal solution, gelatinization process are divided into three phases, 1, reversible water suction stage, 2, irreversible water suction stage, 3, amylum body disintegration rank
Section becomes the double starch adipates of acetylation by converted starch obtained from mixed anhydride cross-linked esterification using ative starch as raw material.
The double starch adipate preparation process conditions differences of acetylation in the prior art, obtained starch heat paste stability,
The performances such as viscosity will be variant, changes process conditions, prepares the double starch adipates of optimal acetylation.
Chinese patent literature (notification number: CN104311678B) discloses a kind of double starch adipate starch of acetylation
Preparation method, comprising the following steps: the tapioca of 1000 unit masses is put into reactor tank and adds water and stirs modulation by step 1
It is greater than 30% starch milk at concentration, 50-80 unit mass sodium chloride is added when the tapioca is mixed with water;Step
Two, starch milk is stirred, the lye that concentration is 1-3mol/L is continuously added during stirring;Step 3, in whipping process
The pH value of starch milk is surveyed, when pH value reaches 10.0-13.0, stops addition lye;Step 4 vacuumizes reactor tank,
Continue to stir and rapidly join in the starch milk 24 unit mass adipic anhydrides~and 20 30 unit mass acetic anhydride, add
Heat is simultaneously reacted 1-1.5 hours, and common process condition, thus the change that different technology conditions are prepared are used in converted starch preparation
Property starch performance it is different.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation processes of the double starch adipates of acetylation, to solve above-mentioned background
The problem of being proposed in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Starch is added in rice bran oil at 100-110 DEG C and reacts 20-30min by step 1, speed of agitator 300-
400r/min, mixing time 35-45min, then washing, centrifugation, drying, are then fed into filling pocket, add water and match
Starch emulsion is made, then adds pectin, temperature is then risen to 55-65 DEG C, reaction by speed of agitator 100-200r/min
25-35min obtains prewired cream, and prepared prewired cream is then got to reactor tank, adjusts pH value with dilute alkaline soln;
Step 2, is added adipic acid and acetic anhydride is reacted, and reacts 20-120min, then adds diluted acid and stops instead
It answers, then cleans, washing, scraper dehydration, pneumatic conveying drying, screening, packed products, storage.
Be as further scheme of the invention: the starch emulsion concentration is 18-27 Baume degrees.
Be as further scheme of the invention: the pectin additional amount is the 2-5% of starch emulsion.
Be as further scheme of the invention: it is 7.8-9.5 that the dilute alkaline soln, which adjusts pH value,.
Be as further scheme of the invention: the adipic acid additive amount is no more than starch on dry basis mass fraction
0.12%.
Be as further scheme of the invention: the acetic anhydride additive amount is no more than starch on dry basis mass fraction
8%.
Be as further scheme of the invention: acetic anhydride adding speed is 200-350L/h.
Be as further scheme of the invention: acetic anhydride adding speed is 275L/h.
Be as further scheme of the invention: the addition diluted acid stopped reaction pH value is 4.5-6.5.
Be as further scheme of the invention: the addition diluted acid stopped reaction pH value is 5.5.
Compared with prior art, the present invention have it is following the utility model has the advantages that
Rice bran oil of the present invention has a variety of fatty acid isoreactivity ingredients, a large amount of hydroxyl is generated at 100-110 DEG C, with shallow lake
Powder combines, and improves starch and acetic anhydride is esterified and adipic acid cross-linking efficiency, while the pectin added can be improved starch emulsion
Viscosity, improve starch cross-linking efficiency in subsequent cross-linking process, when embodiment 6 is relative to comparative example 3,20min viscosity improve
Improve 2900mPa.S when 4670mPa.S, 0min, it is known that from 0-20min, anti-shear performance is been significantly enhanced, simultaneously plus
The pectin entered can also improve anti-shear performance.
Specific embodiment
Combined with specific embodiments below, technical scheme in the embodiment of the invention is clearly and completely described, shows
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Process water is injected in filling pocket, ative starch is put into, adjusting starch concentration is 18 Baume degrees, the shallow lake that will be regulated
Slurry gets to reactor tank;With dilute alkaline soln adjust pH value be 7.8, be added be no more than starch on dry basis mass fraction 0.12% oneself two
Acid and reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride adding speed be 200L/h, add acetic acid
After acid anhydride, acid adding stopped reaction 4.5 then cleans, then washs in disk plate centrifuge, and starch milk conductivity after washing≤
3000 μ s/cm, then scraper is dehydrated, then dry in airflow dryer, and dry a tail wind temperature is 55 DEG C, dry moisture content of finished products
< 18% is then sized to fineness >=99.0%, then packed products, finished product net content 25kg, is then put in storage.
Embodiment 2:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Process water is injected in filling pocket, ative starch is put into, adjusting starch concentration is 27 Baume degrees, the shallow lake that will be regulated
Slurry gets to reactor tank;With dilute alkaline soln adjust pH value be 9.5, be added be no more than starch on dry basis mass fraction 0.12% oneself two
Acid and reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride adding speed be 350L/h, add acetic acid
After acid anhydride, acid adding stopped reaction 6.5 then cleans, then washs in disk plate centrifuge, and starch milk conductivity after washing≤
3000 μ s/cm, then scraper is dehydrated, then dry in airflow dryer, and dry a tail wind temperature is 55 DEG C, dry moisture content of finished products
< 18% is then sized to fineness >=99.0%, then packed products, finished product net content 25kg, is then put in storage.
Embodiment 3:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Process water is injected in filling pocket, puts into ative starch, adjusting starch concentration is 22.5 Baume degrees, by what is regulated
Starch slurry gets to reactor tank;Adjusting pH value with dilute alkaline soln is 8.7, oneself for being no more than starch on dry basis mass fraction 0.12% is added
It diacid and is reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride adding speed is 275L/h, adds vinegar
After acid anhydrides, acid adding stopped reaction 5.5 then cleans, then washs in disk plate centrifuge, starch milk conductivity after washing
≤ 3000 μ s/cm, then scraper is dehydrated, then dry in airflow dryer, and dry a tail wind temperature is 55 DEG C, dry product water
Divide < 18%, be then sized to fineness >=99.0%, then packed products, finished product net content 25kg is then put in storage.
Embodiment 4:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Starch is added in rice bran oil at 100 DEG C and reacts 20min, speed of agitator 300r/min, mixing time is
35min, then washing, centrifugation, drying, are then fed into filling pocket, add water and be configured to starch emulsion, then add
Temperature is then risen to 55 DEG C by 2% pectin of starch emulsion, speed of agitator 100r/min, is reacted 25min, is obtained prewired
Prepared prewired cream is then got to reactor tank by cream, and adjusting pH value with dilute alkaline soln is 7.8, is added and is no more than starch on dry basis
It the adipic acid of mass fraction 0.12% and is reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride addition
Speed is 200L/h, and after adding acetic anhydride, acid adding stopped reaction 4.5 then cleans, then washes in disk plate centrifuge
It washs, starch milk conductivity≤3000 μ s/cm after washing, then scraper is dehydrated, then dry in airflow dryer, dry a tail wind
Temperature is 55 DEG C, and dry moisture content of finished products < 18% is then sized to fineness >=99.0%, then packed products, finished product net content
25kg is then put in storage.
Embodiment 5:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Starch is added in rice bran oil at 110 DEG C and reacts 30min, speed of agitator 400r/min, mixing time is
45min, then washing, centrifugation, drying, are then fed into filling pocket, add water and be configured to starch emulsion, then add
Temperature is then risen to 65 DEG C by 5% pectin of starch emulsion, speed of agitator 200r/min, is reacted 35min, is obtained prewired
Prepared prewired cream is then got to reactor tank by cream, and adjusting pH value with dilute alkaline soln is 9.5, is added and is no more than starch on dry basis
It the adipic acid of mass fraction 0.12% and is reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride addition
Speed is 350L/h, and after adding acetic anhydride, acid adding stopped reaction 6.5 then cleans, then washes in disk plate centrifuge
It washs, starch milk conductivity≤3000 μ s/cm after washing, then scraper is dehydrated, then dry in airflow dryer, dry a tail wind
Temperature is 55 DEG C, and dry moisture content of finished products < 18% is then sized to fineness >=99.0%, then packed products, finished product net content
25kg is then put in storage.
Embodiment 6:
A kind of preparation process of the double starch adipates of acetylation, comprising the following steps:
Starch is added in rice bran oil at 105 DEG C and reacts 25min, speed of agitator 350r/min, mixing time is
40min, then washing, centrifugation, drying, are then fed into filling pocket, add water and be configured to starch emulsion, then add
Temperature is then risen to 60 DEG C by 3.5% pectin of starch emulsion, speed of agitator 150r/min, is reacted 30min, is obtained pre-
With cream, prepared prewired cream is then got into reactor tank, adjusting pH value with dilute alkaline soln is 8.7, is added dry no more than starch
It the adipic acid of base mass fraction 0.12% and is reacted no more than the acetic anhydride of starch on dry basis mass fraction 8%, acetic anhydride adds
Acceleration is 275L/h, and after adding acetic anhydride, acid adding stopped reaction 5.5 then cleans, then washes in disk plate centrifuge
It washs, starch milk conductivity≤3000 μ s/cm after washing, then scraper is dehydrated, then dry in airflow dryer, dry a tail wind
Temperature is 55 DEG C, and dry moisture content of finished products < 18% is then sized to fineness >=99.0%, then packed products, finished product net content
25kg is then put in storage.
Comparative example 1:
It is not both not using rice bran oil processing with embodiment 6.
Comparative example 2:
It is not both to be not added with pectin with embodiment 6.
Comparative example 3:
A kind of double starch adipates shallow lakes of acetylation are disclosed using Chinese patent literature (notification number: CN104311678B)
The raw material and method of embodiment 2 in the preparation method of powder.
Anti-shear performance test
Test method: embodiment 1-6 and comparative example 1-3 starch are configured to 3% starch milk, then in 90 DEG C of water-baths
Gelatinization 20min is carried out, is then cooled to room temperature, shearing 0-20min is then carried out at 1000r/min, measures its viscosity
(mPa.S)。
Viscosity improves 4670mPa.S when embodiment 6 is relative to comparative example 3,20min, and when 0min improves
2900mPa.S, it is known that from 0-20min, anti-shear performance is been significantly enhanced, while the pectin being added can also improve shear resistant
Energy.
Following table is the present invention, gelatinization point, peak paste viscosity performance test standard
Testing standard | |
Cold paste viscosity | GB/T 24427.7-2008 |
Peak paste viscosity | GB/T 24427.7-2008 |
Embodiment 1-6 and comparative example 1-3 the performance test results are as follows
Cold paste viscosity (BU) | Peak paste viscosity (BU) | |
Embodiment 1 | 1570 | 1080 |
Embodiment 2 | 1540 | 1050 |
Embodiment 3 | 1510 | 1100 |
Embodiment 4 | 1740 | 1190 |
Embodiment 5 | 1720 | 1170 |
Embodiment 6 | 1750 | 1210 |
Comparative example 1 | 1620 | 1150 |
Comparative example 2 | 1670 | 1140 |
Comparative example 3 | 1130 | 850 |
It is obtained from embodiment 1-6 and comparative example 1-3, the embodiment of the present invention 6 is relative to comparative example 3, cold paste viscosity, peak value
Viscosity, which all has, to be significantly improved.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1. a kind of preparation process of the double starch adipates of acetylation, which comprises the following steps:
Starch is added in rice bran oil at 100-110 DEG C and reacts 20-30min by step 1, speed of agitator 300-400r/
Min, mixing time 35-45min, then washing, centrifugation, drying, are then fed into filling pocket, add water and be configured to form sediment
Then powder lotion adds pectin, temperature is then risen to 55-65 DEG C by speed of agitator 100-200r/min, reacts 25-
35min obtains prewired cream, and prepared prewired cream is then got to reactor tank, adjusts pH value with dilute alkaline soln;
Step 2, is added adipic acid and acetic anhydride is reacted, and reacts 20-120min, then adds diluted acid stopped reaction, so
After clean, washing, scraper dehydration, pneumatic conveying drying, screening, packed products, storage.
2. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that the shallow lake
Powder emulsion concentration is 18-27 Baume degrees.
3. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that the fruit
Glue additional amount is the 2-5% of starch emulsion.
4. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that described dilute
It is 7.8-9.5 that aqueous slkali, which adjusts pH value,.
5. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that it is described oneself
Diacid additive amount is no more than the 0.12% of starch on dry basis mass fraction.
6. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that the vinegar
Acid anhydrides additive amount is no more than the 8% of starch on dry basis mass fraction.
7. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that acetic anhydride
Adding speed is 200-350L/h.
8. a kind of preparation process of the double starch adipates of acetylation according to claim 7, which is characterized in that acetic anhydride
Adding speed is 275L/h.
9. a kind of preparation process of the double starch adipates of acetylation according to claim 1, which is characterized in that described to add
Entering diluted acid stopped reaction pH value is 4.5-6.5.
10. a kind of preparation process of the double starch adipates of acetylation according to claim 9, which is characterized in that described
It is 5.5 that diluted acid stopped reaction pH value, which is added,.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114916573A (en) * | 2022-05-26 | 2022-08-19 | 大连工业大学 | Pre-mixed flour of mochi bread |
CN118217915A (en) * | 2024-05-22 | 2024-06-21 | 吉林华昊华丰生物科技有限公司 | Mixing equipment and process for production and preparation of acetylated distarch adipate |
-
2018
- 2018-12-27 CN CN201811607167.9A patent/CN109678976A/en active Pending
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114916573A (en) * | 2022-05-26 | 2022-08-19 | 大连工业大学 | Pre-mixed flour of mochi bread |
CN118217915A (en) * | 2024-05-22 | 2024-06-21 | 吉林华昊华丰生物科技有限公司 | Mixing equipment and process for production and preparation of acetylated distarch adipate |
CN118217915B (en) * | 2024-05-22 | 2024-08-13 | 吉林华昊华丰生物科技有限公司 | Mixing equipment and process for production and preparation of acetylated distarch adipate |
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