CN109503726A - A kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch - Google Patents
A kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch Download PDFInfo
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- CN109503726A CN109503726A CN201810747812.0A CN201810747812A CN109503726A CN 109503726 A CN109503726 A CN 109503726A CN 201810747812 A CN201810747812 A CN 201810747812A CN 109503726 A CN109503726 A CN 109503726A
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- C08B31/00—Preparation of derivatives of starch
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Abstract
The invention discloses the preparation methods that a kind of one-step method carries out cross-linked hydroxypropyl base composite modified starch, include the following steps: that swelling inhibitor, etherifying reagent A and crosslinking agent are added in deionized water, it is stirring evenly and then adding into starch, starch slurry cream is tuned into, stirs to obtain reaction solution B；PH adjusting agent is added in reaction solution B, adjusts the pH of reaction solution B, then heats, etherifying reagent D etherification reaction is added and obtains reaction solution C；The pH to 7.0 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；Starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；Up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.It may make cross-linking reaction time to extend using one-step method, also can just reduce the production cost of product due to reducing the dosage of crosslinking agent to control the degree of cross linking of product by reducing dosage of crosslinking agent.
Description
Technical field
The present invention relates to starch technical field, specifically a kind of one-step method carries out the system of cross-linked hydroxypropyl base composite modified starch
Preparation Method.
Background technique
Hydroxypropul starch is that with the alcoholic extract hydroxyl group in starch nucleophilic substitution occurs for propylene oxide under alkaline condition, is being formed sediment
A kind of ether compound for introducing hydroxylpropyl groups in powder and generating.Hydroxypropul starch as one of converted starch representative products,
It is low with gelatinization point, paste transparency height, good fluidity, retrogradation is weak, stability is high, paste liquid small, energy is influenced by electrolyte
The excellent physicochemical property such as use in wider soda acid pH value range, what consumer used in finishing at present is mostly formaldehydes
Adhesive, urea-formaldehyde resin adhesive and phenolic resin adhesive, these three adhesives can be released continuously in use
It releases formaldehyde and release time is long, seriously endanger the health and ecological environment for arriving the mankind.
Summary of the invention
The purpose of the present invention is to provide a kind of one-step method carry out cross-linked hydroxypropyl base composite modified starch preparation method, with
Solve the problems mentioned above in the background art.
To achieve the above object, the invention provides the following technical scheme:
A kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, includes the following steps:
S1: taking the deionized water of a certain amount of starch and 5 times of relative starch quality, is then added in deionized water opposite
In swelling inhibitor of the starch quality than 17~21%, the etherifying reagent A relative to starch quality than 2~5% and relative to shallow lake
The crosslinking agent of powder mass ratio 0.5~1.3%, is stirring evenly and then adding into starch, is tuned into starch slurry cream, stirs 25~40min, obtain instead
Answer solution B；
S2: the pH adjusting agent relative to starch quality than 3.2~4.8% is added in reaction solution B, adjusts reaction solution
The pH to 7.2~9.8 of B is then heated to 45~60 DEG C, and the etherifying reagent D relative to starch quality than 4.8~8% is added,
3~5h of etherification reaction obtains reaction solution C；
S3: the pH to 6.2~7.0 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；
S4: the starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；
S5: up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.
As a further solution of the present invention: sequentially adding expansion in the step S1 in deionized water in stirring and inhibit
Agent, etherifying reagent A and crosslinking agent.
As the present invention further scheme: the etherifying reagent A be propylene oxide, ethylene oxide one kind or and its
Mixture.
As further scheme of the invention: the swelling inhibitor is sodium chloride, and the crosslinking agent is epoxy chloropropionate
Alkane.
As further scheme of the invention: etherifying reagent D is chloroacetic acid in the step C2.
As the present invention further scheme: the step S5 to starch milk centrifugal dehydration five times, and every time dehydration 1~
2h。
As the present invention further scheme: the starch in the step A is corn, potato, in glutinous rice starch
One or more combination.
Compared with prior art, the beneficial effects of the present invention are: the system of cross-linked hydroxypropyl base composite modified starch of the invention
Under the premise of ensureing starch granules integrality in Preparation Method, pH value of starch milk is preconditioned, the alkali in postorder alkalinization is reduced
The dosage of solution, improves the concentration of starch milk indirectly, to improve crosslinking and etherification reaction efficiency, reduces and is produced into
This may make cross-linking reaction time to extend since the etherification reaction time is longer using one-step method, can be by reducing crosslinking agent
Dosage also just reduces the production cost of product, uses effect to control the degree of cross linking of product due to reducing the dosage of crosslinking agent
Fruit is good, and alternative tradition adhesive reduces harm of the building decoration articles to human health and environment as wallpaper glue.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one: a kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, includes the following steps:
S1: taking the deionized water of a certain amount of starch and 5 times of relative starch quality, is then added in deionized water opposite
In swelling inhibitor of the starch quality than 17%, the etherifying reagent A relative to starch quality than 2% and relative to starch quality ratio
0.5% crosslinking agent, is stirring evenly and then adding into starch, is tuned into starch slurry cream, stirs 25min, obtain reaction solution B；
S2: the pH adjusting agent relative to starch quality than 3.2% is added in reaction solution B, adjusts the pH of reaction solution B
To 7.2,45 DEG C are then heated to, the etherifying reagent D relative to starch quality than 4.8% is added, etherification reaction 3h must react
Solution C；
S3: the pH to 6.2 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；
S4: the starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；
S5: up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.
Sequentially add swelling inhibitor, etherifying reagent A and crosslinking agent in the step S1 in deionized water in stirring.
The etherifying reagent A is propylene oxide.
The swelling inhibitor is sodium chloride, and the crosslinking agent is epoxychloropropane.
Etherifying reagent D is chloroacetic acid in the step C2.
The step S5 is dehydrated 1h to starch milk centrifugal dehydration five times every time.
Starch in the step A is cornstarch.
Embodiment two: a kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, includes the following steps:
S1: taking the deionized water of a certain amount of starch and 5 times of relative starch quality, is then added in deionized water opposite
In swelling inhibitor of the starch quality than 19%, the etherifying reagent A relative to starch quality than 3.5% and relative to starch quality
Crosslinking agent than 0.9%, is stirring evenly and then adding into starch, is tuned into starch slurry cream, stirs 30min, obtain reaction solution B；
S2: the pH adjusting agent relative to starch quality than 4% is added in reaction solution B, adjusts the pH of reaction solution B
To 8,50 DEG C are then heated to, the etherifying reagent D relative to starch quality than 6% is added, etherification reaction 4h obtains reaction solution C；
S3: the pH to 6.6 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；
S4: the starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；
S5: up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.
Sequentially add swelling inhibitor, etherifying reagent A and crosslinking agent in the step S1 in deionized water in stirring.
The etherifying reagent A is ethylene oxide.
The swelling inhibitor is sodium chloride, and the crosslinking agent is epoxychloropropane.
Etherifying reagent D is chloroacetic acid in the step C2.
The step S5 is dehydrated 1.5h to starch milk centrifugal dehydration five times every time.
Starch in the step A is potato starch.
Embodiment three: a kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, which is characterized in that packet
Include following steps:
S1: taking the deionized water of a certain amount of starch and 5 times of relative starch quality, is then added in deionized water opposite
In swelling inhibitor of the starch quality than 21%, the etherifying reagent A relative to starch quality than 5% and relative to starch quality ratio
1.3% crosslinking agent, is stirring evenly and then adding into starch, is tuned into starch slurry cream, stirs 40min, obtain reaction solution B；
S2: the pH adjusting agent relative to starch quality than 4.8% is added in reaction solution B, adjusts reaction solution B's
PH to 9.8 is then heated to 6. DEG C, and the etherifying reagent D relative to starch quality than 8% is added, and etherification reaction 5h must react molten
Liquid C；
S3: the pH to 7.0 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；
S4: the starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；
S5: up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.
Sequentially add swelling inhibitor, etherifying reagent A and crosslinking agent in the step S1 in deionized water in stirring.
The etherifying reagent A is the mixture of propylene oxide and ethylene oxide.
The swelling inhibitor is sodium chloride, and the crosslinking agent is epoxychloropropane.
Etherifying reagent D is chloroacetic acid in the step C2.
The step S5 is dehydrated 2h to starch milk centrifugal dehydration five times every time.
Starch in the step A is the combination of corn, potato and glutinous rice starch.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (7)
1. the preparation method that a kind of one-step method carries out cross-linked hydroxypropyl base composite modified starch, which comprises the steps of:
S1: the deionized water of a certain amount of starch and 5 times of relative starch quality is taken, is then added in deionized water relative to shallow lake
The swelling inhibitor of powder mass ratio 17~21%, the etherifying reagent A relative to starch quality than 2~5% and relative to starchiness
The crosslinking agent than 0.5~1.3% is measured, starch is stirring evenly and then adding into, starch slurry cream is tuned into, stirs 25~40min, must react molten
Liquid B；
S2: the pH adjusting agent relative to starch quality than 3.2~4.8% is added in reaction solution B, adjusts reaction solution B's
PH to 7.2~9.8 is then heated to 45~60 DEG C, and the etherifying reagent D relative to starch quality than 4.8~8%, etherificate is added
3~5h is reacted, reaction solution C is obtained；
S3: the pH to 6.2~7.0 that organic acid soln adjusting reaction solution C is added into reaction solution 2 obtains starch milk；
S4: the starch milk after neutralization is passed through into washing removal impurity and byproduct of reaction；
S5: up to cross-linked hydroxypropyl base composite modified starch after last time progress centrifugal dehydration, drying, sieving.
2. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In sequentially adding swelling inhibitor, etherifying reagent A and crosslinking agent in the step S1 in deionized water in stirring.
3. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In the etherifying reagent A is propylene oxide, one kind of ethylene oxide or and its mixture.
4. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In the swelling inhibitor is sodium chloride, and the crosslinking agent is epoxychloropropane.
5. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In etherifying reagent D is chloroacetic acid in the step C2.
6. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In the step S5 is dehydrated 1~2h to starch milk centrifugal dehydration five times every time.
7. one-step method according to claim 1 carries out the preparation method of cross-linked hydroxypropyl base composite modified starch, feature exists
In the starch in the step A is the combination of one or more of corn, potato, glutinous rice starch.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113150176A (en) * | 2021-04-27 | 2021-07-23 | 山东光大赛路新材料科技有限公司 | Preparation method of multi-group cross-linked modified hydroxypropyl starch ether |
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| KR20120075746A (en) * | 2010-12-29 | 2012-07-09 | 주식회사 삼양제넥스 | Hydroxyalkyl carboxyalkyl starch and method for manufacturing the same |
| CN103113478A (en) * | 2013-03-18 | 2013-05-22 | 甘肃圣大方舟马铃薯变性淀粉有限公司 | Preparation method of cross-linked hydroxypropyl composite modified starch by one-step process |
| CN105418775A (en) * | 2015-12-19 | 2016-03-23 | 河南恒瑞淀粉科技股份有限公司 | Cross-linked carboxymethyl hydroxypropylated compound modified starch and preparation method thereof |
| CN107602713A (en) * | 2017-09-25 | 2018-01-19 | 山东神州翔宇科技集团有限公司 | A kind of one-step method carries out the preparation method of cross-linked hydroxypropyl base composite modified starch |
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| KR20120075746A (en) * | 2010-12-29 | 2012-07-09 | 주식회사 삼양제넥스 | Hydroxyalkyl carboxyalkyl starch and method for manufacturing the same |
| CN103113478A (en) * | 2013-03-18 | 2013-05-22 | 甘肃圣大方舟马铃薯变性淀粉有限公司 | Preparation method of cross-linked hydroxypropyl composite modified starch by one-step process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113150176A (en) * | 2021-04-27 | 2021-07-23 | 山东光大赛路新材料科技有限公司 | Preparation method of multi-group cross-linked modified hydroxypropyl starch ether |
| CN113150176B (en) * | 2021-04-27 | 2022-11-22 | 山东光大赛路新材料科技有限公司 | Preparation method of multi-group cross-linked modified hydroxypropyl starch ether |
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Address after: 277400 Residence of Malantun Town, Taierzhuang District, Zaozhuang City, Shandong Province Applicant after: Shandong Shenzhou Xiangyu Science and Technology Group Co., Ltd. Address before: 277400 Residence of Malantun Town, Taierzhuang District, Zaozhuang City, Shandong Province Applicant before: Shandong Shenzhou Xiangyu Technology Group Co., Ltd. |
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Application publication date: 20190322 |