CN107964050A - Preparation method of crosslinked starch - Google Patents
Preparation method of crosslinked starch Download PDFInfo
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
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Abstract
本发明提供一种交联淀粉的制备方法，将玉米淀粉按照预设的温度梯度进行梯度升温，在每个梯度温度各加入预定量的交联剂进行交联反应，得到交联淀粉。本发明通过设置温度梯度对原料进行逐步升温，加速分子间运动，有利于玉米淀粉中的淀粉分子与交联剂充分接触，加强交联反应，提高交联淀粉成品的粘结力，同时充分进行交联反应也能提高交联淀粉的稳定性。
The present invention provides a method for preparing cross-linked starch, wherein corn starch is gradually heated according to a preset temperature gradient, and a predetermined amount of a cross-linking agent is added at each gradient temperature to perform a cross-linking reaction to obtain the cross-linked starch. The present invention gradually heats the raw material by setting a temperature gradient to accelerate the intermolecular movement, which is conducive to the full contact between the starch molecules in the corn starch and the cross-linking agent, strengthens the cross-linking reaction, and improves the bonding force of the cross-linked starch product. At the same time, the full cross-linking reaction can also improve the stability of the cross-linked starch.
Description
Technical field
The present invention relates to technical field of modified starch, and in particular to a kind of preparation method of crosslinked starch.
Background technology
Converted starch is by either physically or chemically making starch molecular chain be cut off, reset or introducing other chemical groups
Obtained with changing its structure, the starch by denaturation has more excellent performance than ative starch.
The application of China's converted starch is quite varied, is applied to weaving, papermaking, food, feed, casting, medicine, builds
Build, during oil etc. is multi-field.For only from the species of converted starch, foreign countries, which have developed, has listed up to more than 2000 denaturation planted
Starch product, including oxidized starch, denaturated starch by acid, starch ester, starch ether, crosslinked starch, cationic starch, graft starch,
Cyclodextrin, white dextrin, starch,pregelatinized, dialdehyde starch etc..
Wherein, since the reaction control of crosslinked starch influences have high stability to heat, acid and shearing force, thus eating
Product, papermaking, medicine, weaving, building materials etc. all have important application.For example, crosslinked starch is added in Flour product production,
Dough water conservation can be made to play shortening rehydration time, surface tension is reduced, make dough bright and clean, the flexible phozy side of cutting, noodles are not
Frangibility.Include being used as thickener and stabilizer in catsup, jam, sauce in flavoring, stablize sauce, store for a long time
It is not stratified.Such as, on medical industry, crosslinked starch can be used as the antitack agent and lubricant of rubber to fork.It can serve as surgery hand
The lubricant of art rubber gloves.
Existing crosslinked starch preparation process is typically to add crosslinking agent under a certain temperature conditionss to carry out cross-linking reaction, instead
Should after obtain crosslinked starch.But the crosslinking degree of crosslinked starch finished product is not high as made from above-mentioned preparation process, do not reach pre-
The viscosity effect of phase.
The content of the invention
To solve the above problems, the application provides a kind of preparation method of crosslinked starch, which can improve friendship
Join the cohesive force and stability of starch, while the preparation method simple process and low cost.
The one of which embodiment of the application provides a kind of preparation method of crosslinked starch, by cornstarch according to default
Temperature gradient carry out gradient increased temperature, each gradient temperature respectively add scheduled volume crosslinking agent carry out cross-linking reaction, handed over
Join starch.
Further, 3 temperature gradients are at least preset.
Further, temperature gradient is respectively：30-32 DEG C, 40-42 DEG C and 50-52 DEG C.
Further, crosslinking agent is at least one of sodium trimetaphosphate, epoxychloropropane, phosphorus oxychloride.
Further, including in detail below step：
Prepare starch slurry：Cornstarch is added to the water, and forms starch slurry, and heating starch is starched to 30-32 DEG C；
First stage cross-linking reaction：Sodium hydroxide solution is added in starch slurry, its pH value is adjusted to after 11-11.2, adds
The crosslinking agent for entering scheduled volume carries out first stage cross-linking reaction；
Second stage cross-linking reaction：The mixed liquor that heating first stage cross-linking reaction obtains adds scheduled volume to 40-42 DEG C
Crosslinking agent carry out second stage cross-linking reaction；
Phase III cross-linking reaction：The mixed liquor that heating second stage cross-linking reaction obtains adds scheduled volume to 50-52 DEG C
Crosslinking agent carry out phase III cross-linking reaction；
Neutralisation treatment：Add in the product that hydrochloric acid is obtained to phase III cross-linking reaction, adjust its pH value to 6-6.2；
Wash drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, sieving, obtains
Crosslinked starch.
Further, in the step of first stage cross-linking reaction, the addition of crosslinking agent is the butt weight of cornstarch
0.5-1.5%.
Further, in the step of second stage cross-linking reaction, the addition of crosslinking agent is the butt weight of cornstarch
0.5-1.5%.
Further, in the step of phase III cross-linking reaction, the addition of crosslinking agent is the butt weight of cornstarch
0.5-1.5%.
Further, first stage cross-linking reaction is into the step of phase III cross-linking reaction, the addition phase of crosslinking agent
Deng.
Further, for first stage cross-linking reaction into the step of phase III cross-linking reaction, the reaction time is 5-7h.
According to the preparation method of above-described embodiment, employ and cornstarch is subjected to gradient liter according to default temperature gradient
Temperature, the crosslinking agent that scheduled volume is respectively added in each gradient temperature carry out cross-linking reaction, obtain the preparation process of crosslinked starch, pass through
Set temperature gradient progressively heats up raw material, is moved between acceleration molecular, is conducive to the starch molecule in cornstarch and friendship
Connection agent comes into full contact with, and strengthens cross-linking reaction, improves the cohesive force of crosslinked starch finished product, while fully progress cross-linking reaction can also carry
The stability of high crosslinked starch.
Brief description of the drawings
Fig. 1 is the method flow diagram of the preparation method of crosslinked starch in a kind of embodiment of the invention.
Embodiment
The present invention is described in further detail below by embodiment combination attached drawing.
Fig. 1 is referred to, in embodiments of the present invention, there is provided a kind of preparation method of crosslinked starch, its step include：
Step 1, prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, add 100-150 parts
In water, uniform starch slurry is dispersed with stirring into.Retort is moved into the water-bath with blender and starts to stir.Meanwhile
The temperature that water-bath is heated to starch slurry reaches 30-32 DEG C.
Step 2, first stage cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts starch slurry
PH value carry out first stage cross-linking reaction 5-7h to after 11-11.2, adding crosslinking agent.Crosslinking agent can be sodium trimetaphosphate,
At least one of epoxychloropropane, phosphorus oxychloride, can be used alone, also can compound two or three of use.Crosslinking agent adds
Enter the 0.5-1.5% for the butt weight that amount is cornstarch.Higher pH value can accelerate cross-linking reaction so that in cornstarch
Chemistry is formed between starch molecule to build bridge, and is added average molecular weight, is strengthened hydrogen bond action between starch molecule, strengthens the particle of starch
Structure, so as to suppress the swelling of starch, settlement volume diminishes.
Step 3, second stage cross-linking reaction：The mixed liquor that heating first stage cross-linking reaction obtains is added to 40-42 DEG C
The crosslinking agent of scheduled volume carries out second stage cross-linking reaction 5-7h.The addition of crosslinking agent is the butt weight of cornstarch
0.5-1.5%.Reaction temperature is high compared with the first stage at this time, accelerates intermolecular movement so that starch molecule and crosslinking agent
Collision probability rise, strengthen crosslinking degree.
Step 4, phase III cross-linking reaction：The mixed liquor that heating second stage cross-linking reaction obtains is added to 50-52 DEG C
The crosslinking agent of scheduled volume carries out phase III cross-linking reaction 5-7h.The addition of crosslinking agent is the butt weight of cornstarch
0.5-1.5%.In the reaction of the first to three stage crosslinked, crosslinking agent can be same crosslinking agent or different crosslinking agent,
The addition of crosslinking agent can be equal, can not also wait.In the cross-linking reaction of same stage, the addition of crosslinking agent can be
It is disposable to add, it can also be slowly added to while stirring during the reaction, so that crosslinking agent is fully reacted with starch molecule.By
After temperature rises to 55 DEG C starch gelatinization degree can aggravate, therefore the maximum temperature of cross-linking reaction is no more than 52 DEG C.
Step 5, neutralisation treatment：In the product that the hydrochloric acid of addition 10%wt is obtained to phase III cross-linking reaction, it is adjusted
PH value is to 6-6.2.
Step 6, washing drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100
Mesh sieve, obtains crosslinked starch.
Embodiment one
In the present embodiment, the preparation method of crosslinked starch is as follows：
Step 1, prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, add 100 parts of water
In, it is dispersed with stirring into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile will
The temperature that water-bath is heated to starch slurry reaches 30 DEG C.
Step 2, first stage cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts starch slurry
0.5% sodium trimetaphosphate of pH value to the butt weight for after 11, being incorporated as cornstarch carry out first stage cross-linking reaction
5h。
Step 3, second stage cross-linking reaction：The mixed liquor that heating first stage cross-linking reaction obtains is incorporated as to 40 DEG C
0.5% sodium trimetaphosphate of the butt weight of cornstarch carries out second stage cross-linking reaction 5h.
Step 4, phase III cross-linking reaction：The mixed liquor that heating second stage cross-linking reaction obtains is incorporated as to 50 DEG C
0.5% sodium trimetaphosphate of the butt weight of cornstarch carries out phase III cross-linking reaction 5h.
Step 5, neutralisation treatment：In the product that the hydrochloric acid of addition 10%wt is obtained to phase III cross-linking reaction, it is adjusted
PH value is to 6.
Step 6, washing drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100
Mesh sieve, obtains crosslinked starch.
Embodiment two
In the present embodiment, the preparation method of crosslinked starch is as follows：
Step 1, prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, add 120 parts of water
In, it is dispersed with stirring into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile will
The temperature that water-bath is heated to starch slurry reaches 31 DEG C.
Step 2, first stage cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts starch slurry
1% sodium trimetaphosphate of pH value to the butt weight for after 11.1, being incorporated as cornstarch carry out first stage cross-linking reaction
6h。
Step 3, second stage cross-linking reaction：The mixed liquor that heating first stage cross-linking reaction obtains is incorporated as to 41 DEG C
1% sodium trimetaphosphate of the butt weight of cornstarch carries out second stage cross-linking reaction 6h.
Step 4, phase III cross-linking reaction：The mixed liquor that heating second stage cross-linking reaction obtains is incorporated as to 51 DEG C
1% sodium trimetaphosphate of the butt weight of cornstarch carries out phase III cross-linking reaction 6h.
Step 5, neutralisation treatment：In the product that the hydrochloric acid of addition 10%wt is obtained to phase III cross-linking reaction, it is adjusted
PH value is to 6.1.
Step 6, washing drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100
Mesh sieve, obtains crosslinked starch.
Embodiment three
In the present embodiment, the preparation method of crosslinked starch is as follows：
Step 1, prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, add 150 parts of water
In, it is dispersed with stirring into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile will
The temperature that water-bath is heated to starch slurry reaches 32 DEG C.
Step 2, first stage cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts starch slurry
1.5% sodium trimetaphosphate of pH value to the butt weight for after 11.2, being incorporated as cornstarch to carry out first stage crosslinking anti-
Answer 7h.
Step 3, second stage cross-linking reaction：The mixed liquor that heating first stage cross-linking reaction obtains is incorporated as to 42 DEG C
1.5% sodium trimetaphosphate of the butt weight of cornstarch carries out second stage cross-linking reaction 7h.
Step 4, phase III cross-linking reaction：The mixed liquor that heating second stage cross-linking reaction obtains is incorporated as to 52 DEG C
1.5% sodium trimetaphosphate of the butt weight of cornstarch carries out phase III cross-linking reaction 7h.
Step 5, neutralisation treatment：In the product that the hydrochloric acid of addition 10%wt is obtained to phase III cross-linking reaction, it is adjusted
PH value is to 6.2.
Step 6, washing drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100
Mesh sieve, obtains crosslinked starch.
Comparative example one
In this comparative example, the preparation method of crosslinked starch is as follows：
Prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, are added in 100 parts of water, stirring
It is dispersed into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile by water-bath plus
The temperature of heat to starch slurry reaches 30 DEG C.
Cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts the pH value of starch slurry to after 11,
0.5% sodium trimetaphosphate for being incorporated as the butt weight of cornstarch carries out first stage cross-linking reaction 15h.
Neutralisation treatment：In the product that hydrochloric acid to the cross-linking reaction of addition 10%wt obtains, its pH value is adjusted to 6.
Wash drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100 mesh sieve mistakes
Sieve, obtains crosslinked starch.
Comparative example two
In this comparative example, the preparation method of crosslinked starch is as follows：
Prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, are added in 120 parts of water, stirring
It is dispersed into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile by water-bath plus
The temperature of heat to starch slurry reaches 40 DEG C.
Cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts the pH value of starch slurry to after 11,
1% sodium trimetaphosphate for being incorporated as the butt weight of cornstarch carries out first stage cross-linking reaction 18h.
Neutralisation treatment：In the product that hydrochloric acid to the cross-linking reaction of addition 10%wt obtains, its pH value is adjusted to 6.1.
Wash drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100 mesh sieve mistakes
Sieve, obtains crosslinked starch.
Comparative example three
In this comparative example, the preparation method of crosslinked starch is as follows：
Prepare starch slurry：By weight, 100 parts of cornstarch are weighed to be fitted into retort, are added in 150 parts of water, stirring
It is dispersed into uniform starch slurry.Retort is moved into the water-bath with blender and starts to stir.Meanwhile by water-bath plus
The temperature of heat to starch slurry reaches 50 DEG C.
Cross-linking reaction：The sodium hydroxide solution of 2.5%wt is added in starch slurry, adjusts the pH value of starch slurry to after 11,
0.5% sodium trimetaphosphate for being incorporated as the butt weight of cornstarch carries out first stage cross-linking reaction 21h.
Neutralisation treatment：In the product that hydrochloric acid to the cross-linking reaction of addition 10%wt obtains, its pH value is adjusted to 6.2.
Wash drying：The product obtained successively to neutralisation treatment filters, distills water washing, drying, crushing, 100 mesh sieve mistakes
Sieve, obtains crosslinked starch.
The converted starch number consecutively that embodiment one to three and comparative example one to three are obtained is 1-6, carries out settlement volume survey
Examination and freeze-thaw stability test.
Settlement volume is tested：
There are linear relationship, linearly related degree to reach R with swellbility for the starch degree of cross linking2=0.898, swellbility is smaller, table
Show that the degree of cross linking is higher.By measuring settlement volume come the secondary indication starch degree of cross linking.
Following operate is carried out respectively to 6 parts of samples：0.5g absolute dried samples accurately are weighed in 100ml beakers, are made into 2%
Starch solution.Beaker is placed in 82-85 DEG C of water-bath, is slightly stirred, keeps the temperature 2min, taking-up is cooled to room temperature.With two scales
Centrifuge tube pours into 10ml paste liquid respectively, and 2min is centrifuged under 4000r/min rotating speeds, centrifuge tube is taken out, supernatant is poured into another 1
In the centrifuge tube of same volume, settling volume is calculated.
Settlement volume (ml)=10-V, V is the volume of clear liquid.
1 settlement volume test result of table
| Numbering | 1 | 2 | 3 | 4 | 5 | 6 |
| Settlement volume (ml) | 1.7 | 1.2 | 1.4 | 2.5 | 2.2 | 2.6 |
As can be known from the above table, the settlement volume for the crosslinked starch that the preparation method of embodiment obtains has been used compared with comparative example preparation side
The settlement volume for the converted starch that method obtains is small, indicate the crosslinking degree of the crosslinked starch that the preparation method of embodiment obtains compared with
Height, better quality.It is certain to illustrate that the method for set temperature gradient has the crosslinking degree for strengthening crosslinked starch finished product at the same time
Effect.
Freeze-thaw stability is tested：Following operate is carried out respectively to 6 parts of samples：A certain amount of sample is weighed, is made into 5% (w/
W, in terms of butt) solution, after being heated to 95 DEG C, keep the temperature 15min, be cooled to room temperature, obtain pasty liquid.
Weigh 50mL centrifuge tube quality (m1), take 20g pasty liquids to pour into centrifuge tube, weigh quality (m2).Centrifuge tube is put
Enter in -10~-20 DEG C of refrigerator, taken out after freezing diel, naturally to thaw, as a Frozen-thawed cycled.
After 5 Frozen-thawed cycleds, 20min is centrifuged under the conditions of 6000/min, abandoning supernatant, weighs sediment quality
(m3), calculate syneresis rate.
Syneresis rate (%)=(m3-m1)/(m2-m1) × 100%
2 freeze-thaw cycle test result of table
As can be seen from Table 2, crosslinked starch made from embodiment one to three, its syneresis rate is than made from comparative example one to three
The syneresis rate of crosslinked starch is small, illustrate the present invention preparation method as a result of temperature gradient method to cornstarch into
Row order section cross-linking reaction, can be effectively reduced the syneresis rate of converted starch finished product, reduce the rupture that starch coagulates limb structure.Through
The crosslinked starch finished product crossed after 5 freeze thawing still keeps relatively low syneresis rate, illustrates that its freeze-thaw stability is higher.
Use above specific case is illustrated the present invention, is only intended to help and understands the present invention, not limiting
The system present invention.For those skilled in the art, according to the thought of the present invention, can also make some simple
Deduce, deform or replace.
Claims (10)
1. a kind of preparation method of crosslinked starch, it is characterised in that cornstarch is subjected to gradient according to default temperature gradient
Heating, the crosslinking agent that scheduled volume is respectively added in each gradient temperature carry out cross-linking reaction, obtain crosslinked starch.
2. the preparation method of crosslinked starch according to claim 1, it is characterised in that at least default 3 temperature ladders
Degree.
3. the preparation method of crosslinked starch according to claim 2, it is characterised in that the temperature gradient is respectively：30-
32 DEG C, 40-42 DEG C and 50-52 DEG C.
4. the preparation method of crosslinked starch according to claim 1, it is characterised in that the crosslinking agent is three metaphosphoric acids
At least one of sodium, epoxychloropropane, phosphorus oxychloride.
5. the preparation method of the crosslinked starch according to any one of claim 1-4, it is characterised in that including in detail below
Step：
Prepare starch slurry：Cornstarch is added to the water, and forms starch slurry, and heating starch is starched to 30-32 DEG C；
First stage cross-linking reaction：Sodium hydroxide solution is added in the starch slurry, its pH value is adjusted to after 11-11.2, adds
The crosslinking agent for entering scheduled volume carries out first stage cross-linking reaction；
Second stage cross-linking reaction：Mixed liquor that the first stage cross-linking reaction obtains is heated to 40-42 DEG C, adds scheduled volume
Crosslinking agent carry out second stage cross-linking reaction；
Phase III cross-linking reaction：Mixed liquor that the second stage cross-linking reaction obtains is heated to 50-52 DEG C, adds scheduled volume
Crosslinking agent carry out phase III cross-linking reaction；
Neutralisation treatment：Add in the product that hydrochloric acid is obtained to the phase III cross-linking reaction, adjust its pH value to 6-6.2；
Wash drying：The product obtained successively to the neutralisation treatment filters, distills water washing, drying, crushing, sieving, obtains
Crosslinked starch.
6. the preparation method of crosslinked starch according to claim 5, it is characterised in that the first stage cross-linking reaction
In step, the addition of the crosslinking agent is the 0.5-1.5% of the butt weight of the cornstarch.
7. the preparation method of crosslinked starch according to claim 5, it is characterised in that the second stage cross-linking reaction
In step, the addition of the crosslinking agent is the 0.5-1.5% of the butt weight of the cornstarch.
8. the preparation method of crosslinked starch according to claim 5, it is characterised in that the phase III cross-linking reaction
In step, the addition of the crosslinking agent is the 0.5-1.5% of the butt weight of the cornstarch.
9. the preparation method of crosslinked starch according to claim 5, it is characterised in that the first stage cross-linking reaction is extremely
In the step of phase III cross-linking reaction, the addition of the crosslinking agent is equal.
10. the preparation method of crosslinked starch according to claim 5, it is characterised in that the first stage cross-linking reaction
Into the step of phase III cross-linking reaction, the reaction time is 5-7h.
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| CN110903406A (en) * | 2019-12-22 | 2020-03-24 | 南通通地生物技术有限公司 | Method for preparing oxidized corn starch paste by using composite oxidant |
| CN111793222A (en) * | 2020-08-12 | 2020-10-20 | 东莞建泰生物科技有限公司 | Reverse control method for starch-sodium trimetaphosphate crosslinking and application thereof |
| CN115043950A (en) * | 2022-06-27 | 2022-09-13 | 上海交通大学 | POCl 3 Preparation method of cross-linked starch |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110903406A (en) * | 2019-12-22 | 2020-03-24 | 南通通地生物技术有限公司 | Method for preparing oxidized corn starch paste by using composite oxidant |
| CN111793222A (en) * | 2020-08-12 | 2020-10-20 | 东莞建泰生物科技有限公司 | Reverse control method for starch-sodium trimetaphosphate crosslinking and application thereof |
| CN115043950A (en) * | 2022-06-27 | 2022-09-13 | 上海交通大学 | POCl 3 Preparation method of cross-linked starch |
| CN115043950B (en) * | 2022-06-27 | 2023-12-26 | 上海交通大学 | POCl (point of care testing) 3 Preparation method of crosslinked starch |
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