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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 PDF

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Publication number
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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China
Prior art keywords
starch
preparation process
acetylation
adipates
double
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CN201811607167.9A
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Chinese (zh)
Inventor
张晋滔
张晋源
何佳蔚
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Huazhong Agricultural University
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Huazhong Agricultural University
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Priority to CN201811607167.9A priority Critical patent/CN109678976A/en
Publication of CN109678976A publication Critical patent/CN109678976A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B31/00Preparation of derivatives of starch
    • C08B31/02Esters
    • C08B31/04Esters of organic acids, e.g. alkenyl-succinated starch
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/24Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/246Intercrosslinking of at least two polymers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2303/00Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
    • C08J2303/04Starch derivatives
    • C08J2303/06Esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2405/00Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
    • C08J2405/06Pectin; Derivatives thereof

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

A kind of preparation process of the double starch adipates of acetylation
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,.
CN201811607167.9A 2018-12-27 2018-12-27 A kind of preparation process of the double starch adipates of acetylation Pending CN109678976A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
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

Cited By (3)

* Cited by examiner, † Cited by third party
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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