CN107433189A - A kind of preparation method and applications of novel microporous starch - Google Patents
A kind of preparation method and applications of novel microporous starch Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The present invention relates to a kind of preparation method of novel microporous starch, comprise the following steps：(1) it is gelatinized：Starch suspension is formed after a certain amount of starch is mixed with distilled water.Starch suspension is heated into 30min under conditions of 100 DEG C, obtains the gelatinized corn starch of complete gelation.(2) bring back to life：After obtained gelatinized corn starch is cooled into room temperature, 1~10 day is refrigerated at 4 DEG C until forming gel structure, obtains starch hydrogel.(3) freeze：Freezed 2 days at 20 DEG C or 80 DEG C after starch gel is cut into the cube that the length of side is 1cm with mould, the water in starch gel can build-up ice, and volumetric expansion separates out to form starch ice gel.(4) dehydrate.(5)CS2It is modified.The present invention prepares the micropore starch in micron order aperture, this material has certain suction-operated after chemical modification for heavy metal, and it has the advantages of not soluble in water, bulk is easily isolated after adsorbing, and the absorption used time is short by the combination of Four processes.
Description
Technical field
The invention belongs to the modification field of starch, more particularly, to a kind of preparation method and its warp of preferably micropore starch
Cross CS2The modified absorption for being used for heavy metal in waste water solution.
Background technology
Micropore starch (microporous starch) also known as porous-starch, it is a kind of new converted starch.Tradition meaning
The micropore starch of justice refers to amylase less than the porous cellular products for acting on uncooked amylum under gelatinization point and being formed.
With the further development of technology of preparing, micropore starch has been assigned wider definition.The method for preparing micropore starch at present
Mainly there are four classes：Physical method, chemical method, biological method and composite algorithm.Physical method mainly includes：Ultrasonic wave, spraying, machine
The extraneous physical actions such as tool shock；Chemical method is mainly sour water solution；Biological method is mainly enzymatic isolation method.Therefore, micropore is studied
The preparation of starch and structure are advantageous to the natural structure of further research starch, compare micropore starch and native starch in structure and
Qualitative difference.In addition, due to micropore starch unique property and function, it or a kind of very valuable material
Material, is widely used in each field such as food, medicine, agricultural chemicals, printing, sewage disposal, daily-use chemical industry, cosmetics.Led in food
Domain, porous-starch is as a kind of embedded material, it can be ensured that spices, sweetener, acid condiment, the stable release of flavor enhancement with
And make oxidizable compound from the destruction of light or oxygen.In medicine, pesticide field, porous-starch is used as microcapsules core, first
Specific medicine is adsorbed with porous-starch, is then discharged in certain circumstances.It is larger using porous-starch in sewage disposal
Specific surface area, the effect for the absorption heavy metal for reaching good is modified to it.In cosmetic field, porous-starch has adsorbed respectively
Kind cosmetic composition (organic and inorganic powder, moisturizing, surfactant, vitamin, bactericide), can effectively be reduced to skin
Excitant.
Although the method for preparing micropore starch at present is numerous, such as enzymatic isolation method, because its preparation process needs to add alphalise starch
Enzyme and amylo-transglucosidase, so need higher cost in industrial applications, the highly crystalline obtained in addition it is more
Hole starch easily collapses in use；Remaining method some causes industrial applications to receive necessarily because of preparation technology complexity
Limitation, the micropore starch that at present prepared by most methods in addition is all to be powdered, because it is not easy point in terms of wastewater treatment
It is difficult to carry out from recovery, limits its application.How to solve preparing the technical problem present in micropore starch at present, so as to
Develop the emphasis that the new technique for preparing micropore starch is research.
The micropore starch being prepared early stage and carbon disulfide are reacted in the basic conditions, obtain porous-starch xanthic acid
Ester, the absorption for heavy metal in waste water.Ative starch also has absorption property, and it is mainly by the chemical valence of surface atom group
Caused attraction is adsorbed, and this attraction is fainter, when the attraction in the external world gradually increases, quilt
Adsorbate will progressively disengage, therefore the absorption of ative starch is more fragile, be unable to reach the purpose of absorption.And the suction of porous-starch
Attached is that adsorption and hole adsorb coefficient result.Porous-starch is due to many apertures, and inner hollow, can
To produce huge attraction, absorbate can be adsorbed onto in aperture, than stronger, absorbate is not easy to take off for this absorption
From., can by modification because starch surface has been covered with hydrophilic hydroxyl, therefore to the limited sorption capacity of some oily matters
Further to improve the absorption property of porous-starch, expand adsorption range.
It is that raw material progress chemical modification prepares sorbing material for heavy metal suction using polysaccharide, microorganism, carbon material etc.
Attached example has a lot, such as using carbon material as raw material, is carried out to improve absorption property some using CNT and graphite
Modification prepares adsorbent, and it is present, and material therefor cost is higher, the reagent cost and building-up process used in addition in modifying process
In time cost, it is difficult to large-scale application.And raw material are modified the sample for heavy metal adsorption for microorganism
It is difficult to the adsorption time of the separation and needs length from waste water to be powdered, after absorption.Answered by raw material of cornstarch
Although closing the modified adsorbent adsorbance that obtains be better than this method, sample making course complexity, it is necessary to up to 12h adsorption time.Always
, although some sorbing material absorption properties are high, but material therefor cost be present in raw material and preparation process relatively in it
Time used in high, preparation technology complexity, absorption is longer and is difficult to solve the problems such as recycling.How the above is solved
The problem of each side, while ensure that higher absorption property is another research emphasis.
The content of the invention
In view of this, the invention be directed to it is a kind of it is easy to operate, the time is shorter, cost is relatively low, more homogeneity
Novel microporous chemical modification of starch preparation method, by this new material be used for heavy metal in waste water absorption.
To reach above-mentioned purpose, what the technical scheme of the invention was realized in：
A kind of novel microporous chemical modification of starch preparation method, its method and step are：
(1) it is gelatinized：Starch suspension is formed after a certain amount of starch (butt) is mixed with distilled water.By starch suspension
30min is heated under conditions of 100 DEG C, obtains the gelatinized corn starch of complete gelation.
Wherein, starch is mixed with distilled water by different proportion, the ratio (w/v)=1 of starch and water:2-1:9.
(2) bring back to life：After obtained gelatinized corn starch is cooled into room temperature, 1~10 day is refrigerated at 4 DEG C until forming gel knot
Structure, obtain starch hydrogel.
(3) freeze：After starch hydrogel is cut into the cube that the length of side is 1cm with mould 2 are freezed at -20 DEG C or -80 DEG C
My god, the water in starch hydrogel can build-up ice, and volumetric expansion separates out to form starch ice gel.
Starch hydrogel can be prepared into various shapes with mould, such as：It is disc-shaped, square shape, cube, spherical, round
Column etc..The present invention, which uses, is cut into cube of the length of side for 1cm, because it is beneficial to the ethanol dehydration in later stage, can be prepared into
The material arrived is more homogeneous, while simpler in terms of sign, is easier to separate in the heavy metal adsorption process in later stage.
(4) dehydrate：Starch ice gel is put into absolute ethyl alcohol and washed, is washed 3 times, every time 2 hours altogether.After dehydration
Obtained porous gel block dries 6h in 50 DEG C of baking ovens, finally obtains micropore starch.
The dosage of absolute ethyl alcohol is twice of distilled water volume used in step (1).
(5)CS2It is modified：Add 20mL 0.5%NaOH solution in centrifuge tube, add 1g micropore starch, slowly gradually
Add the CS of respective amount2, 1.5h is reacted under the conditions of 30 DEG C in magnetic agitation water-bath, it is each with distilled water and absolute ethyl alcohol rinse
3 times, 5h is dried in vacuo in 40 DEG C, obtains porous-starch xanthate.
The NaOH solution of low concentration weakens the interaction between starch molecule, accelerates micropore starch and CS2Reaction, high concentration
NaOH solution cause the dissolving of starch, therefore select 0.5%NaOH solution.Washing is the alkali for washing away residual after reaction terminates
Liquid, it is to wash away unreacted CS that alcohol, which is washed,2, because of CS2It is dissolved in ethanol.
It is used for heavy metal in waste water solution according to modified micropore starch porous-starch xanthate made from the inventive method
Absorption.
The advantages and positive effects of the present invention:
(1) in terms of micropore starch is prepared, this method has preparation technology relatively easy, and the chemical reagent used only has second
Alcohol, it is relatively green, while to be that bulk is different from traditional powdered for obtained material, in its absorption property of later-stage utilization
Field advantageously.
(2) because the present invention is that micropore starch has been connected into the xanthic acid ester group with chelating heavy metal ability, therefore, with
Simple native starch is compared with not modified micropore starch, and adsorbance significantly improves, and reaches 79mg/ to the maximal absorptive capacity of lead ion
g。
(3) present invention carries out chemical modification to it on the basis of micropore starch is prepared and obtains porous-starch xanthate,
It is applied to the absorption of heavy metal.The adsorbent of preparation has absorption is rapid (to inhale on the basis of certain adsorption effect is ensured
It is attached only to need 20min when reaching balance) the advantages of, while obtained sorbing material is bulk, it is not soluble in water so that adsorption reaction
Easily occur and be easy to recycling, there is no the advantages of secondary pollution, be easy to industrial applications.
(4) for the present invention in sorbing material whole process is prepared, the material and reagent cost used are relatively low, are readily available,
And chemical modification process is relatively easy, greatlys save time cost, good economic benefit can be produced.
Brief description of the drawings
Fig. 1-8 is the micropore starch electron microscope obtained under different in moisture content and different cryogenic temperatures
Fig. 1 is that the ratio of starch and water is 1：3, cryogenic temperature is -20 DEG C, and Fig. 2 is that the ratio of starch and water is 1：3, freezing temperature
Degree is -80 DEG C, and Fig. 3 is that the ratio of starch and water is 1：5, cryogenic temperature is -20 DEG C, and Fig. 4 is that the ratio of starch and water is 1：5, freezing
Temperature is -80 DEG C, and Fig. 5 is that the ratio of starch and water is 1：6.7, cryogenic temperature is -20 DEG C, and Fig. 6 is that the ratio of starch and water is 1：
6.7, cryogenic temperature is -80 DEG C, and Fig. 7 is that the ratio of starch and water is 1：8, cryogenic temperature is -20 DEG C, and Fig. 8 is the ratio of starch and water
For 1：8, cryogenic temperature is -80 DEG C；
Fig. 9-14 is different CS2With the porous-starch xanthate Electronic Speculum prepared under the mol ratio of starch glucose unit
Figure, mol ratio is respectively 1.34,1.61,1.88,2.15,2.42,2.69；
Figure 15 is PSX equilibrium adsorption ability and CS2With the mol ratio figure of starch glucose unit；
Figure 16 is adsorption time and CS2Dosage adsorbs Pb for PSX2+Influence figure；
Figure 17 is the adsorption dynamics adsorption kinetics figures of PSX 2.15；
Figure 18 is PSX 2.15 to Pb2+Adsorption isotherm line chart；
Figure 19 is PSX 2.15 Langmuir adsorption isothermal curve figures；
Embodiment
The specific embodiment for preparing novel microporous chemical modification of starch is：
First, gelatinization process
Weigh after a certain amount of starch (butt) mixes with distilled water and form starch suspension.By starch suspension 100
30min is heated under conditions of DEG C, obtains the gelatinized corn starch of complete gelation.The present embodiment selects common corn starch.Wherein, starch
Mixed with distilled water by different proportion, refer to table 1.
1 different starch of table and distilled water proportioning starch addition
2nd, retrogradation process
After obtained gelatinized corn starch is cooled into room temperature, 2 days are refrigerated at 4 DEG C until forming gel structure, obtains starch water
Gel.
The number of days of refrigeration depends on the species of starch, and common corn starch needs 2-3 days, and waxy corn starch needs 8-10
My god, amylomaize needs 1-2 days, and the time for refrigerating needs is to see that it forms the number of days of starch hydrogel.Several factors
Retrogradation process, such as crystal formation of amylose content, moisture, starch etc. in starch can be influenceed, because factors above can obtain
Different retrogradation effect, so can be impacted to the starch hydrogel of formation.
3rd, refrigerating process
1. starch hydrogel is cut into the cube that the length of side is 1cm with mould.
2. being freezed 2 days at -20 DEG C or -80 DEG C, the water in starch hydrogel can build-up ice, and volumetric expansion separates out to form starch
Ice gel.
4th, process is dehydrated
Starch ice gel is put into absolute ethyl alcohol and washed, is washed 3 times, every time 2 hours altogether.What is obtained after dehydration is porous solidifying
Blob of viscose dries 6h in 50 DEG C of baking ovens, finally obtains micropore starch.
Electron microscopes all Fig. 1-Fig. 8 is shot under identical multiplication factor, amplifies 200 times, thus can be direct
Compare pore size.As can be seen that the micropore starch aperture formed under different starch concentrations is differed, with starch from figure
The reduction of concentration is pasted, the ice crystal formed in gel is also gradually reduced by the constraint strength of starch molecule, washed with absolute ethyl alcohol
When, ethanol substitutes the ice crystal in different gels, can obtain the micropore starch that aperture gradually increases.In same moisture
Under, starch gel is freezed with -20 DEG C and -80 DEG C of two kinds of temperature respectively, because the water in starch gel can build-up ice, institute
Its quick-frozen speed can be influenceed with temperature, -80 DEG C, relative at -20 DEG C, there is faster cooldown rate, often prepare smaller
Crystal because without abundance time formed bulky grain, the relatively small micropore starch in aperture can be obtained.Wherein, with corn
Starch is raw material, is 1 in the ratio of starch and water：8, cryogenic temperature is that the micropore starch aperture prepared at -20 DEG C is about 52 μm,
Consider that the sample has more preferable structure and adsorptivity relative to other samples, therefore is selected as down from absorption property angle
The raw material of one step chemical modification.
5th, CS2Modifying process
1. adding 20mL 0.5%NaOH solution in centrifuge tube, 1g micropore starch is added, is slowly gradually added into corresponding
The CS of amount2(being shown in Table 2), react 1.5h under the conditions of 30 DEG C in magnetic agitation water-bath.
The CS of table 22To the different mol ratio of starch glucose unit
After 2. reaction terminates, each 3 times with distilled water and absolute ethyl alcohol rinse, 5h is dried in vacuo in 40 DEG C.
Electron microscopes all Fig. 9-Figure 14 is shot under identical multiplication factor, amplifies 200 times, so convenient to compare.
From scanning electron microscopic picture as can be seen that starch xanthate is in CS2It is more to all existing under different moles of starch glucose unit
Pore structure, even if under very high mol ratio, loose structure will not be also destroyed, but pore structure is slightly different.As starch is yellow
The formation of ortho acid ester group, obtained starch xanthate aperture ratio micropore starch slightly increase.With the increase of mol ratio, aperture
Gradually increase, PSX2.69 aperture is about 113 μm, and when mol ratio is 2.15, obvious thickening occurs in hole wall, it may be possible to
Because with the increase of mol ratio, the addition of more xanthic acid ester groups, the stability of loose structure is strengthened, makes it follow-up
It is more stable in reaction.
Porous-starch xanthate adsorbs Pb2+Specific embodiment be：
1. accurately weigh six kinds of different carbon disulfide (CS2) porous-starch xanthate (PSX) 0.02g of ratio is placed in
In 15mL centrifuge tubes, lead nitrate solution that 10mL plumbum ion concentrations are 500mg/L is taken to exist at room temperature in centrifuge tube with pipette
Rotating speed is fully to be adsorbed in 140RPM shaking table, and adsorption equilibrium is reached after 2h.After the completion of absorption, by the liquid in centrifuge tube
Filtered through filter membrane (0.45 μm of PES), be then 1 with volume ratio:After 499 salpeter solution dilutes 100 times, with Atomic absorption point
Light photometer detects its absorbance, and the Pb of raffinate is calculated according to standard curve2+Concentration.Each sample does three and parallel made even
Average.Obtain PSX equilibrium adsorption ability and CS2Relation between the mol ratio of starch glucose unit.
2. accurately weigh six kinds of different carbon disulfide (CS2) porous-starch xanthate (PSX) 0.02g of ratio is placed in
In 15mL centrifuge tubes, lead nitrate solution that 10mL plumbum ion concentrations are 500mg/L is taken to exist in centrifuge tube in room temperature with pipette
Rotating speed is to be adsorbed in 140RPM shaking table, and the raffinate of intervals is tested, and is obtained corresponding to different time points
Adsorbance (qt), so as to carry out adsorption dynamics adsorption kinetics analysis.
3. adsorption isotherm is to take Pb2+Concentration is 0.1-0.7g/L, and the concentration of adsorbent is 2g/L, and same rotating speed is
Fully adsorbed in 140RPM shaking table, adsorption equilibrium is reached after 2h, the Pb of raffinate is calculated after the filtered dilution of solution2+It is dense
Degree carries out isothermal adsorption analysis.
Figure 15 is PSX equilibrium adsorption ability and CS2With the mol ratio of starch glucose unit, CS2With starch glucose list
The mol ratio of member determines the quantity of the xanthic acid group on porous-starch wall, thus determines adsorbent when absorption reaches balance
Equilibrium adsorption capacity.PSX is to Pb2+Equilibrium adsorption capacity with CS2Increase to the mol ratio of starch glucose unit and increase.
Work as CS2When reaching 2.15 to the mol ratio of starch glucose unit, PSX is to Pb2+Absorption reach and be up to 74.83mg/g, and
Work as CS2After the further increase of mol ratio of starch glucose unit, equilibrium adsorption capacity remains constant substantially, i.e. CS2To starch Portugal
The mol ratio of grape sugar unit is 2.15,2.42, the equilibrium adsorption capacity of 2.69 3 kind of sample is not significantly different.Illustrate CS2Amount
Saturation may have been reached for porous-starch, then increased CS on the basis of this2To the mol ratio pair of starch glucose unit
Absorption there will not be obvious raising.In addition, what mol ratio reacted when being 0 is corn porous starch to Pb2+Absorption, be
2.00mg/g is very small.Because of CS2When mol ratio to starch glucose unit is 2.15, PSX equilibrium adsorption ability has reached
To maximum, and equilibrium adsorption ability does not significantly improve after increase mol ratio, therefore it is research object to use PSX 2.15, enters one
Step research PSX adsorption process and mechanism.
Figure 16 reactions are adsorption time and CS2Dosage adsorbs Pb for PSX2+Influence.As can be seen that initial
10min absorption is an adsorption process quickly, followed by a slow adsorption process (10min-20min), Zhi Daoda
To adsorption equilibrium.
Figure 17 carries out adsorption dynamics adsorption kinetics analysis, PSX 2.15 t/q using pseudo-second order kinetic model to PSXtWith when
Between curve linear obtained by t it is fine, coefficient correlation is close to 1.It can show that PSX 2.15 adsorption process meets well
Quasi- secondary absorption model.Illustrate that chemisorbed occupies mainly.Relevant parameter is shown in Table 3.
The pseudo-second order kinetic parameter of table 3
Figure 18 is PSX 2.15 to Pb2+Adsorption isotherm.As starting adsorption concentration (C0) than it is relatively low when, equilibrium adsorption capacity
(qe) increase it is very fast, work as C0For 300mg/L when, qe increase become slow, until C0Qe is maintained constant substantially during=400mg/L,
No longer change.Work as C0During=400mg/L, qe=75mg/g.
Figure 19 is PSX Langmuir adsorption isothermal curves.Relevant parameter is shown in Table 4.PSX isothermal adsorptions perfectly agree with
Langmuir isotherm adsorption models, R2It is in close proximity to 1.Also demonstrate that PSX to Pb simultaneously2+Absorption be mono layer adsorption.By
Table 4 understands that PSX2.15 is to Pb2+Maximum monolayer adsorption amount be 79.1766mg/g.
The Langmuir isotherm adsorption model parameters of table 4
The section Example of the invention is the foregoing is only, is not intended to limit the invention creation, it is all at this
Within the spirit and principle of innovation and creation, any modification, equivalent substitution and improvements made etc. should be included in the invention
Within protection domain.
Claims (4)
1. a kind of preparation method of novel microporous starch, it is characterised in that comprise the following steps：
(1) it is gelatinized：Starch suspension is formed after starch is mixed with distilled water, starch suspension is added under conditions of 100 DEG C
Hot 30min, obtain the gelatinized corn starch of complete gelation；
(2) bring back to life：After obtained gelatinized corn starch is cooled into room temperature, 1~10 day is refrigerated at 4 DEG C until forming gel structure, is obtained
To starch hydrogel；
(3) freeze：Freeze 2 days, form sediment at -20 DEG C or -80 DEG C after starch hydrogel is cut into the cube that the length of side is 1cm with mould
Water in flour hydrogel can build-up ice, and volumetric expansion separates out to form starch ice gel；
(4) dehydrate：Starch ice gel is put into absolute ethyl alcohol and washed, washs 3 times, 2 hours every time, is obtained after dehydration altogether
Porous gel block in 50 DEG C of baking ovens dry 6h, finally obtain micropore starch；
(5)CS2It is modified：Add 20mL 0.5%NaOH solution in centrifuge tube, add 1g micropore starch, be slowly gradually added into
CS2, 1.5h is reacted under the conditions of 30 DEG C in magnetic agitation water-bath, it is true in 40 DEG C each 3 times with distilled water and absolute ethyl alcohol rinse
Sky dries 5h, obtains porous-starch xanthate.
A kind of 2. preparation method of novel microporous starch according to claim 1, it is characterised in that step (1) starch with
Distilled water is mixed by different proportion, the ratio (w/v)=1 of starch and water:2-1:9.
A kind of 3. preparation method of novel microporous starch according to claim 1, it is characterised in that step (5) CS2Plus
It is 0.5-1.0mL to enter amount.
A kind of 4. preparation method of novel microporous starch described in claim 1, it is characterised in that obtained porous-starch xanthan
Acid esters is used for the absorption of heavy metal in waste water solution.
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Cited By (5)
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| CN108841014A (en) * | 2018-06-29 | 2018-11-20 | 青岛农业大学 | A kind of preparation method of starch nano hydrogel |
| CN109054076A (en) * | 2018-09-10 | 2018-12-21 | 齐鲁工业大学 | The preparation method and products obtained therefrom of a kind of three-dimensional porous modified starch and application |
| WO2021077290A1 (en) * | 2019-10-22 | 2021-04-29 | 浙江大学 | Nanopore starch-based adsorbent and preparation method therefor |
| CN115226777A (en) * | 2022-07-13 | 2022-10-25 | 无锡沃莱特生物新材料科技有限公司 | Preparation method of microcapsule powder butter with porous starch as carrier |
| CN117003221A (en) * | 2023-08-21 | 2023-11-07 | 河北省科学院能源研究所 | Preparation method of carbon aerogel |
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| CN117003221A (en) * | 2023-08-21 | 2023-11-07 | 河北省科学院能源研究所 | Preparation method of carbon aerogel |
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