CN109824789A - A method of preparing dialdehyde starch in homogeneous system - Google Patents
A method of preparing dialdehyde starch in homogeneous system Download PDFInfo
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- CN109824789A CN109824789A CN201910177466.1A CN201910177466A CN109824789A CN 109824789 A CN109824789 A CN 109824789A CN 201910177466 A CN201910177466 A CN 201910177466A CN 109824789 A CN109824789 A CN 109824789A
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- starch
- dialdehyde
- dialdehyde starch
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Abstract
The method that the present invention provides a kind of to prepare dialdehyde starch in homogeneous system, provided method are made from starch, and first making starch, Heat Gelatinization forms homogeneous system in water, are then reacted again with oxidant periodic acid and are prepared dialdehyde starch.Reaction condition is mild, reaction rate is high, occurs without side reaction；Prepared product oxidizability is uniform, and properties of product are excellent.
Description
Technical field
The method that the present invention relates to a kind of to prepare dialdehyde starch in homogeneous system.
Background technique
There is excellent materialization, biochemical property due to dialdehyde starch is with many active aldehyde groups.Currently, dialdehyde forms sediment
Powder is widely used to the industries such as papermaking, weaving, leather, medicine.The production method of traditional dialdehyde starch is heterogeneous system oxygen
Change method, it is by the starch direct oxidation without dissolution process, and using dialdehyde starch prepared by this method, there is oxidizabilities
Inhomogenous, the disadvantages of reaction rate is low, product poorly water-soluble.
How to improve the reaction generating rate of dialdehyde starch, make oxidizability uniform, and then improves the quality of dialdehyde starch,
It is a problem to be solved.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of methods for preparing dialdehyde starch, can be mentioned using the synthetic method
The reaction generating rate of high dialdehyde starch, dialdehyde starch oxidizability obtained are uniform.
In order to solve the above technical problems, the present invention provides a kind of method that dialdehyde starch is prepared in homogeneous system, including
Following steps:
(1) it mixes: under stirring, 6-7 weight starch being added into 100 parts by weight deionized waters, forms starch
Cream；
(2) it is gelatinized: being 1.2-1.5 × 10 by pressure5The vapor of Pa is passed through in starch milk prepared by step (1), to
Stop being passed through steam after keeping temperature 10-15min when starch milk temperature reaches 72-78 DEG C, is cooled to 38-40 DEG C, obtains gelatinized corn starch；
(3) it aoxidizes: under stirring, hydrochloric acid being added into gelatinized corn starch prepared by step (2), adjusts gelatinized corn starch solution
PH value is to 0.8-1.2；Temperature is controlled under the conditions of 38-40 DEG C, then periodic acid is added into gelatinized corn starch, periodic acid and starch rub
You react 3-3.5h, obtain dialdehyde starch mixed liquor than being 1: 1.1-1: 1.2；
(4) it separates: the resulting dialdehyde starch mixed liquor of step (3) being added in the centrifuge with filter cloth and separates to obtain dialdehyde shallow lake
Powder crude product；
(5) it washes: after dialdehyde starch crude product is washed, is dehydrated, obtaining wet dialdehyde starch；
(6) dry: the resulting wet dialdehyde starch of step (5) is drying to obtain product dialdehyde starch.
In step (1), it to be kept stirring state, to prevent starch granules from precipitating, dialdehyde made from guarantee below forms sediment
The oxidizability of powder is uniform.
As optimization, step (5) washing washes dialdehyde starch crude product to be passed through deionized water in centrifuge
It washs, be dehydrated 3-5 times.
For the sake of concise explanation problem, a kind of dialdehyde starch is prepared in homogeneous system to of the present invention below
Provided method is made from starch, first make starch in water Heat Gelatinization formed homogeneous system, then again with
The reaction of oxidant periodic acid.Reaction condition is mild, reaction rate is high, occurs without side reaction；Prepared product oxidizability uniformly,
Good water solubility.
According to the dialdehyde starch that this patent method produces, aldehyde group content is greater than 90%.
In conclusion the reaction generating rate of dialdehyde starch can be improved using this method, dialdehyde starch oxidizability obtained
It is uniform.
Specific embodiment
Below by specific embodiment, the invention will be further described:
Embodiment 1:
A method of preparing dialdehyde starch in homogeneous system, comprising the following steps:
(1) it mixes: under stirring, 6 weight starch being added into 100 parts by weight deionized waters, form starch milk；
(2) it is gelatinized: being 1.2 × 10 by pressure5The vapor of Pa is passed through in starch milk prepared by step (1), to starch
When newborn temperature reaches 72 DEG C, stops being passed through steam after maintaining 72 DEG C of 15min, be cooled to 38 DEG C, obtain gelatinized corn starch；
(3) it aoxidizes: under stirring, hydrochloric acid being added into gelatinized corn starch prepared by step (2), adjusts gelatinized corn starch pH value
To 0.8；Temperature is controlled under the conditions of 38 DEG C, periodic acid (HIO is added into gelatinized corn starch4), HIO4Molar ratio with starch is 1:
1.1, the reaction time controls in 3.5h, obtains dialdehyde starch mixed liquor；
(4) it separates: the resulting dialdehyde starch mixed liquor of step (3) being added in GK800N horizontal scraper discharging centrifuge and is divided
From dialdehyde starch crude product；
(5) it washes: being passed through deionized water in GK800N horizontal scraper discharging centrifuge and dialdehyde starch crude product is washed
It washs, be dehydrated 3 times, the control of water washing operations centrifuge speed is 1500r/min, obtains wet dialdehyde starch；
(6) dry: the resulting wet dialdehyde starch of step (5) is dried in airstream drying tower to get product dialdehyde starch.
Embodiment 2:
A method of preparing dialdehyde starch in homogeneous system, comprising the following steps:
(1) it mixes: under stirring, 7 weight starch being added into 100 parts by weight deionized waters, form starch milk；
(2) it is gelatinized: being 1.5 × 10 by pressure5The vapor of Pa is passed through in starch milk prepared by step (1), to starch
When newborn temperature reaches 78 DEG C, stops being passed through steam after keeping 78 DEG C of temperature 10min, be cooled to 40 DEG C, obtain gelatinized corn starch；
(3) it aoxidizes: under stirring, hydrochloric acid being added into gelatinized corn starch prepared by step (2), adjusts gelatinized corn starch solution
PH value 1.2；Temperature is controlled under the conditions of 40 DEG C, then periodic acid (HIO is added into gelatinized corn starch4), HIO4Molar ratio with starch is
1: 1.2, the reaction time controls in 3h, obtains dialdehyde starch mixed liquor；
(4) it separates: the resulting dialdehyde starch mixed liquor of step (3) being added in GK800N horizontal scraper discharging centrifuge and is divided
From dialdehyde starch crude product；
(5) it washes: being passed through deionized water in GK800N horizontal scraper discharging centrifuge and dialdehyde starch crude product is washed
It washs, be dehydrated 5 times, obtain wet dialdehyde starch；
(6) dry: the resulting wet dialdehyde starch of step (5) is dry under the conditions of 90 DEG C, obtain product dialdehyde starch.
Embodiment 3:
A method of preparing dialdehyde starch in homogeneous system, comprising the following steps:
(1) it mixes: under stirring, 6 weight starch being added into 100 parts by weight deionized waters, form starch milk；
(2) it is gelatinized: being 1.3 × 10 by pressure5The vapor of Pa is passed through in starch milk prepared by step (1), to starch
When newborn temperature reaches 75 DEG C, stops being passed through steam after keeping 75 DEG C of temperature 12min, be cooled to 40 DEG C, obtain gelatinized corn starch；
(3) it aoxidizes: under stirring, hydrochloric acid being added into gelatinized corn starch prepared by step (2), adjusts gelatinized corn starch solution
PH value 1.0；Temperature is controlled under the conditions of 40 DEG C, then periodic acid (HIO is added into gelatinized corn starch4), HIO4Molar ratio with starch is
1: 1.1, the reaction time controls in 3h, obtains dialdehyde starch mixed liquor；
(4) it separates: the resulting dialdehyde starch mixed liquor of step (3) being added in GK800N horizontal scraper discharging centrifuge and is divided
From obtaining dialdehyde starch crude product；
(5) it washes: being passed through deionized water in GK800N horizontal scraper discharging centrifuge and dialdehyde starch crude product is washed
It washs, be dehydrated 4 times, obtain wet dialdehyde starch；
(6) dry: the resulting wet dialdehyde starch of step (5) is dry under the conditions of 90 DEG C, obtain product dialdehyde starch.
Above-described is only three kinds of embodiments of the invention, it is noted that for those of ordinary skill in the art
For, it without departing from the principle of the present invention, can also make several improvements, these also should be regarded as belonging to guarantor of the invention
Protect range.
Claims (2)
1. a kind of method for preparing dialdehyde starch in homogeneous system, comprising the following steps:
(1) it mixes: under stirring, 6-7 weight starch being added into 100 parts by weight deionized waters, forms starch milk；
(2) it is gelatinized: being 1.2-1.5 × 10 by pressure5The vapor of Pa is passed through in starch milk prepared by step (1), to starch milk
Stop being passed through steam after keeping temperature 10-15min when temperature reaches 72-78 DEG C, is cooled to 38-40 DEG C, obtains gelatinized corn starch；
(3) it aoxidizes: under stirring, hydrochloric acid being added into gelatinized corn starch prepared by step (2), adjusts gelatinized corn starch solution ph
To 0.8-1.2；Temperature is controlled under the conditions of 38-40 DEG C, then periodic acid is added into gelatinized corn starch, the molar ratio of periodic acid and starch
It is 1: 1.1-1: 1.2, reacts 3-3.5h, obtain dialdehyde starch mixed liquor；
(4) separate: the resulting dialdehyde starch mixed liquor of step (3) is added in the centrifuge with filter cloth separate dialdehyde starch is thick
Product；
(5) it washes: after dialdehyde starch crude product is washed, is dehydrated, obtaining wet dialdehyde starch；
(6) dry: the resulting wet dialdehyde starch of step (5) is drying to obtain product dialdehyde starch.
2. a kind of method for preparing dialdehyde starch in homogeneous system according to claim 1, it is characterised in that: step
(5) washing is washed dialdehyde starch crude product, is dehydrated 3-5 times to be passed through deionized water in centrifuge.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910177466.1A CN109824789A (en) | 2019-03-09 | 2019-03-09 | A method of preparing dialdehyde starch in homogeneous system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910177466.1A CN109824789A (en) | 2019-03-09 | 2019-03-09 | A method of preparing dialdehyde starch in homogeneous system |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580076A (en) * | 2003-08-07 | 2005-02-16 | 南京工业大学 | Prepuration of oxidation starch by pseudo homogeneous system |
| CN101948548A (en) * | 2010-07-20 | 2011-01-19 | 长春工业大学 | Device and method for preparing dialdehyde starch from corn starch by photo-catalytic oxidation |
| CN105646723A (en) * | 2016-03-30 | 2016-06-08 | 中南林业科技大学 | Dialdehyde starch and preparation method thereof |
| CN107779122A (en) * | 2017-11-17 | 2018-03-09 | 广东玉兰集团股份有限公司 | A kind of starch adhesive and preparation method thereof |
-
2019
- 2019-03-09 CN CN201910177466.1A patent/CN109824789A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1580076A (en) * | 2003-08-07 | 2005-02-16 | 南京工业大学 | Prepuration of oxidation starch by pseudo homogeneous system |
| CN101948548A (en) * | 2010-07-20 | 2011-01-19 | 长春工业大学 | Device and method for preparing dialdehyde starch from corn starch by photo-catalytic oxidation |
| CN105646723A (en) * | 2016-03-30 | 2016-06-08 | 中南林业科技大学 | Dialdehyde starch and preparation method thereof |
| CN107779122A (en) * | 2017-11-17 | 2018-03-09 | 广东玉兰集团股份有限公司 | A kind of starch adhesive and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 庄培贤 等: "拟均相法制备双醛淀粉", 《三明学院学报》 * |
| 朱颖 等: "双醛淀粉酸解氧化制备工艺优化研究", 《西南林业大学学报》 * |
| 罗菊香 等: "正交法优化拟均相体系制备双醛淀粉的工艺", 《化学与生物工程》 * |
| 高娜: "《马铃薯变性淀粉》", 31 October 2015, 武汉大学出版社 * |
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Application publication date: 20190531 |