CN108285497A - A kind of preparation method of acetate starch - Google Patents
A kind of preparation method of acetate starch Download PDFInfo
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- CN108285497A CN108285497A CN201711434348.1A CN201711434348A CN108285497A CN 108285497 A CN108285497 A CN 108285497A CN 201711434348 A CN201711434348 A CN 201711434348A CN 108285497 A CN108285497 A CN 108285497A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
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- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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Abstract
The invention belongs to converted starch preparing technical fields, and in particular to a kind of preparation method of acetate starch.The preparation method of acetate starch of the present invention; using tapioca as raw material; acetic anhydride is esterifying reagent; the cassava acetate starch of different acetyl contents and degree of substitution is prepared for by acetylization reaction, the acetyl content and degree of substitution of gained acetate starch meet the requirement of its market-oriented application field.
Description
Technical field
The invention belongs to converted starch preparing technical fields, and in particular to a kind of preparation method of acetate starch.
Background technology
Starch is the main component of green plants fruit, seed, root tuber, is CO in air2And H2O is synthesized through photosynthesis
Storage polysaccharide.As the recyclability resource for being only second to cellulose, starch is main carbohydrate in human diet,
It is also the main source of body energy.China is a large agricultural country, and starch resource is abundant, and great variety of goods, includes mainly paddy
The starch resource etc. of object starch, potato starch, bean starch and other kinds.Currently, industrialized high-purity starch and its spreading out
Biology is widely used in the different fields such as food, medicine, weaving, papermaking, chemical industry.Therefore, starch and its product deep processing
Have a vast market foreground.
Native starch is although widely used, but its intrinsic some characteristics such as cold water is insoluble, paste liquid is made in heat, acid, shearing
The defects of unstable under, easy to aging, film forming and the transparency are bad, freeze-thaw stability is poor greatly limits its application.Therefore,
Often ative starch is modified in the prior art, to improve starch structure and property, increase functional or new characteristic, to meet
The requirement of various new technologies, expands starch application field, and this product for changing the original property of starch is referred to as converted starch.
Acetate starch is a kind of widely used converted starch, and acetate starch is also known as acetylated starch, is in alkali
Property under the conditions of starch and acetic anhydride, vinyl acetate and acetic acid etc. react a kind of esterification starch generated through esterifying agent.Acetate forms sediment
Powder is white powder, and the retrogradation of gelatinized corn starch is low, has that acidproof, alkaline-resisting, thermal stability and freeze-thaw stability are high, transparency it is good with
And it is intermolecular be not easy to form the good characteristics such as hydrogen bond, while being improved in various degree in viscosity, dilation and solubility,
Peomote the interaction of starch and water.This is because accessing one on the molecule of acetate starch there is steric hindrance to make
Acetyl group significantly reduces gelatinization point to weaken the association of hydrogen bond, and makes its condensational growth, freeze-thaw stability
Property, thermal stability and transparency obtain improving and improve.In addition, Kayode O A etc. point out that the acetylation of ative starch also expands
The rheology volume of big starch system, and then improve the viscosity and consistency coefficient of starch\；It is pointed out in the reports such as Ancona D B
The molecular force of steric hindrance and generation caused by acetyl group, substantially reduces the Hyarogen-bonding between starch molecule,
To make the freeze-thaw stability of starch be improved, starch retrogradation is inhibited；Research also indicates that the acetate of low degree of substitution forms sediment
The property of powder is stablized relatively, and is widely used in food industry；In addition, acetate starch can improve the steady of ative starch
Qualitative and ageing resistance.Recently, low degree of substitution (DS) starch due to good film forming, bound, stability, texture,
Adhesion strength and thickening property, and cause the great commercial interest of people.
Currently, acetate starch has had very extensive use scope, including bakery product, can, cake filling in food
The numerous areas such as material, tartar sauce, frozen food, baby food, salad dressing and snack food.Acetate starch is also commonly used in
In chilled food, to reduce degree of aging of the food in cold storage procedure.According to United States Federal Regulations, all acetate starch exist
In application, acetyl content is no more than 2.5% in food.Therefore, it is suitable that performance stabilization, acetyl content how to be prepared
Acetate starch has great importance.
Invention content
For this purpose, technical problem to be solved by the present invention lies in provide a kind of preparation method of acetate starch.
In order to solve the above technical problems, a kind of preparation method of acetate starch of the present invention, includes the following steps：
(1) it takes starch to add water mixing that starch emulsion is made, and lye is added and carries out basification；
(2) acetylating agent is added dropwise into the starch emulsion after basification, is carried out under 25-45 DEG C, pH alkaline conditions
Esterification；
(3) reaction solution is adjusted with acid solution to be neutralized, and reaction solution is separated by solid-liquid separation after reaction；
(4) take solid portion to be washed, be dried after separation of solid and liquid to get.
In the step (1), the mass concentration for controlling the starch emulsion is 30-50wt%.
In the step (1), the lye is the sodium hydroxide solution of 2-4wt%.
In the step (1), the starch is tapioca.
In the step (2), the addition of the acetylating agent accounts for the 1-7wt% of the starch emulsion quality.
In the step (2), the acetylating agent is acetic anhydride.
Further include that the sodium hydroxide solution of 2-4wt% is added dropwise to control reaction solution pH7.5-10.0 in the step (2)
Step.
In the step (2), the reaction time of esterification is 1.0-3.0h.
In the step (3), the neutralization procedure is to adjust reaction solution pH6.0- with the hydrochloric acid solution of 0.4-0.6mol/L
6.5。
In the step (4), the drying steps are pneumatic conveying drying.
The preparation method of acetate starch of the present invention, using tapioca as raw material, acetic anhydride is esterifying reagent, is passed through
Acetylization reaction is prepared for the cassava acetate starch of different acetyl contents and degree of substitution, the acetyl group of gained acetate starch
Content and degree of substitution meet the requirement of its market-oriented application field.
The present invention is by the influence of structure and physicochemical properties to different acetyl content cassava acetate starch, such as
Scanning electron microscope (SEM), Birefringence microscope, infrared spectrum (FT-IR), viscosity, transparency and freeze-thaw stability.As a result table
It is bright：Petrographic microscope the result shows that the front and back Birefringence of tapioca esterification is still high-visible, illustrate starch internal structure
The esterification of destruction unobvious, tapioca and acetic anhydride is happened at the surface of tapioca particle；Infrared spectrum collection of illustrative plates knot
Fruit shows acetate starch due to introducing new chemical group, in 1375cm-1、1252cm-1And 1013cm-1Occur apparent
Starch ester characteristic absorption peak, in 1733cm-1There is apparent carbonyl characteristic absorption peak in place, special with the increase of degree of substitution
The peak height for levying absorption peak increases apparent, esterification degree intensification；According to the acetyl content pair of cassava acetate starch sample
Effect On Gelatinization Characteristics, transparency and freeze-thaw stability carry out comprehensive systematic analysis technique, and tapioca ester is viscous after esterification treatment
Degree increases, and gelatinization point reduces, and with the increase of acetyl content, gelatinization point reduction and viscosity increase apparent.Cassava acetic acid
The syneresis rate of ester starch reduces, and freeze-thaw stability is significantly improved；The transparency of acetate starch is with acetyl content
It is in increased trend to increase, more beneficial to the demand of application market.
Description of the drawings
In order to make the content of the present invention more clearly understood, it below according to specific embodiments of the present invention and combines
Attached drawing, the present invention is described in further detail, wherein
Fig. 1 is the process flow chart of acetate preparation method of the present invention；
Fig. 2 is the scanning electron microscopic picture of different acetyl content tapiocas；
Fig. 3 is Birefringence structure chart of the different acetyl contents to cassava acetate；
Fig. 4 is the infrared absorpting light spectra of different acetyl content acetate starch；
Fig. 5 is the Brabender viscosity profiles of different acetyl content acetate starch；
Fig. 6 is the light transmittance result of different acetyl content acetate starch paste.
Specific implementation mode
Embodiment 1
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) solid portion washing is collected to remove the impurity such as unreacted sodium hydroxide, opens retort discharge port valve,
Starch milk is pumped into the first order of multitube cyclone, washings are added from the afterbody of cyclone, and the two carries out counter current contacting,
Converted starch breast after washing is drawn from the underflow of most final stage, and into next step centrifugal dehydration, the washings after separation are sent to dirt
Water treatment system is handled, and is discharged after up to standard；
Acetate starch breast after washing is pumped into horizontal centrifuge to be dehydrated, by rotary drum high speed rotation generate from
Mental and physical efforts are automatically drained out converted starch particle entrapment in acetate starch breast in rotary drum and under force to outside machine, simultaneously
Under the action of the centrifugal force, filtrate by rotary drum aperture discharge machine outside, to achieve the purpose that solid-liquor separation, filtered filtrate is also
Containing certain converted starch, recyclable progress secondary centrifuging dehydration, then be sent to sewage water treatment system and handled, after up to standard
Discharge；
Processing is dried using pneumatic conveying drying method in converted starch after centrifugal dehydration, and not only the thermal efficiency is high, dry speed
Degree is fast, and product is powdered, convenient for follow-up screening；The pneumatic drier with disperser is added in wet acetic acid ester starch, point
Device is dissipated by material scattering, and is thrown into dry bottom of the tube.The hot wind of converted starch and heater comes into full contact with, and moment realizes that heat transfer passes
Matter process, and with hot wind cocurrent and on, finally enter cyclone separator and hot wind separator.Hot wind is discharged into air, after dry
Converted starch enters screening link with conveyer belt；
Starch after pneumatic conveying drying is mostly uniform starch, first passes through linear vibrating screen, with 100 mesh screens into
Row screening, for a small number of bulky grain starch, vibrating screen can play pulverization, and only a few oversize is collected to send back to and is sized mixing
It is reprocessed, screenings is the product of qualification, and communicated band is delivered to the packaging that carries out an acceptance inspection in next step；
Qualified product with 25kg woven bags using automatic packaging machine packed to get.
Embodiment 2
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,30 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 3
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,35 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 4
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,40 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 5
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5, control temperature 45 C carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 6
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH7.5-7.9, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 7.5-7.9,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 7
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.6-9.0, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in pH8.6-9.0,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride with
20min is added dropwise and is advisable before reaction terminates；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 8
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH9.1-9.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in pH9.1-9.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride with
20min is added dropwise and is advisable before reaction terminates；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 9
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH9.6-10.0, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in pH9.6-10.0,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride with
20min is added dropwise and is advisable before reaction terminates；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 10
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 1wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 11
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 2wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 12
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 3wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 13
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 4wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 14
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 5wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 15
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 6wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 16
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 1h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 17
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 1.5h；The rate of addition of the acetic anhydride with
20min is added dropwise and is advisable before reaction terminates；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 18
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2.5h；The rate of addition of the acetic anhydride with
20min is added dropwise and is advisable before reaction terminates；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 19
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion (w/w density about 1.18) that mass concentration is 40wt%,
Even stirring 10min keeps starch fully dispersed, obtains uniform starch emulsion, and alkalize with the sodium hydroxide solution of 3wt%
Processing adjusts lotion pH8.0-8.5, then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 3wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 3h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.5mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 20
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion that mass concentration is 30wt%, uniform stirring 10min makes shallow lake
Powder is fully dispersed, obtains uniform starch emulsion, and carry out basification with the sodium hydroxide solution of 2wt%, adjusts lotion
PH8.0-8.5 then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 2wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.4mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Embodiment 21
As shown in Figure 1, the preparation method of acetate starch of the present invention includes the following steps：
(1) take tapioca that water is added to prepare to obtain the starch emulsion that mass concentration is 50wt%, uniform stirring 10min makes shallow lake
Powder is fully dispersed, obtains uniform starch emulsion, and carry out basification with the sodium hydroxide solution of 4wt%, adjusts lotion
PH8.0-8.5 then stands 10min；
(2) acetic anhydride is added dropwise into the starch emulsion after basification and is esterified (the additive amount of the acetic anhydride
Account for the 7wt% of the starch milk liquid measure), while using atomizer that the sodium hydroxide solution of 4wt% is added dropwise to control reaction solution
PH stable in 8.0-8.5,25 DEG C of temperature of control carries out reaction esterification 2h；The rate of addition of the acetic anhydride is with anti-
20min is added dropwise and is advisable before should terminating；
(3) after reaction, the hydrochloric acid solution of 0.6mol/L is added dropwise with nozzle with adjust the pH to 6.0-6.5 of reaction solution into
Row neutralizes, and with stopped reaction, then detaches reaction solution centrifugal solid-liquid；
(4) with 1 step of embodiment (4).
Experimental example
One, the measurement of acetate starch acetyl content and degree of substitution
Acetate starch obtained in 5.000g embodiments 1-19 is accurately weighed 50mL is added and steams in 250mL iodine flasks
3 drop phenolphthalein indicators are added after mixing, are titrated with the NaOH of 0.1mol/L for distilled water, until blush does not disappear for terminal, with cassava
Ative starch is control.25mL0.5mol/LNaOH standard solution is added, in room temperature reaction 60min.It uses after reaction
It is terminal, record volume V that the HCl standard solution of 0.5mol/L, which is titrated to red disappear,1(mL).Blank is done with cassava ative starch
Control, the volume V of record consumption hydrochloric acid2(mL).Due to-OH there are three in each glucose unit of ative starch, and it is modified
Starch is-COCH2CH3The product that substitution-OH is obtained, theoretic maximum degree of substitution (DS) are 3.According to experimental data, as the following formula
(formula 1 and formula 2) calculates：
Wherein, W is acetyl group mass fraction；V1By the volume (mL) for the HCl that sample consumes；V2For ative starch blank institute
The volume (mL) of the HCl of consumption；m1、m2The quality (g) of test sample and ative starch blank is indicated respectively；C is HCl standard solution
Concentration (mol/L)；0.043 for the comparable acetyl group quality of the normal hydrochloric acid of a concentration of 1.000mol/L of 1mL.
The acetyl content that acetate starch is made in embodiment 1-19 and degree of substitution are recorded respectively in the following table 1.
The acetyl content and degree of substitution of 1 acetate starch of table
| Number | Acetyl content (%) | Degree of substitution |
| Embodiment 1 | 2.40 | 0.093 |
| Embodiment 2 | 1.73 | 0.067 |
| Embodiment 3 | 1.68 | 0.064 |
| Embodiment 4 | 1.62 | 0.062 |
| Embodiment 5 | 1.54 | 0.059 |
| Embodiment 6 | 1.46 | 0.048 |
| Embodiment 7 | 2.25 | 0.087 |
| Embodiment 8 | 2.19 | 0.084 |
| Embodiment 9 | 2.16 | 0.082 |
| Embodiment 10 | 0.26 | 0.011 |
| Embodiment 11 | 0.85 | 0.035 |
| Embodiment 12 | 0.99 | 0.039 |
| Embodiment 13 | 1.41 | 0.055 |
| Embodiment 14 | 1.75 | 0.081 |
| Embodiment 15 | 2.01 | 0.092 |
| Embodiment 16 | 1.77 | 0.068 |
| Embodiment 17 | 1.81 | 0.069 |
| Embodiment 18 | 1.99 | 0.075 |
| Embodiment 19 | 1.85 | 0.071 |
From upper table data as it can be seen that its acetyl content of acetate starch made from the method for the invention reaches as high as
2.40%, degree of substitution is up to 0.093, can meet the performance requirement of acetate starch.
Two, acetate starch structure and property representation
1, influence of the different acetyl contents to cassava acetate starch grain structure
Field emission scanning electron microscope (SEM) analysis test method and condition：Scanning electron microscope is to utilize fine focusing electronics
The various physical signals that beam is ejected when sample surfaces scan are imaged to modulate, and wherein secondary electron and backscattered electron are seen
The starch sample dried on a small quantity is uniformly pasted onto on sample stage by the pattern for examining sample by sample to be tested with two-sided conducting resinl,
Metal spraying under vacuum is then attached on objective table simultaneously label, then sample is put into sample room, observes under the microscope
Starch granules pattern shoots representative pattern photo, and sample is amplified 500 times and 2000 times shooting observations respectively.
The scanning electron microscopic picture of different acetyl content tapiocas, CAS-1, CAS-2, CAS- are set forth in Fig. 2
3, CAS-4, CAS-5, CAS-6 and CAS-7 respectively represent cassava acetate starch obtained by embodiment 10-15 and embodiment 1
As a result (similarly hereinafter).From figure 2 it can be seen that ative starch particle is in regular and smooth round or ellipse, and cassava acetate
Starch granules regularity is deteriorated, and in the form of sheets or fine particle shape, starch ester surface become rough and uneven in surface.It can be seen that esterification is anti-
The surface of starch granules should be happened at.Cassava ative starch particle surface is smooth, the tapioca granulated after esterification treatment
Shape is not substantially change, and partial particulate surface then becomes uneven, rough, illustrates the esterification of low degree of substitution
Reaction is happened at starch particle surface, grain structure of the acetylation without obviously destruction starch.Starch particle surfaces is bright individually
Point be possible in reaction process by the result of alkali liquid corrosion.
2, influence of the different acetyl contents to cassava acetate starch Birefringence structure
There are crystallization and amorphous two different structures inside starch granules, the starch molecular chain in crystal region is ordered into
Arrangement, and the starch molecular chain of amorphous region is disorderly arranged, due to difference of two kinds of structures in density and refractive index,
To polarisation by when form Birefringence.Starch can be intuitively observed after denaturation using petrographic microscope, it is brilliant
Whether body structure changes.Starch sample is tuned into starch milk according to a certain percentage, is dripped in the glass that on glass slide, closes the lid
Piece is put on objective table, selects suitable amplification factor and brightness, observes and shoot the Birefringence of sample under polarized light
Photo.
The Birefringence pattern of log sweet potato starch particle and cassava acetate starch particle is shown in Fig. 3.Log sweet potato starch particle
Birefringence it is apparent, be located at tapioca granular center in apparent positive cross and Saint Andrew's cross cross shaped head, crosspoint.Through esterification
The Birefringence of tapioca is obviously weakened after processing, this illustrates that esterification is happened at the amorphous domain of starch.Through
After over-churning reaction, the crystal structure of cassava acetate starch is not destroyed significantly, and good particle can be still kept
Structure.Illustrate crystal region structure of the esterification without obviously destruction tapioca.
3, the infrared spectrum analysis of starch acetate
Using KBr pressed disc methods, specific method for making sample is for sample preparation in examination of infrared spectrum：About 2mg samples are weighed, are added dry
After dry KBr powder is ground uniformly together, it is fitted into compression mold and vacuumizes, it is tabletted.The KBr tablettings that will be suppressed, dress
Enter on specimen holder, carries out IR spectrum scanning, resolution ratio 2cm-1, scanning range 4000-400cm-1。
Fig. 4 is the infrared absorpting light spectra of ative starch and converted starch.The basic component units of ative starch are dewatered grapes
Sugar, the infrared absorption peak positions and structural assignment of main feature group are respectively：3380cm-1For the stretching vibration peak of O-H,
2930cm-1For CH2CH asymmetric stretching vibration absorption peaks；In fingerprint region 1020cm-1、1081cm-1、1158cm-1Three of place
Absorption peak is respectively the C-O stretching vibration absworption peaks of primary alconol, secondary alcohol, the tertiary alcohol.1654cm-1For the bending vibration absorption peak of O-H.
1340cm-1-1500cm-1For the bending vibration absorption peak of CH；978cm-1Master Home is in cyclic ethers C-O-C absorption peaks；926cm-1For
The D types peak ring vibration of glucopyranose.Cassava acetate starch is in 1733cm-1There is new absorption peak in position, this is carbonyl
Feature inhale peak.1375cm-1And 1252cm-1Place is also respectively CH3The stretching vibration absworption peak at stretching absorbance peak and C-O singly-bounds,
There is-COCH during esterification3The generation of group, it was demonstrated that the generation of esterification.Thus illustrate occur second in starch
Acyl group, tapioca have synthesized cassava acetate starch with acetic anhydride effect.With the increase of degree of substitution, 1654cm-1Neighbouring
Polysaccharide hydroxyl peak is also gradually reduced, and illustrates that the hydroxyl on starch glucose unit also gradually decreases.1733cm-1Neighbouring carbonyl
Peak gradually increases, and is gradually replaced by acetyl group after the hydrogen atom on starch glucose unit hydroxyl is reacted and esterification occurs instead
It answers, while with the raising of degree of substitution measured value, acetyl content increases, this also demonstrates degree of substitution measurement to a certain extent
The accuracy of value.
4, influence of the different acetyl contents to cassava acetate starch viscosity
Brabender viscosity curves measure：Accurately weighing 6.00g (butt) starch sample is placed in Brabender viscosity apparatus
Revolution cup in, a certain amount of deionized water is added, make starch milk mass fraction be 6% (w/w), setting torque be 350cmg,
The rotating speed for turning round cup is 250r/min.Starch milk is heated up with 1.5 DEG C/min speed, is started to warm up to 95 DEG C from 30 DEG C, is then protected
Warm 30min, then 50 DEG C are cooled to from 95 DEG C with the speed of 1.5 DEG C/min, keep the temperature 30min.Brabender viscosity apparatus continuously records
The variation of gelatinized corn starch viscosity, obtains Brabender viscosity curves during all.
The acetate starch of different acetyl contents and the intrinsic viscosity value of tapioca are shown in respectively shown in Fig. 5 and table 2.From
Fig. 5 and 2 data of table are it is found that the viscosity of cassava ative starch is less than the viscosity of cassava acetate starch, the paste of cassava acetate starch
Change temperature and is less than cassava ative starch gelatinization point.With the increase of acetyl content, cassava acetate starch gelatinization point is presented
Reduction trend, peak viscosity are in increased trend.Peak paste viscosity represents the ability of gelatinized corn starch free wxpansion before disintegration, starch
Expansion and amylopectin have substantial connection.Disintegration value increases, and shows that gelatinized corn starch heat-resisting ability weakens, and paste stability reduces,
The hot and cold paste stability of starch increases.The main reason for cassava acetate starch gelatinization point reduces has two：One side starch becomes
Acetyl group is introduced after property, the hydrophily of molecule is increased, weakens the hydrogen bond between starch molecule；It forms sediment after another aspect acetylation
Powder particles structure is changed, and surface relief is uneven, cave or even crack occurs, hydrone is made to be easy to go deep into starch granules
Inside is absorbed by starch molecule.
The Brabender intrinsic viscosity values of 2 cassava ative starch of table and different acetyl content cassava acetate starch
5, influence of the different acetyl contents to cassava acetate starch freeze-thaw stability
Tapioca ester pastes the measurement of freeze-thaw stability：The starch of certain mass is weighed, 250ml deionized waters are added and are made into
The starch suspension of mass fraction 6% (butt), is placed in boiling water bath and is gelatinized 30min, be cooled to room temperature, then by gelatinized corn starch point
At 5 parts, pour into 5 plastic centrifuge tubes of known quality, weigh respectively, be put into -15 in refrigerator~-18 DEG C of freezings for 24 hours, take out
Naturally to thaw takes a pipe to centrifuge 20min at 3000r, discards supernatant liquid, weighs, remaining is freezed again, thaws, weighs, every time
Claim a pipe, finishes for five times to 5 pipes repeatedly.Its syneresis rate X (%) is calculated by formula 3：
In formula：X- syneresis rates, %；m1The quality of centrifuge tube, g；m2The gross mass of centrifuge tube and gelatinized corn starch, g；m3Freeze thawing
The quality sum of centrifuge tube and starch after water, g are removed in centrifugation.
Table 3 illustrates the freeze-thaw stability of tapioca and different acetyl content acetate starch.Tapioca is through filling
After dividing gelatinization, strand has the parallel ability for tending to form gel strands, hydrone to be extruded from gel.Freeze-thaw stability reflects
Be exactly performance that gelatinized corn starch keeps colloform texture after freezing and thawing repeatedly, the molecular structure of this and starch has prodigious pass
System, and the active force between starch molecule weakens with the extension of cooling time.Syneresis rate is the index for characterizing freeze-thaw stability,
The more big then freeze-thaw stability of syneresis rate is poorer.With the increase of acetic anhydride additive amount, the acetyl content of acetate starch and take
Dai Du is in increase trend, and the syneresis rate of gelatinized corn starch declines, and freeze-thaw stability improves.Tapioca passes through acetic anhydride esterification modification
Afterwards, the Hyarogen-bonding between starch molecule is reinforced, and the freeze-thaw stability of gelatinized corn starch makes moderate progress.
The freeze-thaw stability of table 3 log sweet potato starch and cassava acetate starch
- represent no elutriation and go out.
Cassava ative starch just has large quantity of moisture precipitation after a freeze thawing, becomes spongy.The acetyl of acetic anhydride is turned into
With the freeze-thaw stability for improving starch, raising and the being proportionate property of acetyl content of freeze-thaw stability.When adding for acetic anhydride
When dosage is more than 3%, preceding freeze-thaw stability effect three times is preferable, illustrates that acetyl content is obviously improved freeze-thaw stability.
The freeze-thaw stability of acetylation raising starch is mainly reflected in hydrophilic Acetyl Groups can keep moisture well, tie up
Hold good gelatinized corn starch state.Steric hindrance and molecule the repulsion effect of acetyl group reduce the hydrogen bond action of hydroxyl on starch, inhibit
The aggregation and retrogradation of starch.Compared with high substituted degree acetate starch after 5 freeze thawing, starch system is still more stable.
6, influence of the different acetyl contents to cassava acetate starch transparency
The measurement of gelatinized corn starch transparency：A certain amount of starch ester sample (butt) is weighed, the starch milk of 1% (w/w) is made into,
It sets and heats 1h in boiling water bath, completely after gelatinization, take out and be cooled to room temperature.Using distilled water as blank, spectrophotometric determination is used
Light transmittance of the gelatinized corn starch at 620nm wavelength.It is repeated three times, is averaged.The transparency of gelatinized corn starch is indicated with light transmittance.
Fig. 6 gives the transparency results of tapioca and different acetyl content acetate starch.It can from Fig. 6
Go out, with the increase of tapioca acetate degree of substitution, the transparency of gelatinized corn starch improves therewith.The heated abundant suction of starch granules
Water expands to form gelatinized corn starch, when gelatinized corn starch has light transmission, it may occur that transmission, reflection and the refraction of light.It influences in gelatinized corn starch
The factor of molecule and particle shape is mainly starch varieties and modification means, and the saturating of light is generated when light passes through gelatinized corn starch
The intensity penetrated, reflect and reflected is also different, and the transparency of gelatinized corn starch also has difference.The introduced acetyl group of esterification is hydrophilic
Group, acetyl group are incorporated into the form of covalent bond in tapioca, and group is negatively charged so that tapioca has certain
The property of polyelectrolyte.It is mutually exclusive between acetyl group, so that starch granules is easy to water swelling and gelatinization, gelatinized corn starch have compared with
High viscosity, transparency are also preferable.Acetyl group hinders the hydrogen bond association between starch molecule, reduce light refraction and
Reflected intensity, to improve transparency.Light transmittance reflects the size of starch and water binding ability to a certain extent.If
Starch is heated through water suction and is expanded completely, when there's almost no the pearl starch of unexpanded gelatinization in gelatinized corn starch, cannot be drawn
Light refraction is played, then the transparency of gelatinized corn starch is just very high.To make food that there is good color and luster and quality, in food processing
It is general to require starch that there is suitable transparency.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of preparation method of acetate starch, which is characterized in that include the following steps：
(1) it takes starch to add water mixing that starch emulsion is made, and lye is added and carries out basification；
(2) acetylating agent is added dropwise into the starch emulsion after basification, is esterified under 25-45 DEG C, pH alkaline conditions
Reaction；
(3) reaction solution is adjusted with acid solution to be neutralized, and reaction solution is separated by solid-liquid separation after reaction；
(4) take solid portion to be washed, be dried after separation of solid and liquid to get.
2. the preparation method of acetate starch according to claim 1, which is characterized in that in the step (1), control institute
The mass concentration for stating starch emulsion is 30-50wt%.
3. the preparation method of acetate starch according to claim 1 or 2, which is characterized in that in the step (1), institute
State the sodium hydroxide solution that lye is 2-4wt%.
4. according to the preparation method of claim 1-3 any one of them acetate starch, which is characterized in that the step (1)
In, the starch is tapioca.
5. according to the preparation method of claim 1-4 any one of them acetate starch, which is characterized in that the step (2)
In, the addition of the acetylating agent accounts for the 1-7wt% of the starch emulsion quality.
6. according to the preparation method of claim 1-5 any one of them acetate starch, which is characterized in that the step (2)
In, the acetylating agent is acetic anhydride.
7. according to the preparation method of claim 1-6 any one of them acetate starch, which is characterized in that the step (2)
In, further include the steps that the sodium hydroxide solution of 2-4wt% is added dropwise to control reaction solution pH7.5-10.0.
8. according to the preparation method of claim 1-7 any one of them acetate starch, which is characterized in that the step (2)
In, the reaction time of esterification is 1.0-3.0h.
9. according to the preparation method of claim 1-8 any one of them acetate starch, which is characterized in that the step (3)
In, the neutralization procedure is to adjust reaction solution pH6.0-6.5 with the hydrochloric acid solution of 0.4-0.6mol/L.
10. according to the preparation method of claim 1-9 any one of them acetate starch, which is characterized in that the step (4)
In, the drying steps are pneumatic conveying drying.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108935356A (en) * | 2018-08-17 | 2018-12-07 | 巢湖市翔宇渔具有限公司 | A kind of degradable bionical simulation attracting plug material |
| CN109569201A (en) * | 2018-11-27 | 2019-04-05 | 华南理工大学 | A kind of vinylacetate prepares the processing method of acetaldehyde byproduct in acetate starch production process |
| CN112369496A (en) * | 2020-10-20 | 2021-02-19 | 珠海市德海生物科技有限公司 | Modified fermented cassava starch and application thereof in aquatic feed |
| CN114680282A (en) * | 2020-12-31 | 2022-07-01 | 武汉大汉口食品有限公司 | Quick-frozen convenient soda water surface and production method thereof |
| CN115850777A (en) * | 2021-09-27 | 2023-03-28 | 广西民族大学 | Preparation and application of efficient hydrophobic acetylated starch nanoparticles |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903884A (en) * | 2005-07-28 | 2007-01-31 | 四平帝达变性淀粉有限公司 | Predextrinization acetate starch and its preparation method |
| CN103059148A (en) * | 2012-12-13 | 2013-04-24 | 玉林师范学院 | Method for preparing acetate starch with mechanical activation solid phase reaction |
| CN103254449A (en) * | 2012-12-25 | 2013-08-21 | 广西恒优淀粉有限责任公司 | Acetate starch preparation method |
-
2017
- 2017-12-26 CN CN201711434348.1A patent/CN108285497A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903884A (en) * | 2005-07-28 | 2007-01-31 | 四平帝达变性淀粉有限公司 | Predextrinization acetate starch and its preparation method |
| CN103059148A (en) * | 2012-12-13 | 2013-04-24 | 玉林师范学院 | Method for preparing acetate starch with mechanical activation solid phase reaction |
| CN103254449A (en) * | 2012-12-25 | 2013-08-21 | 广西恒优淀粉有限责任公司 | Acetate starch preparation method |
Non-Patent Citations (1)
| Title |
|---|
| 刘文娟等: "木薯醋酸酯淀粉的制备及性能研究", 《中国食品添加剂》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108935356A (en) * | 2018-08-17 | 2018-12-07 | 巢湖市翔宇渔具有限公司 | A kind of degradable bionical simulation attracting plug material |
| CN109569201A (en) * | 2018-11-27 | 2019-04-05 | 华南理工大学 | A kind of vinylacetate prepares the processing method of acetaldehyde byproduct in acetate starch production process |
| CN112369496A (en) * | 2020-10-20 | 2021-02-19 | 珠海市德海生物科技有限公司 | Modified fermented cassava starch and application thereof in aquatic feed |
| CN114680282A (en) * | 2020-12-31 | 2022-07-01 | 武汉大汉口食品有限公司 | Quick-frozen convenient soda water surface and production method thereof |
| CN115850777A (en) * | 2021-09-27 | 2023-03-28 | 广西民族大学 | Preparation and application of efficient hydrophobic acetylated starch nanoparticles |
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