CN110054703A - A kind of preparation method of enzyme modification pre-gel hydroxypropyl starch - Google Patents
A kind of preparation method of enzyme modification pre-gel hydroxypropyl starch Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of enzyme modification pre-gel hydroxypropyl starch, are related to modified starch technical field.Technical solution disclosed by the invention is to be pre-processed as catalyst to starch using biological enzyme (amylase), makes the etherification reaction of starch and propylene oxide be easier to carry out, improves the degree of substitution of hydroxypropyl, enzymic catalytic reaction is environmentally protective.Use a small amount of pure water as solvent, propylene oxide is added under alkaline condition and is reacted for starch after enzymatic, it is to obtain hydroxypropul starch after being washed to product, being dry, it is not necessary that other solvents are additionally added, it can be realized under condition of normal pressure, it is easy to operate, low for equipment requirements, production cost is low；Directly being dried after hydroxypropul starch and a small amount of glue can be obtained pre-gel hydroxypropyl starch solid, and step is simple, production efficiency is greatly improved, it is easy to accomplish industrialized production.
Description
Technical field
The present invention relates to technical field of starch modification more particularly to a kind of preparation sides of enzyme modification pre-gel hydroxypropyl starch
Method.
Background technique
Hydroxypropul starch is very widely used a kind of converted starch.A certain number of hydroxypropyls are introduced to starch molecule
On, it can make the property of gelatinized corn starch that effective improve occur.On the one hand hydroxypropyl can generate space steric effect, prevent starch chain
Aggregation and crystallization；On the other hand, the hydrophilicity of hydroxypropyl weakens the inside HYDROGEN BOND INTENSITY of starch granules structure, makes it easier to
Expansion and gelatinization, gained gelatinized corn starch transparency is high, mobility is strong, retrogradation is weak, stability is high, freeze-thaw stability is good.
Pregelatinized starch is called pre-gelatinized starch, its compressibility, good fluidity compared with common starch, therefore being called can
Pressure property starch.
Pre-gel hydroxypropyl starch are a kind of composite modified starch, combine the excellent of pregelatinized starch and hydroxypropul starch
Point had not only had the characteristics that compressibility was good, good fluidity, but also had that gelatinized corn starch transparency is high, mobility is strong, retrogradation is weak, stablizes
Property high, advantage that freeze-thaw stability is good.
The patent of 108203470 A of Publication No. CN discloses a kind of preparation method of pre-gel hydroxypropyl starch, however
This method uses tetramethylammonium hydroxide as catalyst, and tetramethylammonium hydroxide is highly basic, has strong corrosive, misoperation
Safety accident easily occurs；Product is handled using the mode of alcohol precipitation and freeze-drying, production cost is big, production efficiency is low；And due to
It is very big that hydroxypropul starch is dissolved in a small amount of hot water medium viscosity, is difficult to carry out spray drying treatment, therefore be industrially difficult to realize.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of easy to operate, production safety, it is at low cost, be easily achieved work
The preparation method for the enzyme modification pre-gel hydroxypropyl starch that industry metaplasia produces.
To solve the above-mentioned problems, the present invention proposes following technical scheme:
A kind of preparation method of enzyme modification pre-gel hydroxypropyl starch, comprising the following steps:
A. 1 weight starch is dissolved in 1-3 parts by weight of purified water, amylase is added and carries out enzyme reaction, reaction temperature is
20-100 DEG C, the additional amount of the amylase is 1~10000u/g dry weight of starch；
B. after the completion of enzyme reaction, pH to 9-11 is adjusted, the propylene oxide of 0.01-0.2 parts by weight is added, in 10-45 DEG C, height
It is reacted under purity nitrogen protection；
C. after reaction, product washed, dried, obtain hydroxypropul starch；
D. hydroxypropul starch is dissolved in the pure water of 0.2-2 times of quality and forms aqueous paste, pre- glue is drying to obtain after gelatinization
Change hydroxypropul starch solid.
Further technical solution is for it, and the amylase is alpha amylase, beta amylase, glucose saccharogenic amylase, Propiram
Enzyme, glucose oxidase, glucose sugar isomerase, cyclodextrin glycosyl transferases, Q-enzyrne, glucose sugar turn in glycosides enzyme at least
It is a kind of.
Further technical solution is for it, in the step c, before washing to product, further includes: adjust product
PH to 6-8.
Further technical solution is for it, and dry mode is that vacuum drying, spray drying or air-flow are dry after the gelatinization
It is dry.
Further technical solution is for it, and the pure water temperature in the step d is 0-60 DEG C.
Further technical solution is for it, and the mode of washing of the step c is centrifuge washing or filtration washing.
Further technical solution is for it, and the drying mode of the step c is pneumatic conveying drying.
Further technical solution is for it, and the reaction time of the enzyme reaction is 0.5-24 hours.
Further technical solution is for it, and the starch is food-grade starches.
Further technical solution is for it, and the starch is food-grade corn starch, food-grade tapioca, food-grade horse
At least one of bell sweet potato starch.
Compared with prior art, the accessible technical effect of the present invention includes:
Starch is pre-processed as catalyst using biological enzyme (amylase), keeps the etherificate of starch and propylene oxide anti-
It should be easier to carry out, improve the degree of substitution of hydroxypropyl, enzymic catalytic reaction is environmentally protective.Use a small amount of pure water as solvent, warp
Propylene oxide is added under alkaline condition and is reacted for starch after crossing enzymatic, is to obtain hydroxypropyl after washing to product, being dry
Base starch can be realized, easy to operate, low for equipment requirements, production cost it is not necessary that other solvents are additionally added under condition of normal pressure
It is low；Directly being dried after hydroxypropul starch and a small amount of glue can be obtained pre-gel hydroxypropyl starch solid, step is simple,
Production efficiency is greatly improved, it is easy to accomplish industrialized production.
Specific embodiment
The technical solution in embodiment will be clearly and completely described below.
It should be appreciated that ought use in this specification and in the appended claims, term " includes " and "comprising" instruction
Described feature, entirety, step, operation, the presence of element and/or component, but one or more of the other feature, whole is not precluded
Body, step, operation, the presence or addition of element, component and/or its set.
It is also understood that in this embodiment of the present invention term used in the description merely for the sake of description particular implementation
Example purpose and be not intended to limit the embodiment of the present invention.Such as the institute in specification and appended book of the embodiment of the present invention
As use, other situations unless the context is clearly specified, otherwise " one " of singular, "one" and "the" are intended to wrap
Include plural form.
The embodiment of the present invention provides a kind of preparation method of enzyme modification pre-gel hydroxypropyl starch, comprising the following steps:
A. 1 weight starch is dissolved in 1-3 parts by weight of purified water, amylase is added and carries out enzyme reaction, reaction temperature is
20-100 DEG C, the reaction time is 0.5-24 hours, and the additional amount of the amylase is 1~10000u/g dry weight of starch；
B. it after the completion of enzyme reaction, adjusts pH to 9-11 and carries out destroy the enzyme treatment, the propylene oxide of 0.01-0.2 parts by weight is added,
It is slowly stirred, is reacted under 10-45 DEG C, High Purity Nitrogen protection, reaction time 8-48h；
C. after reaction, the pH to 6-8 of product is adjusted, washing, drying obtain hydroxypropul starch；
D. hydroxypropul starch is dissolved in the 0-60 DEG C of pure water of 0.2-2 times of quality and forms aqueous paste, after gelatinization drying be
Pre-gel hydroxypropyl starch solid is obtained, pre-gel hydroxypropyl starch solid is crushed to predetermined size range.
In certain embodiments, the amylase is alpha amylase, beta amylase, glucose saccharogenic amylase, Pullulanase, glucose
Carbohydrate oxidase, glucose sugar isomerase, cyclodextrin glycosyl transferases, Q-enzyrne, glucose sugar turn at least one of glycosides enzyme.
For example, in one embodiment, the amylase is alpha amylase.
In one embodiment, the amylase is the mixture of alpha amylase, beta amylase.
In one embodiment, the amylase is that glucose saccharogenic amylase, Pullulanase, glucose oxidase, glucose sugar are different
The mixture of structure enzyme.
In one embodiment, the amylase is cyclodextrin glycosyl transferases, Q-enzyrne, glucose sugar turn the mixed of glycosides enzyme
Close object.
In one embodiment, the mode of washing of the step c is centrifuge washing.
In one embodiment, the mode of washing of the step c is filtration washing.
In one embodiment, the drying mode of the step c is pneumatic conveying drying.
In certain embodiments, mode dry after the gelatinization of step d is that aqueous paste is kept 10- in 75-100 DEG C
Pneumatic conveying drying is directly carried out after 60min.
For example, in one embodiment, directly carrying out pneumatic conveying drying after aqueous paste is kept 60min in 75 DEG C.
In one embodiment, pneumatic conveying drying is directly carried out after aqueous paste being kept 10min in 100 DEG C.
In one embodiment, pneumatic conveying drying is directly carried out after aqueous paste being kept 40min in 85 DEG C.
In one embodiment, pneumatic conveying drying is directly carried out after aqueous paste being kept 20min in 95 DEG C.
In one embodiment, mode dry after the gelatinization of step d is that extrusion dehydration drying is carried out to aqueous paste.Specifically
Extrusion dehydration mode is to be squeezed using extruder.
For example, in one embodiment, aqueous paste being placed in screw extruder after squeezing out and carrying out pneumatic conveying drying.
In one embodiment, mode dry after the gelatinization of step d is directly to be spray-dried.
In one embodiment, mode dry after the gelatinization of step d is directly to be dried in vacuo.
In certain embodiments, used starch is food-grade starches.
In certain embodiments, used starch is food-grade corn starch, food-grade tapioca, food-grade Ma Ling
At least one of sweet potato starch.
Cornstarch, tapioca or the potato starch of food-grade.With odorlessness, tasteless, paste is limpid, viscosity
Many advantages, such as height, freeze-thaw stability is high, has in industries such as food, drug, chemical industry, papermaking and weavings and widely answers
With.
For example, in one embodiment, used starch is the mixing of food-grade corn starch, food-grade tapioca
Object.
In one embodiment, used starch is food-grade corn starch.
In one embodiment, used starch is food-grade corn starch, food-grade tapioca, food-grade potato
The mixture of starch.
The embodiment of the present invention pre-processes starch as catalyst using biological enzyme (amylase), makes starch and epoxy
The etherification reaction of propane is easier to carry out, and improves the degree of substitution of hydroxypropyl, and enzymic catalytic reaction is environmentally protective.Use a small amount of pure water
As solvent, propylene oxide is added under alkaline condition and is reacted, is to obtain hydroxypropul starch after being washed to product, being dry,
It is not necessary that other solvents are additionally added, can be realized under condition of normal pressure, it is easy to operate, low for equipment requirements, production cost is low；Hydroxypropyl
Directly being dried after base starch and a small amount of hot water gelatinization can be obtained pre-gel hydroxypropyl starch solid, and step is simple, produces
Efficiency is greatly improved, it is easy to accomplish industrialized production.
Specific embodiment 1
It weighs food-grade corn starch 100kg to be placed in stainless steel reactor, 200kg pure water is added, alpha amylase is added
100000 u, 55 DEG C of reaction 10h are slowly stirred uniformly with sodium hydroxide solution tune pH to 11,10kg propylene oxide are added, is then existed
Under the protection of High Purity Nitrogen, 43 DEG C are reacted 20 hours；After reaction with salt acid for adjusting pH value to 7, through centrifuge washing, pneumatic conveying drying
Hydroxypropul starch 97kg is made；Hydroxypropul starch is dissolved in 60 DEG C of 100kg of hot water and stirs evenly to form aqueous paste, through spiral shell
Bar extruder squeezes out, pneumatic conveying drying pre-paying hydroxypropul starch solid 96.5kg to obtain the final product, is finally crushed to required particle size range i.e.
It can.
The propoxyl mass content of the present embodiment pre-gel hydroxypropyl starch is 6.5% (hydroxypropoxy content measurement side
Method is referring to 2015 editions 0,712 first methods of " Chinese Pharmacopoeia " general rule).
Specific embodiment 2
1 parts by weight food-grade tapioca and 1 parts by weight pure water are added to the container, alpha amylase and beta amylase is added
Total 5000u/g dry weight of starch, with sodium hydroxide solution tune pH to 9, is slowly stirred uniformly after 99 DEG C of reaction 1h, is added 0.2 times
The propylene oxide of quality, then under the protection of High Purity Nitrogen, 10 DEG C are reacted 48 hours；After reaction extremely with salt acid for adjusting pH value
6.8, hydroxypropul starch is made through filtration washing, pneumatic conveying drying；Hydroxypropul starch is dissolved in the pure water of 45 DEG C of 2 times of quality and being stirred
It is formed uniformly aqueous paste, is squeezed out through screw extruder, pneumatic conveying drying pre-paying hydroxypropul starch solid to obtain the final product, is finally crushed to institute
Need particle size range.
Specific embodiment 3
1 parts by weight food-grade tapioca and 3 parts by weight pure water are added to the container, glucoamylase, Portugal is added
Grape carbohydrate oxidase and the total 10u/g dry weight of starch of beta amylase, with sodium hydroxide solution tune pH to 10, delay after 60 DEG C of reactions for 24 hours
Slowly it stirs evenly, the propylene oxide of 0.01 times of quality is added, then under the protection of High Purity Nitrogen, 20 DEG C are reacted 36 hours；Reaction
After with salt acid for adjusting pH value to 7.2, hydroxypropul starch is made through filtration washing, pneumatic conveying drying；Hydroxypropul starch is dissolved in 1
Stir evenly to form aqueous paste in times 20 DEG C of quality of pure water, to aqueous paste directly using the mode of spray drying it is dry after to obtain the final product
Pre-gel hydroxypropyl starch solid is finally crushed to required particle size range.
Specific embodiment 4
1.5 parts by weight food-grade corn starch and 3 parts by weight pure water are added to the container, cyclodextrin glycosyl transfer is added
Enzyme, Q-enzyrne and glucose sugar turn the total 1000u/g dry weight of starch of glycosides enzyme, after 40 DEG C of reaction 14h, with sodium hydroxide solution tune
PH to 10 is slowly stirred uniformly, the propylene oxide of 0.15 times of quality is added, then under the protection of High Purity Nitrogen, 30 DEG C of reactions 28
Hour；After reaction with salt acid for adjusting pH value to 7.5, hydroxypropul starch is made through filtration washing, pneumatic conveying drying；By hydroxypropyl
Starch, which is dissolved in the pure water of 10 DEG C of 1.6 times of quality, to stir evenly to form aqueous paste, squeezes out, is dried in vacuo through screw extruder to obtain the final product
Pre-gel hydroxypropyl starch solid is finally crushed to required particle size range.
Specific embodiment 5
1.5 parts by weight food-grade corn starch, 1.5 parts by weight food-grade tapiocas and 4 parts by weight pure water are added
In container, Q-enzyrne is added and glucose sugar turns the total 8000u/g dry weight of starch of glycosides enzyme, after 90 DEG C of reaction 3h, uses hydroxide
Sodium solution tune pH to 10 is slowly stirred uniformly, the propylene oxide of 0.18 times of quality is added, then under the protection of High Purity Nitrogen, 38
DEG C reaction 25 hours；After reaction with salt acid for adjusting pH value to 7.1, hydroxypropul starch is made through filtration washing, pneumatic conveying drying；
Hydroxypropul starch is dissolved in the pure water of 0 DEG C of 1.1 times of quality and stirs evenly to form aqueous paste, squeezed out through screw extruder, vacuum
It is drying to obtain pre-gel hydroxypropyl starch solid, is finally crushed to required particle size range.
In the above-described embodiments, it all emphasizes particularly on different fields to the description of each embodiment, is not described in some embodiment
Part, reference can be made to the related descriptions of other embodiments.
The above is a specific embodiment of the invention, but scope of protection of the present invention is not limited thereto, any ripe
It knows those skilled in the art in the technical scope disclosed by the present invention, various equivalent modifications can be readily occurred in or replaces
It changes, these modifications or substitutions should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with right
It is required that protection scope subject to.
Claims (10)
1. a kind of preparation method of enzyme modification pre-gel hydroxypropyl starch, which comprises the following steps:
A. 1 weight starch is dissolved in 1-3 parts by weight of purified water, amylase is added and carries out enzyme reaction, reaction temperature 20-
100 DEG C, the additional amount of the amylase is 1~10000u/g dry weight of starch；
B. after the completion of enzyme reaction, pH to 9-11 is adjusted, the propylene oxide of 0.01-0.2 parts by weight is added, in 10-45 DEG C, High Purity Nitrogen
It is reacted under protection；
C. after reaction, product washed, dried, obtain hydroxypropul starch；
D. hydroxypropul starch is dissolved in the pure water of 0.2-2 times of quality and forms aqueous paste, formed aqueous paste, after gelatinization drying be
Obtain pre-gel hydroxypropyl starch solid.
2. the preparation method of enzyme modification pre-gel hydroxypropyl starch as described in claim 1, which is characterized in that the amylase
For alpha amylase, beta amylase, glucose saccharogenic amylase, Pullulanase, glucose oxidase, glucose sugar isomerase, cyclodextrin glycosyl
Transferase, Q-enzyrne, glucose sugar turn at least one of glycosides enzyme.
3. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 2, which is characterized in that in the step c, to production
Before object is washed, further includes: adjust the pH to 6-8 of product.
4. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 3, which is characterized in that drying after the gelatinization
Mode is vacuum drying, spray drying or pneumatic conveying drying.
5. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 4, which is characterized in that pure in the step d
Coolant-temperature gage is 0-60 DEG C.
6. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 5, which is characterized in that the washing of the step c
Mode is centrifuge washing or filtration washing.
7. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 6, which is characterized in that the drying of the step c
Mode is pneumatic conveying drying.
8. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 7, which is characterized in that the reaction of the enzyme reaction
Time is 0.5-24 hours.
9. such as the preparation method of the described in any item pre-gel hydroxypropyl starch of claim 1-8, which is characterized in that the starch
For food-grade starches.
10. the preparation method of pre-gel hydroxypropyl starch as claimed in claim 9, which is characterized in that the food-grade starches
For at least one of food-grade corn starch, food-grade tapioca, food-grade potato starch.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111518224A (en) * | 2020-06-16 | 2020-08-11 | 佛山市国农淀粉有限公司 | Preparation method of hydroxypropyl distarch phosphate for reducing chloropropanol byproduct content |
| CN112142865A (en) * | 2020-09-15 | 2020-12-29 | 湖州展望药业有限公司 | Modified pregelatinized starch and production method thereof |
| CN114395055A (en) * | 2022-01-28 | 2022-04-26 | 江苏思颖柏霖生物科技有限公司 | Production and processing technology for hydroxypropyl starch |
| CN116199943A (en) * | 2023-04-11 | 2023-06-02 | 东莞东美食品有限公司 | Modified hydroxypropyl starch for capsules |
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| CN111518224A (en) * | 2020-06-16 | 2020-08-11 | 佛山市国农淀粉有限公司 | Preparation method of hydroxypropyl distarch phosphate for reducing chloropropanol byproduct content |
| CN112142865A (en) * | 2020-09-15 | 2020-12-29 | 湖州展望药业有限公司 | Modified pregelatinized starch and production method thereof |
| CN114395055A (en) * | 2022-01-28 | 2022-04-26 | 江苏思颖柏霖生物科技有限公司 | Production and processing technology for hydroxypropyl starch |
| CN116199943A (en) * | 2023-04-11 | 2023-06-02 | 东莞东美食品有限公司 | Modified hydroxypropyl starch for capsules |
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