CN110028593A - A kind of cationic glutinous rice starch flocculant and its preparation method and application for microalgae harvesting - Google Patents
A kind of cationic glutinous rice starch flocculant and its preparation method and application for microalgae harvesting Download PDFInfo
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- CN110028593A CN110028593A CN201910195808.2A CN201910195808A CN110028593A CN 110028593 A CN110028593 A CN 110028593A CN 201910195808 A CN201910195808 A CN 201910195808A CN 110028593 A CN110028593 A CN 110028593A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/003—Crosslinking of starch
- C08B31/006—Crosslinking of derivatives of starch
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
- C08B31/08—Ethers
- C08B31/12—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch
- C08B31/125—Ethers having alkyl or cycloalkyl radicals substituted by heteroatoms, e.g. hydroxyalkyl or carboxyalkyl starch having a substituent containing at least one nitrogen atom, e.g. cationic starch
Abstract
A kind of preparation method of the cationic glutinous rice starch flocculant for microalgae harvesting: the glutinous rice starch of 3g parts by weight is mixed with the NaCl of 1.2~1.8g parts by weight, it is put into the ice state potassium hydroxide solution that 1.2~6g parts by weight concentration is 0.1~0.3wt%, is stirred at room temperature 5~20 minutes；1~2 parts by weight GTA is added, is stirred at room temperature 0.75~1.25 hour, 20~60 DEG C of water-baths are shaken 1~3 hour；The adipic acid of 0.09~0.15 parts by weight is added, is stirred at room temperature 15~40 minutes, is then shaken 60~100 minutes in 20~25 DEG C of water-baths；Then the ethyl alcohol that 3~15 parts by weight are added precipitates product, filters, and washs, dry.The cross-linked cationic glutinous rice starch flocculant recovery ratio of this method preparation can reach 100%, and preparation method simple process, and the reaction time is shorter, and reaction efficiency is high, non-environmental-pollution.
Description
Technical field
The present invention relates to the cationic glutinous rice starch flocculant and preparation method thereof for microalgae harvesting, belong to flocculant and
Microalgae recovery technical field.
Background technique
Microalgae is the quasi-microorganism that nature is widely present, and is the important original of biomass energy, biological-based chemicals etc.
Expect source, in recent years hot spot always concerned by people.During microalgae utilizes, microalgae harvesting is crucial processing step
Suddenly.It is often time-consuming and laborious using conventional solid-liquid separation means because microalgae frond partial size is smaller, increase microalgae frond recycling at
This.The method for collecting microalgae at present has: centrifugal process, freeze-drying, flocculant method etc..Centrifugal process and freeze-drying all compare
Compared with consumption energy, in contrast energy consumption is big.Therefore the flocculant of function admirable can more efficiently collect microalgae, give subsequent work
Provide great convenience.Being often used Cross-linking Cationic Starch in document report in recent years, (such as: cross-linked cationic corn forms sediment
Powder, potato starch, tapioca etc.) it is used as flocculant.Starch is a kind of people with extensive and resourceful resource substance,
It selects starch as raw material, cost can be reduced.Existing literature is shown, is the wadding of raw material using cornstarch and potato starch
Solidifying agent is most commonly seen, but because its flocculating effect is undesirable, limits its application range.
Starch is a kind of high glycan substance, and starch molecule is to exist in plant in the form of white solid amylum body, is formed sediment
Powder is the aggregation of starch molecule, it is made of amylose, amylopectin and osculant polysaccharide.The straight chain of glutinous rice starch forms sediment
Powder structure is relatively fewer, is largely that intergrade and amylopectin are constituted.The weight average molecular weight of glutinous rice amylopectin be 8.96 ×
107G/mol~7.96 × 109g/mol。
Cationic starch is that starch reacts generation, different location in amino therein and starch molecule with aminated compounds
Hydroxyl etherification reaction occurs, make starch molecule with tertiary amino or quaternary ammonium group, be a kind of ether derivant, molecule is taken after replacing
Band has the nitrogen-atoms of positive charge, the positive electricity with the property that common starch molecule does not have, in cationic starch molecule
Lotus can neutralize with the substance for carrying negative electrical charge, and the phenomenon that adsorbing negatively charged substance, referred to as cationic starch is presented.
Starch reacts with the chemical reagent with two or more functional groups, forms ether between the hydroxyl of different starch molecules
Change or be esterified key and be crosslinked, resulting derivative is known as crosslinked starch.A kind of most important be denaturalized is exactly in converted starch
Crosslinked starch.The derivative of so-called starch is exactly to carry out cross-linking reaction with the means of crosslinking agent and starch crosslinking, so that two
Or the bridge formation carried out between above starch molecule.The viscosity of starch is not very high, but the viscosity of the starch after being crosslinked
It is more higher than starch viscosity before.
When the Cross-linking Cationic Starch developed at present carries out microalgae recovery as flocculant, it is lower that there are recovery ratios
Problem.Therefore, the preparation process and recovery process of optimization Cross-linking Cationic Starch are needed, efficiently separates, harvest to reach
Purpose.
Summary of the invention
In view of the above problems in the prior art, the present invention provide it is a kind of can improve microalgae recovery efficiency it is cross-linking modified sun from
Sub- glutinous rice starch flocculant and preparation method thereof.
To achieve the above object, the present invention includes following technical solution:
A kind of preparation method of the cationic glutinous rice starch flocculant for microalgae harvesting, this method comprises the following steps:
I. the glutinous rice starch of 3 parts by weight is uniformly mixed with the NaCl of 1.2~1.8 parts by weight, is put into 1.2~6 parts by weight
Concentration is to be stirred at room temperature 5~20 minutes in the ice state potassium hydroxide solution or ice state sodium hydroxide solution of 0.1~0.3wt%；Add
Enter 1~2 parts by weight N- epoxypropyltrimethylchloride chloride, is stirred at room temperature 0.75~1.25 hour, 40~60 DEG C of water-bath concussions 1~
3 hours；
II. the adipic acid of 0.06~0.15 parts by weight is added in the mixture obtained to step I, is stirred at room temperature 15~40 points
Then clock shakes 60~100 minutes in 20~25 DEG C of water-baths；
III. the ethyl alcohol of the acetic acid Han 10~20wt% is added in the mixture obtained to step II, impregnates 15~30 minutes,
It filters, washing, it is dry to get cationic starch flocculant.
Preparation method as described above, it is preferable that the glutinous rice starch the preparation method comprises the following steps: according to solid-to-liquid ratio be 1g:
0.085mol/L aqueous slkali is added into glutinous rice flour by 5mL, and under conditions of 40 DEG C, agitating and heating 3h, centrifugation, separation lower layer sinks
It forms sediment, washing is dried to get glutinous rice starch.
Preparation method as described above, it is preferable that the concrete operations of step I are as follows: by the glutinous rice starch of 3 parts by weight and 1.8
The NaCl of parts by weight is uniformly mixed, and is put into the ice state potassium hydroxide aqueous solution that 1.6 parts by weight concentration are 0.3wt%, room temperature is stirred
It mixes 5 minutes；1.8 parts by weight N- epoxypropyltrimethylchloride chlorides are added, are stirred at room temperature 1 hour, 50 DEG C of water-baths are shaken 1 hour.
Preparation method as described above, it is preferable that the concrete operations of step II are as follows: add in the mixture obtained to step I
The adipic acid for entering 0.06 parts by weight is stirred at room temperature 25 minutes, then shakes 100 minutes in 20 DEG C of water-baths；
Preparation method as described above, it is preferable that the concrete operations of step III are as follows: in the mixture obtained to step II
The ethyl alcohol of the acetic acid containing 10-20wt% of 3 parts by weight is added, impregnates 30 minutes, filters, washing is dry to get cationic starch wadding
Solidifying agent.
On the other hand, the present invention provides a kind of cationic starch flocculant, is prepared using method as described above.
Another aspect, the present invention provide a kind of microalgae flocculating setting harvesting method, are using cation as described above
Starch flocculant carries out microalgae flocculating setting harvest.
Harvesting method as described above, it is preferable that this method comprises the following steps:
A. microalgae density in culture solution is measured；
B. flocculant as claimed in claim 6 is added into the solution containing microalgae under stirring, flocculant usage is microalgae
The 5~15% of dry weight are shaken 30 seconds~1 minute；
C. it settles 15~30 minutes, microalgae is deposited to flocculation container bottom after flocculation；
D. algal gel is collected after flocculating, and is dehydrated, dry.
Harvesting method as described above, it is preferable that the step A further includes that the concentration of microalgae in culture solution is adjusted to dry
Weigh 0.5~1 grams per liter.
Harvesting method as described above, it is preferable that this method comprises the following steps:
A. microalgae density in culture solution is measured, the concentration of microalgae in culture solution is adjusted to 1 grams per liter of dry weight；
B. flocculant as claimed in claim 6 is added into the solution containing microalgae under stirring, flocculant usage is microalgae
The 1-10% of dry weight shakes 1 minute；
C. it settles 30 minutes, microalgae is deposited to flocculation container bottom after flocculation；
D. algal gel is collected after flocculating, and is dehydrated, dry.
Crosslinking agent used in the present invention is adipic acid, wherein there is difunctional in the molecule of adipic acid, two
With the glutinous rice starch of the hydroxyl contained esterification can occur for carboxyl, generate the glutinous rice starch of crosslinking, and this reaction is esterification
Crosslinking.Reaction equation are as follows:
2Str-OH+HOOC(CH2)4COOH→Str-O-OC(CH2)4CO-O-Str+2H2O
The beneficial effects of the present invention are: it is raw material that the present invention, which selects glutinous rice starch, with GTA (N- epoxy
Ammonium chloride) it is used as cationic reagent, adipic acid is crosslinking agent, prepares cross-linked cationic glutinous rice starch flocculant, has studied
The relevance of the degree ofacationic substitution of flocculant, the degree of cross linking and microalgae recovery effect prepares the crosslinking sun of efficient harvesting microalgae
Ionic flocculant, recovery ratio can reach 100%.Compared with existing potato starch and corn starch flocculant, glutinous rice forms sediment
Powder amylopectin content is high, it is easier to form flocculation harvest bridge formation process, settle convenient for microalgae harvesting, reduce flocculant and use
Amount improves yield rate.And the preparation method simple process, the reaction time is shorter, and reaction efficiency is high, non-environmental-pollution.
Detailed description of the invention
Fig. 1 is the infrared spectrogram of 1 product of embodiment.
Fig. 2 is flocculant addition-microalgae harvesting rate curve in embodiment 4.
Specific embodiment
The experimental raw of following embodiment:
(1) glutinous rice starch
It is prepared as follows: according to solid-liquid (glutinous rice flour/water) than being 1g: 5mL, being added into glutinous rice flour
0.085mol/L aqueous slkali, under conditions of 40 DEG C, agitating and heating 3h takes out beaker, liquid is poured into centrifugation after reaction
Guan Zhong, centrifugation time 5min, speed are 3500r/min, outwell supernatant after centrifugation, and distilled water is added and carries out second
Supernatant is outwelled in secondary centrifugation after taking-up, lower sediment is glutinous rice starch, is put into baking oven and is dried.It is taken out after drying,
It grinds, fills sealed bag, it is spare.
(2) microalgae: chlorella.
Embodiment 1: cross-linked cationic glutinous rice starch flocculant (one) is prepared
3g glutinous rice starch is weighed, 1.8g NaCl is added, is stirred evenly with glass bar, 1.6g concentration is added later is
The ice state KOH aqueous solution of 0.3wt% stirs 10min at room temperature, and 1.8g N- epoxypropyl trimethylammonium chloride is added
Ammonium (GTA) cationic reagent, stirs 1h at room temperature, is put into 50 DEG C of thermostatic water bath vibrator, concussion reaction
1.5h is added the adipic acid of 0.06g, 25min is sufficiently stirred, is put into 20 DEG C of thermostatic control oscillator vibration and reacts after taking-up
100min.After taking-up, 30min is impregnated with the ethyl alcohol containing 20wt% acetic acid prepared, is filtered, drying is ground, as with mortar
Product.
The infrared spectroscopy of product is as shown in Figure 1, visible in 917.24cm in figure-1, 1026.89cm-1, 1082.52cm-1Place
There are absorption peak, absorption peak is-C-O-C- key.In 1649.92cm-1What place had that absorption peak illustrates is in molecule containing-C=O key,
It can prove that esterification has occurred in the alcoholic extract hydroxyl group in glutinous rice starch with the carboxyl inside adipic acid, have suction at 1474.05
Receiving peak is-C-N, can illustrate that etherification reaction has occurred in glutinous rice starch.
Embodiment 2: cross-linked cationic glutinous rice starch flocculant (two) is prepared
3g glutinous rice starch is weighed, 1.2g NaCl is added, is stirred evenly with glass bar, 1.4g concentration is added later is
The ice state KOH aqueous solution of 0.3wt% stirs 5min at room temperature, and 1g N- epoxypropyltrimethylchloride chloride is added
(GTA) cationic reagent stirs 0.75h at room temperature, is put into 40 DEG C of thermostatic water bath vibrator, concussion reaction
1h is added the adipic acid of 0.09g, 15min is sufficiently stirred, is put into 20 DEG C of thermostatic control oscillator vibration and reacts 60min after taking-up.
After taking-up, 15min is impregnated with the ethyl alcohol containing 10wt% acetic acid prepared, is filtered, drying is ground, as product with mortar.
Embodiment 3: cross-linked cationic glutinous rice starch flocculant (three) is prepared
3g glutinous rice starch is weighed, 1.5g NaCl is added, is stirred evenly with glass bar, 2.0g concentration is added later is
The ice state KOH aqueous solution of 0.3wt% stirs 20min at room temperature, and 2g N- epoxypropyltrimethylchloride chloride is added
(GTA) cationic reagent stirs 1.25h at room temperature, is put into 60 DEG C of thermostatic water bath vibrator, concussion reaction
3, the adipic acid of 0.15g is added after taking-up, 40min is sufficiently stirred, is put into 20 DEG C of thermostatic control oscillator vibration and reacts 80min.
After taking-up, 20min is impregnated with the ethyl alcohol containing 20wt% acetic acid prepared, is filtered, drying is ground, as product with mortar.
The experiment of 4 harvesting microalgae of embodiment
(1) microdisk electrode
The 1000mL BG-11 culture medium prepared is dispensed into the conical flask of two 1000mL, mouth is sealed with sealing film,
It is put into autoclave and sterilizes.It is put into super-clean bench, opens ultraviolet light irradiation 20min, after waiting BG-11 culture medium cooling, inoculation
The algae of chlorella, inoculum concentration are every bottle of 10ml.It is finally putting into illumination box and is cultivated.After 2 weeks, by the bead of culture
Algae is placed on shaking table and continues to cultivate.
(2) by microalgae liquid H2O is diluted to 1g (dry weight)/L.
(3) water is added to be configured to 1g/L flocculant solution flocculant prepared by Examples 1 to 3.
(4) three kinds of flocculant solutions take 1mL, 2mL, 3mL, 4mL, 5mL, 6mL to be added in the algae solution of 30mL respectively, concussion
30min is stood after 1min.
(5) part among supernatant is taken to measure absorbance.
(6) effect is harvested
Flocculant harvesting result prepared by embodiment 1 is as shown in Fig. 2, the yield rate that 3mL flocculant solution is added is
93.4%, the yield rate that 5mL flocculant solution is added is 100%.
The yield rate that flocculant solution prepared by 3mL embodiment 2 is added is 90.6%, and the receipts of 5mL flocculant solution are added
Obtaining rate is 100%.
The yield rate that flocculant solution prepared by 3mL embodiment 3 is added is 91.8%, and the receipts of 5mL flocculant solution are added
Obtaining rate is 100%.
Claims (10)
1. a kind of preparation method of the cationic glutinous rice starch flocculant for microalgae harvesting, which is characterized in that this method includes
Following steps:
I. the glutinous rice starch of 3 parts by weight is uniformly mixed with the NaCl of 1.2~1.8 parts by weight, is put into 1.2~6 parts by weight concentration
To be stirred at room temperature 5~20 minutes in the ice state potassium hydroxide solution or ice state sodium hydroxide solution of 0.1~0.3wt%；It is added 1
~2 parts by weight N- epoxypropyltrimethylchloride chlorides are stirred at room temperature 0.75~1.25 hour, and 40~60 DEG C of water-bath concussions 1~3 are small
When；
II. the adipic acid of 0.06~0.15 parts by weight is added in the mixture obtained to step I, is stirred at room temperature 15~40 minutes,
Then it is shaken 60~100 minutes in 20~25 DEG C of water-baths；
III. the ethyl alcohol of the acetic acid Han 10~20wt% is added in the mixture obtained to step II, impregnates 15~30 minutes, filters,
Washing, it is dry to get cationic starch flocculant.
2. preparation method as described in claim 1, which is characterized in that the glutinous rice starch the preparation method comprises the following steps: according to solid-liquid
Than for 1g:5mL, the addition 0.085mol/L aqueous slkali into glutinous rice flour, under conditions of 40 DEG C, agitating and heating 3h is centrifuged, separation
Lower sediment, washing are dried to get glutinous rice starch.
3. preparation method as claimed in claim 1 or 2, which is characterized in that the concrete operations of step I are as follows: by the glutinous of 3 parts by weight
Rice starch is uniformly mixed with the NaCl of 1.8 parts by weight, and it is water-soluble to be put into the ice state potassium hydroxide that 1.6 parts by weight concentration are 0.3wt%
In liquid, it is stirred at room temperature 5 minutes；1.8 parts by weight N- epoxypropyltrimethylchloride chlorides are added, are stirred at room temperature 1 hour, 50 DEG C of water-baths
Concussion 1 hour.
4. preparation method as claimed in claim 1 or 2, which is characterized in that the concrete operations of step II are as follows: obtained to step I
Mixture in the adipic acids of 0.06 parts by weight is added, be stirred at room temperature 25 minutes, then shaken 100 minutes in 20 DEG C of water-baths.
5. preparation method as claimed in claim 1 or 2, which is characterized in that the concrete operations of step III are as follows: obtained to step II
Mixture in be added 3 parts by weight the acetic acid containing 10-20wt% ethyl alcohol, impregnate 30 minutes, filter, washing, it is dry to get
Cationic starch flocculant.
6. a kind of cationic starch flocculant, which is characterized in that it is using method according to any one of claims 1 to 5
Preparation.
7. a kind of microalgae flocculating setting harvesting method, which is characterized in that it is using cationic starch as claimed in claim 6
Flocculant carries out microalgae flocculating setting harvest.
8. harvesting method as claimed in claim 7, which is characterized in that this method comprises the following steps:
A. microalgae density in culture solution is measured；
B. flocculant as claimed in claim 6 is added into the solution containing microalgae under stirring, flocculant usage is microalgae dry weight
5~15%, shake 30 seconds~1 minute；
C. it settles 15~30 minutes, microalgae is deposited to flocculation container bottom after flocculation；
D. algal gel is collected after flocculating, and is dehydrated, dry.
9. harvesting method as claimed in claim 6, which is characterized in that the step A further include by culture solution microalgae it is dense
Degree is adjusted to 0.5~1 grams per liter of dry weight.
10. harvesting method as claimed in claim 9, which is characterized in that this method comprises the following steps:
A. microalgae density in culture solution is measured, the concentration of microalgae in culture solution is adjusted to 1 grams per liter of dry weight；
B. flocculant as claimed in claim 6 is added into the solution containing microalgae under stirring, flocculant usage is microalgae dry weight
1-10%, shake 1 minute；
C. it settles 30 minutes, microalgae is deposited to flocculation container bottom after flocculation；
D. algal gel is collected after flocculating, and is dehydrated, dry.
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Cited By (4)
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| CN110642357A (en) * | 2019-10-31 | 2020-01-03 | 内江师范学院 | Flocculating agent for microalgae capture and preparation method and application thereof |
| CN110698566A (en) * | 2019-10-31 | 2020-01-17 | 内江师范学院 | Flocculating agent for microalgae capture and preparation method and application thereof |
| CN111534437A (en) * | 2020-03-31 | 2020-08-14 | 厦门大学 | Preparation method of dry porphyridium powder |
| CN113322186A (en) * | 2021-06-21 | 2021-08-31 | 昆明理工大学 | Method for rapidly harvesting microalgae by using ionic liquid |
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| CN113322186A (en) * | 2021-06-21 | 2021-08-31 | 昆明理工大学 | Method for rapidly harvesting microalgae by using ionic liquid |
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