CN106832016A - Carboxy methylation porous-starch and preparation method thereof - Google Patents
Carboxy methylation porous-starch and preparation method thereof Download PDFInfo
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- C08B31/00—Preparation of derivatives of starch
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Abstract
The invention discloses a kind of carboxy methylation porous-starch and preparation method thereof.The preparation method includes：Just porous-starch mixes and the insulation that flows back with solvent, and treatment is dried afterwards, obtains dried object；Chloroacetic carbon tetrachloride solution and hybrid reaction are added after above-mentioned dried object is mixed with triethylamine；To addition solvent and sediment separate out in above-mentioned reactant mixture；And successively by above-mentioned reactant mix with acid solution and aqueous slkali cleaning obtain sediment；And carboxy methylation porous-starch will be obtained after the final drying precipitate treatment for obtaining.The preparation method technological process that the present invention is provided is simple, low production cost, it is adapted to large-scale production and applies, the carboxy methylation porous-starch feel that the present invention is obtained simultaneously is more satiny, the water surface can be suspended in, and with a thin layer of wax-like layer, and its is safe and nontoxic, can be widely applied to the fields such as food, medicine, health.
Description
Technical field
The present invention relates to a kind of porous-starch and preparation method thereof, more particularly to a kind of carboxy methylation porous-starch and its system
Preparation Method, belongs to technical field of food additives.
Background technology
Porous-starch be uncooked amylum under less than starch gelatinization temperature through peracid or amylorrhexis after, and particle is presented
A kind of cavernous new converted starch.It is porous to produce very big specific surface area, thus porous-starch is mainly used as absorption
Carrier.Compared with other adsorbents, porous-starch has good absorption property.But through porous-starch obtained in Partial digestion
Particle, its structure is subject to a certain degree of destruction, its antilysis, anti-swelling, pasting temperature, freeze-thaw stability and viscosity stablization
The performance indications such as property are below ative starch.And cross-linking reaction can strengthen the structure of starch granules, increase the broken ability of resistance to mechanical
With expansion of the suppression amylum body in water, gelatinized corn starch is become stabilization and be difficult retrogradation, therefore can be changed using Chemical Crosslinking Methods
The rheology of kind porous-starch forms a kind of converted starch of many apertures that center is stretched to from surface on surface.
Carboxy methylation porous-starch is that the porous-starch particle that carboxymethyl group is obtained is introduced in porous-starch molecule.It
It is a kind of composite modified starch, with larger specific surface area, and is dispersed in holding in water and other solvents under certain condition
The integrality of its structure, with good water suction, oil absorbency.Also there is hydrophily, easily gelatinization in addition, cold water can be swelling, glues
Degree stabilization, transparency is high, and retrogradation is weak, the advantages of freeze-thaw stability is good.It can as spices, flavor substance, pigment, medicament and
The absorption carrier of functional component in health food, at the same time as emulsifying agent, thickener, adhesive, stabilizer, food addition
Agent, sizing agent, suspending agent, film forming agent, agent etc. is homogenized, there is broad prospect of application at aspects such as food, medicine, chemical industry, agriculturals.
The preparation technology of country's carboxy methylation porous-starch is more with cornstarch and farina as raw material at present, passes through
Alkalization, etherificate, washing, filtering, dry and crush etc. step, finished product.But proterties is not often notable, on a large scale should be unfavorable for
With.
The content of the invention
It is a primary object of the present invention to provide a kind of carboxy methylation porous-starch and preparation method thereof, to overcome existing skill
The deficiency of art.
To realize aforementioned invention purpose, the technical solution adopted by the present invention includes：
The one side of the embodiment of the present invention provides a kind of preparation method of carboxy methylation porous-starch, and it includes as follows
Step：
(1) porous-starch is mixed and the insulation that flows back with solvent, treatment is dried afterwards, obtain dried object；
(2) after step (1) resulting dried thing is uniformly mixed with triethylamine, add containing chloroacetic carbon tetrachloride solution
And hybrid reaction；
(3) to solvent is added in step (2) finally obtained mixed reactant, after uniform mixing, precipitation therein is isolated
Thing is simultaneously cleaned；
(4) by step (3), finally obtained sediment mixes with acid solution, then isolates sediment therein and clean；
(5) by step (4), finally obtained sediment mixes with aqueous slkali, then isolates sediment therein and clean；
(6) by final the obtained drying precipitate of step (5), carboxy methylation porous-starch is obtained.
Further, abovementioned steps (1) include：Porous-starch is mixed with solvent and in 98~99 DEG C of backflow insulation 24h
More than, and soxhlet type is carried out, and treatment is dried afterwards, obtain dried object.
Preferably, the temperature of the dried process for being used in abovementioned steps (1) is 100~110 DEG C, and the time is 2~3h.
Further, abovementioned steps (2) include：Step (1) resulting dried thing is mixed and stirring at normal temperature 30h with triethylamine
More than, triethylamine is continuously added afterwards and forms mixture, thereafter in 15min to adding chloroacetic four in the mixture
Carbon chloride solution, continues 3~4h of stirring reaction；Preferably, the dried object is molten with triethylamine and chloroacetic carbon tetrachloride
The mass ratio of liquid is 1：0.4~0.8：0.2~0.4：0.2~0.4；Preferably, the chloroacetic carbon tetrachloride solution is dense
It is 0.45~0.5g/100mL to spend.
Preferably, step (2) includes：Chloroacetic carbon tetrachloride solution will be contained with the speed of 1 drop/5s and add the mixing
Thing.
Further, abovementioned steps (3) include：To adding solvent in step (2) finally obtained mixed reactant, and continue
0.5~1h of stirring, afterwards centrifugation goes out sediment therein, then with solvent cyclic washing 2~3 times, after washing is finished every time
Centrifugation goes out sediment.
Preferably, the centrifugal speed for being used in abovementioned steps (3) is 3000~4000rpm, and the time is 10~15min.
Further, abovementioned steps (4) include：By step (3), finally obtained sediment mixes with water, adds acid molten afterwards
Liquid regulation mixed system to acidity, then centrifugation goes out sediment therein and cleans；Preferably, the acid solution includes concentration
It is the hydrochloric acid solution of 0.1mol/L.
Preferably, step (4) includes：The pH value for adding acid solution regulation mixed system is 2.1~2.3.
Preferably, be in step (4) temperature be 4 DEG C under conditions of be centrifuged, centrifugal speed be 3000~
4000rpm, centrifugation time is 10~15min.
Further, abovementioned steps (5) include：By step (4), finally obtained sediment mixes with aqueous slkali, forms pH value
It is 7.1~7.2 mixture, then centrifugation goes out sediment therein and cleans.
Preferably, the aqueous slkali includes sodium hydroxide solution that concentration is 0.1~0.2mol/L.
Preferably, be in step (5) temperature be 4 DEG C under conditions of be centrifuged, centrifugal speed be 3000~
4000rpm, centrifugation time is 10~15min.
Further, abovementioned steps (6) include：By step (5) finally obtained sediment in 100~110 DEG C of dryings 2~
3h, obtains carboxy methylation porous-starch.
Further, the porous-starch is including corn porous starch etc., but not limited to this.
Further, the solvent include ethanol, 95% particularly common (V/V) ethanol, it can be by commercially available approach
Obtain.
In some more specifically case study on implementation, described preparation method is specifically included：
(1) dephosphorization：A certain amount of corn porous starch is added into 95% appropriate ethanol, 98~99 DEG C of backflows are incubated 24h,
Soxhlet type (dephosphorization), dries (105 DEG C, 2~3h)；
(2) react：A certain amount of dry triethylamine, stirring at normal temperature 30h are added in above-mentioned dried object；Add appropriate dry
Triethylamine, add in 15min and contain chloroacetic carbon tetrachloride solution, add speed about 1 drop/5s, stir 3~4h；
(3) alcohol is washed：95% appropriate ethanol is added in above-mentioned reactant, 0.5~1h is stirred, be centrifuged (3000~
4000rpm, 10~15min), it is precipitated；Again with 95% ethanol cyclic washing 2~3 times；95% ethanol of each addition, then from
The heart (3000~4000rpm, 10~15min)；
(4) pickling：A certain amount of water is added in above-mentioned precipitation repeatedly, pH value 2.2 is adjusted with 0.1mol/L hydrochloric acid, because of carboxylic
Methyl starch is insoluble, forms precipitation, is centrifuged (3000~4000rpm, 10~15min, 4 DEG C)；
(5) alkali cleaning：0.1mol/L NaOH is added to adjust pH value 7.1 in above-mentioned precipitation, be centrifuged (3000~4000rpm,
10~15min, 4 DEG C)；
(6) dry：By above-mentioned centrifugal sediment in 105 DEG C of 2~3h of drying, carboxy methylation porous-starch is obtained.
Further, the yield of the preparation method of the carboxy methylation porous-starch is more than 80%.
The one side of the embodiment of the present invention additionally provides the carboxy methylation porous-starch prepared by foregoing any one method.
Compared with prior art, the preparation method technological process that the present invention is provided is simple, low production cost, is adapted to extensive
Production and application；Meanwhile, carboxy methylation porous-starch feel prepared by the present invention is more satiny, can be suspended in the water surface, and have
There is a thin layer of wax-like layer, and carboxy methylation porous-starch prepared by the present invention is safe and nontoxic, can be widely applied to food
The fields such as product, medicine, health.
Specific embodiment
In view of deficiency of the prior art, inventor is able to propose of the invention through studying for a long period of time and largely put into practice
Technical scheme.The technical scheme, its implementation process and principle etc. will be further explained in conjunction with the embodiments as follows.
Embodiment 1：Take 40g corn porous starch and add the ethanol of 125mL 95%, flow back insulation 24h, rope at a temperature of 98 DEG C
Family name extracts (dephosphorization), dries (105 DEG C, 2h)；The dry triethylamines of 20mL, stirring at normal temperature 30h, mixing are added in above-mentioned dried object
The dry triethylamines of 10mL are added after reaction, the chloroacetic 10mL carbon tetrachloride solutions containing 0.478g are then added in 15min, plus
Enter speed about 1 drop/5s, stir 3.5h；95% ethanol 40mL is added in above-mentioned reactant, 0.5h is stirred, be centrifuged (3000rpm,
10min), it is precipitated；Again with the above-mentioned precipitation of 95% ethanol cyclic washing 2 times；95% ethanol 40mL is added every time, then is centrifuged
(3000rpm, 10min)；40mL water is added in the precipitation of above-mentioned cyclic washing three times, adjusts the pH value to be with 0.1mol/L hydrochloric acid
2.2, it is centrifuged (3000rpm, 10min, 4 DEG C)；It is 7.1 to add 0.1mol/L NaOH to adjust pH value in above-mentioned precipitation, centrifugation
(3000rpm, 10min, 4 DEG C)；Above-mentioned centrifugal sediment is dried into 2h in 105 DEG C, carboxy methylation porous-starch is obtained.
It is as follows with existing carboxy methylation porous-starch process ration：
Embodiment 2：Take 60g corn porous starch and add the ethanol of 135mL 95%, 99 DEG C of backflow insulation 24h, soxhlet type
(dephosphorization), dries (105 DEG C, 2h)；The dry triethylamines of 25mL, stirring at normal temperature 30h, after hybrid reaction are added in above-mentioned dried object
The dry triethylamines of 15mL are added, the chloroacetic 10mL carbon tetrachloride solutions containing 0.5g are then added in 15min, add speed about
1 drop/5s, stirs 4h；95% ethanol 50mL is added in above-mentioned reactant, 0.5h is stirred, is centrifuged (3500rpm, 15min), obtained
To precipitation；Again with the above-mentioned precipitation of 95% ethanol cyclic washing 2 times；95% ethanol 40mL of each addition, then be centrifuged (3500rpm,
15min)；50mL water is added in the precipitation of above-mentioned cyclic washing three times, it is 2.2 to adjust pH value with 0.1mol/L hydrochloric acid, centrifugation
(3500rpm, 15min, 4 DEG C)；It is 7.2 to add 0.1mol/L NaOH to adjust pH value in above-mentioned precipitation, centrifugation (3500rpm,
10min, 4 DEG C)；Above-mentioned centrifugal sediment is dried into 3h in 105 DEG C, carboxy methylation porous-starch is obtained.
It is as follows with existing carboxy methylation porous-starch process ration：
Embodiment 3：Take 100g corn porous starch and add the ethanol of 150mL 95%, 98 DEG C of backflow insulation 24h, soxhlet type
(dephosphorization), dries (105 DEG C, 3h)；The dry triethylamines of 30mL, stirring at normal temperature 30h, after hybrid reaction are added in above-mentioned dried object
The dry triethylamines of 20mL are added, the chloroacetic 15mL carbon tetrachloride solutions containing 0.5g are then added in 15min, add speed about
1 drop/5s, stirs 4h；95% ethanol 65mL is added in above-mentioned reactant, 0.5h is stirred, is centrifuged (3500rpm, 10min), obtained
To precipitation；Again with the above-mentioned precipitation of 95% ethanol cyclic washing 2 times；95% ethanol 50mL of each addition, then be centrifuged (3500rpm,
10min)；50mL water is added in the precipitation of above-mentioned cyclic washing three times, it is 2.2 to adjust pH value with 0.1mol/L hydrochloric acid, centrifugation
(3500rpm, 10min, 4 DEG C)；It is 7.1 to add 0.1mol/L NaOH to adjust pH value in above-mentioned precipitation, centrifugation (3500rpm,
10min, 4 DEG C)；Above-mentioned centrifugal sediment is dried into 3h in 105 DEG C, carboxy methylation porous-starch is obtained.
It is as follows with existing carboxy methylation porous-starch process ration：
It should be appreciated that above-described embodiment is only explanation technology design of the invention and feature, this is familiar with its object is to allow
The personage of item technology will appreciate that present disclosure and implement according to this that it is not intended to limit the scope of the present invention.It is all
According to the equivalent change or modification that spirit of the invention is made, should all be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of carboxy methylation porous-starch, it is characterised in that comprise the following steps：
(1) porous-starch is mixed and the insulation that flows back with solvent, treatment is dried afterwards, obtain dried object；
(2) after step (1) resulting dried thing is uniformly mixed with triethylamine, add containing chloroacetic carbon tetrachloride solution and mix
Close reaction；
(3) to solvent is added in step (2) finally obtained mixed reactant, after uniform mixing, sediment therein is isolated simultaneously
Cleaning；
(4) by step (3), finally obtained sediment mixes with acid solution, then isolates sediment therein and clean；
(5) by step (4), finally obtained sediment mixes with aqueous slkali, then isolates sediment therein and clean；
(6) by final the obtained drying precipitate of step (5), carboxy methylation porous-starch is obtained.
2. preparation method according to claim 1, it is characterised in that step (1) includes：Porous-starch is mixed with solvent
And in 98~99 DEG C of backflow insulation more than 24h, and soxhlet type is carried out, and treatment is dried afterwards, obtain dried object；It is preferred that
, the temperature of the dried process is 100~110 DEG C, and the time is 2~3h.
3. preparation method according to claim 1, it is characterised in that step (2) includes：By step (1) resulting dried thing
Mix with triethylamine and more than stirring at normal temperature 30h, triethylamine continuously added afterwards and forms mixture, thereafter in 15min to
Chloroacetic carbon tetrachloride solution is added in the mixture, continues 3~4h of stirring reaction；Preferably, the dried object and three
The mass ratio of ethamine and chloroacetic carbon tetrachloride solution is 1：0.4~0.8：0.2~0.4：0.2~0.4；Preferably, institute
The concentration for stating chloroacetic carbon tetrachloride solution is 0.45~0.5g/100mL；Preferably, step (2) includes：With 1 drop/5s's
Speed will contain chloroacetic carbon tetrachloride solution and add the mixture.
4. preparation method according to claim 1, it is characterised in that step (3) includes：It is finally obtained mixed to step (2)
Solvent is added in conjunction reactant, and continues 0.5~1h of stirring, centrifugation afterwards goes out sediment therein, then with solvent repeatedly
Washing 2~3 times, each washing finishes rear centrifugation and goes out sediment；Preferably, wherein the centrifugal speed for using for 3000~
4000rpm, the time is 10~15min.
5. preparation method according to claim 1, it is characterised in that step (4) includes：Step (3) is finally obtained heavy
Starch mixes with water, adds acid solution regulation mixed system to acidity, then centrifugation to go out sediment therein and clean afterwards；
Preferably, the acid solution includes that concentration is the hydrochloric acid solution of 0.1mol/L；Preferably, step (4) includes：Acid solution is added to adjust
The pH value for saving mixed system is 2.1~2.3；Preferably, it is to be centrifuged under conditions of temperature is for 4 DEG C in step (4), is centrifuged
Speed is 3000~4000rpm, and centrifugation time is 10~15min.
6. preparation method according to claim 1, it is characterised in that step (5) includes：Step (4) is finally obtained heavy
Starch mixes with aqueous slkali, forms the mixture that pH value is 7.1~7.2, then centrifugation goes out sediment therein and cleans；It is excellent
Choosing, the aqueous slkali includes sodium hydroxide solution that concentration is 0.1~0.2mol/L；Preferably, it is in temperature in step (5)
To be centrifuged under conditions of 4 DEG C, centrifugal speed is 3000~4000rpm, and centrifugation time is 10~15min.
7. preparation method according to claim 1, it is characterised in that step (6) includes：Step (5) is finally obtained heavy
Starch obtains carboxy methylation porous-starch in 100~110 DEG C of 2~3h of drying.
8. preparation method according to claim 1, it is characterised in that：The porous-starch includes corn porous starch.
9. the preparation method according to claim 1,2 or 4, it is characterised in that：The solvent includes ethanol；Preferably, institute
Stating solvent includes 95% ethanol.
10. the carboxy methylation porous-starch for being prepared as method any one of claim 1~9.
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| CN201710108660.5A CN106832016A (en) | 2017-02-27 | 2017-02-27 | Carboxy methylation porous-starch and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107433189A (en) * | 2017-08-14 | 2017-12-05 | 天津科技大学 | A kind of preparation method and applications of novel microporous starch |
| CN107714267A (en) * | 2017-08-25 | 2018-02-23 | 安徽鑫露达医疗用品有限公司 | A kind of warmer |
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| CN101830994A (en) * | 2010-05-25 | 2010-09-15 | 西南大学 | Preparation method of potato carboxymethyl starch |
| JP2016128545A (en) * | 2015-01-09 | 2016-07-14 | 日本食品化工株式会社 | Method for producing carboxymethylated starch, carboxymethylated starch and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101541836A (en) * | 2006-09-25 | 2009-09-23 | 阿彻-丹尼尔斯-米德兰德公司 | Superabsorbent surface-treated carboxyalkylated polysaccharides and process for producing same |
| CN101830994A (en) * | 2010-05-25 | 2010-09-15 | 西南大学 | Preparation method of potato carboxymethyl starch |
| JP2016128545A (en) * | 2015-01-09 | 2016-07-14 | 日本食品化工株式会社 | Method for producing carboxymethylated starch, carboxymethylated starch and use thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107433189A (en) * | 2017-08-14 | 2017-12-05 | 天津科技大学 | A kind of preparation method and applications of novel microporous starch |
| CN107714267A (en) * | 2017-08-25 | 2018-02-23 | 安徽鑫露达医疗用品有限公司 | A kind of warmer |
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