CN106589145A - Bi-crosslinking cassava starch chelating agent and preparation method thereof - Google Patents
Bi-crosslinking cassava starch chelating agent and preparation method thereof Download PDFInfo
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- CN106589145A CN106589145A CN201611196665.XA CN201611196665A CN106589145A CN 106589145 A CN106589145 A CN 106589145A CN 201611196665 A CN201611196665 A CN 201611196665A CN 106589145 A CN106589145 A CN 106589145A
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- Prior art keywords
- starch
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- cassava starch
- crosslinking
- chelating agen
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
- B01J20/267—Cross-linked polymers
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/26—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof
- C02F2103/28—Nature of the water, waste water, sewage or sludge to be treated from the processing of plants or parts thereof from the paper or cellulose industry
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a bi-crosslinking cassava starch chelating agent and a preparation method thereof. The bi-crosslinking cassava starch chelating agent is prepared by the following steps: carrying out etherifying modification on the basis of crosslinking cassava starch, and then taking carbon disulfide as a crosslinking agent to finally prepare a metal ion chelating agent with a bi-crosslinking structure. The bi-crosslinking cassava starch chelating agent prepared based on the method is relatively high in chelating capacity for ions such as Cr<2+>, Cu<2+> and Ni<2+>, has the advantages of low production cost, simplicity in operation and the like, and has a potential application value in the field of water treatment and the like.
Description
Technical field
The present invention relates to environmental conservation and water treatment field, and in particular to a kind of pair of crosslinked cassava starch chelating agen and its system
Preparation Method.
Background technology
New Wastewater processing absorbent is developed using modified starch, water purification quality and reduces cost not only can be improved, and
And China is large agricultural country, starch yield is at the forefront in the world, with starch derivatives production wastewater treatment adsorbent, is conducive to starch
The development of deep processing, takes full advantage of the starch resource of China again.
The present invention adopts tapioca for raw material, first which is carried out etherification modified, obtains crosslinking etherified starch, then with
Based on this, further it is crosslinked by Carbon bisulfide, obtains a kind of adsorption of metal ions performance more preferably chelating agen.This kind of chelating
Agent has raw material sources wide, and low cost and other advantages have using value in fields such as pulping wastewater treatments.
The content of the invention
The invention provides a kind of raw material sources are wide, the more preferably double crosslinked cassava starch chelatings of low cost, absorption property
Agent and preparation method thereof.
For achieving the above object, the present invention is employed the following technical solutions：
The first aspect of the invention is to provide the preparation method of a kind of pair of crosslinked cassava starch chelating agen, including following step
Suddenly：
(1) crosslinked cassava starch is carried out it is etherification modified, by tapioca disperse in ethanol, add tapioca quality
5～10% NaOH and the etherifying agent of tapioca quality 10～50%, react 2～6 hours under the conditions of 40～60 DEG C, point
It is standby after drying；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；Slowly
Deca 0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, and 1-3h is reacted in 45-55 DEG C of water-bath, takes out, adds
0.1g/mL Adlerikas, continue reaction 10-20min；
(3), after reaction stops, washing, sucking filtration are washed 2-4 time with acetone, ether afterwards successively；
(4), and then after vacuum drying, double crosslinked cassava starch chelating agen are obtained final product.
Further, in the step (1), crosslinked cassava starch is epoxychloropropane crosslinked starch, and 200 mesh sieving rates are big
In 95%.
Further, the etherifying agent be 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, active substance in the tapioca
Content is 60～70%.
Further, according to the mass fraction, in the step (2), each reactant consumption proportion is as follows：
Preferably, according to the mass fraction, in the step (2), each reactant consumption proportion is as follows：
It is highly preferred that according to the mass fraction, in the step (2), each reactant consumption proportion is as follows：
Further, the reaction temperature in the step (2) in water-bath is 48-52 DEG C of reaction 2h.Preferably, institute
State the reaction 2h that the reaction temperature in step (2) in water-bath is 50 DEG C.
The second aspect of the invention aspect is to provide a kind of such as the double crosslinked cassava starch prepared using said method
Chelating agen.
The third aspect of the invention is to provide a kind of described double crosslinked cassava starch chelating agen in pulping wastewater treatment
In application.
The present invention adopts above-mentioned technical proposal, compared with prior art, has the following technical effect that：
Obtained in the inventive method, double crosslinked cassava starch chelating agen, adopt tapioca for raw material, first which are carried out
It is etherification modified, crosslinking etherified starch is obtained, then based on this, is further crosslinked by Carbon bisulfide, obtain a kind of metal
Ionic adsorption performance more preferably chelating agen.This quasi-chelate compound has raw material sources wide, low cost and other advantages, at paper waste
The fields such as reason have using value.
Description of the drawings
Fig. 1 is the schematic diagram of complexation of metal ions content in a kind of pair of crosslinked cassava starch chelating agen of the invention.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1 prepares double crosslinked cassava starch chelating agen, comprises the following steps that：
(1) tapioca is carried out it is etherification modified, by starch dispersion in ethanol, add starch quality 8% NaOH with
And the etherifying agent of starch quality 24%, react 5 hours under the conditions of 50 DEG C, separate standby after being dried；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；Slowly
Deca 0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, in 50 DEG C of water-bath reacts 2h；Taking-up adds 0.1g/mL
Adlerika, continues reaction 15min；Wherein, by mass, ratio is as follows for each reactant of this step：
(3), after reaction stops, washing, sucking filtration wash 2 times with acetone, ether afterwards successively；
And then vacuum drying obtains double crosslinked cassava starch chelating agen (4).
Embodiment 2 prepares double crosslinked cassava starch chelating agen, comprises the following steps that：
(1) tapioca is carried out it is etherification modified, by starch dispersion in ethanol, add starch quality 8% NaOH with
And the etherifying agent of starch quality 24%, react 5 hours under the conditions of 50 DEG C, separate standby after being dried；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；Slowly
Deca 0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, in 50 DEG C of water-bath reacts 2h；Taking-up adds 0.1g/mL
Adlerika, continues reaction 15min；Wherein, by mass, ratio is as follows for each reactant of this step：
(3), after reaction stops, washing, sucking filtration wash 2 times with acetone, ether afterwards successively；
And then vacuum drying obtains double crosslinked cassava starch chelating agen (4).
Embodiment 3 prepares double crosslinked cassava starch chelating agen, comprises the following steps that：
(1) tapioca is carried out it is etherification modified, by starch dispersion in ethanol, add starch quality 8% NaOH with
And the etherifying agent of starch quality 24%, react 5 hours under the conditions of 50 DEG C, separate standby after being dried；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；Slowly
Deca 0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, in 50 DEG C of water-bath reacts 2h；Taking-up adds 0.1g/mL
Adlerika, continues reaction 15min；Wherein, by mass, ratio is as follows for each reactant of this step：
(3), after reaction stops, washing, sucking filtration wash 2 times with acetone, ether afterwards successively.
And then vacuum drying obtains double crosslinked cassava starch chelating agen (4).
Embodiment 4 prepares double crosslinked cassava starch chelating agen, comprises the following steps that：
(1) tapioca is carried out it is etherification modified, by starch dispersion in ethanol, add starch quality 8% NaOH with
And the etherifying agent of starch quality 24%, react 5 hours under the conditions of 50 DEG C, separate standby after being dried；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；Slowly
Deca 0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, in 50 DEG C of water-bath reacts 2h；Taking-up adds 0.1g/mL
Adlerika, continues reaction 15min；Wherein, by mass, ratio is as follows for each reactant of this step：
(3), after reaction stops, washing, sucking filtration wash 2 times with acetone, ether afterwards successively；
And then vacuum drying obtains double crosslinked cassava starch chelating agen (4).
Relative analyses：
With double crosslinked cassava starch chelating agen obtained in above-described embodiment 1-4 as test example；With amphoteric starch chelating agen it is
Control sample, configuration quality concentration are 0.03% Cr2+Solution, 0.002% Cu2+Solution, 0.006% Ni2+Solion,
Fixing metal ions/chelating agen mass ratio is 0.10, adds chelating agen, places shaking table constant temperature oscillation, is taken after a period of time
Go out, centrifugation, obtain the supernatant as a comparison case；Respectively determine supernatant in ion concentration, calculate complexing metal from
Sub- content, as a result measurement result as shown in figure 1, show, the chelating agen of the present invention is substantially better than comparative example.
Above the specific embodiment of the present invention is described in detail, but which has been intended only as example, the present invention has not been limited
It is formed on particular embodiments described above.To those skilled in the art, any equivalent modifications carried out by the present invention and
Replacement is also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, should all cover within the scope of the invention.
Claims (8)
1. the preparation method of a kind of pair of crosslinked cassava starch chelating agen, it is characterised in that comprise the steps：
(1) crosslinked cassava starch is carried out it is etherification modified, by tapioca disperse in ethanol, add tapioca quality 5～
10% NaOH and the etherifying agent of tapioca quality 10～50%, react 2～6 hours under the conditions of 40～60 DEG C, separate
It is standby after drying；
(2) a certain amount of crosslinking etherified starch is accurately weighed, makes the starch milk that quality is 20%, stir；It is slowly added dropwise
0.2g/mL sodium hydroxide, is subsequently adding Carbon bisulfide, and 1-3h is reacted in 45-55 DEG C of water-bath, takes out, adds 0.1g/
ML Adlerikas, continue reaction 10-20min；
(3), after reaction stops, washing, sucking filtration are washed 2-4 time with acetone, ether afterwards successively；
(4), and then after vacuum drying, double crosslinked cassava starch chelating agen are obtained final product.
2. preparation method according to claim 1, it is characterised in that crosslinked cassava starch is epoxy in the step (1)
Chloropropane crosslinked starch, 200 mesh sieving rates are more than 95%.
3. preparation method according to claim 1, it is characterised in that etherifying agent is the chloro- 2- hydroxypropyls of 3- in the step (1)
Base trimethyl ammonium chloride, in the tapioca, activity substance content is 60～70%.
4. preparation method according to claim 1, it is characterised in that according to the mass fraction, respectively react in the step (2)
Thing consumption proportion is as follows：
5. preparation method according to claim 4, it is characterised in that according to the mass fraction, respectively react in the step (2)
Thing consumption proportion is as follows：
6. preparation method according to claim 1, it is characterised in that the reaction temperature in the step (2) in water-bath
Spend the reaction 2h for 48-52 DEG C.
7. a kind of such as double crosslinked cassava starch chelating agen of any one of claim 1-6 methods described preparation.
8. application of a kind of as claimed in claim 7 pair of crosslinked cassava starch chelating agen in pulping wastewater treatment.
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| CN201611196665.XA CN106589145A (en) | 2016-12-22 | 2016-12-22 | Bi-crosslinking cassava starch chelating agent and preparation method thereof |
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| CN201611196665.XA CN106589145A (en) | 2016-12-22 | 2016-12-22 | Bi-crosslinking cassava starch chelating agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084283A (en) * | 2017-12-19 | 2018-05-29 | 东莞东美食品有限公司 | A kind of crosslinked starch and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| US3979286A (en) * | 1974-10-16 | 1976-09-07 | The United States Of America As Represented By The Secretary Of Agriculture | Removal of heavy metal ions from aqueous solutions with insoluble cross-linked-starch-xanthates |
| US4664806A (en) * | 1985-01-22 | 1987-05-12 | Ciba-Geigy Corporation | Anionically modified polysaccharides chromatography agents |
| CN104649398A (en) * | 2015-02-12 | 2015-05-27 | 广东电网有限责任公司电力科学研究院 | Organic polymer heavy metal chelating flocculant as well as preparation method and application thereof |
| CN106117377A (en) * | 2016-06-20 | 2016-11-16 | 上海东升新材料有限公司 | A kind of preparation method of curing carbaminate modified tapioca starch chelating agen and products thereof |
-
2016
- 2016-12-22 CN CN201611196665.XA patent/CN106589145A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3979286A (en) * | 1974-10-16 | 1976-09-07 | The United States Of America As Represented By The Secretary Of Agriculture | Removal of heavy metal ions from aqueous solutions with insoluble cross-linked-starch-xanthates |
| US4664806A (en) * | 1985-01-22 | 1987-05-12 | Ciba-Geigy Corporation | Anionically modified polysaccharides chromatography agents |
| CN104649398A (en) * | 2015-02-12 | 2015-05-27 | 广东电网有限责任公司电力科学研究院 | Organic polymer heavy metal chelating flocculant as well as preparation method and application thereof |
| CN106117377A (en) * | 2016-06-20 | 2016-11-16 | 上海东升新材料有限公司 | A kind of preparation method of curing carbaminate modified tapioca starch chelating agen and products thereof |
Non-Patent Citations (1)
| Title |
|---|
| 刘欣: "复合交联淀粉制备及对造纸废水中金属离子吸附作用探究", 《华东纸业》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084283A (en) * | 2017-12-19 | 2018-05-29 | 东莞东美食品有限公司 | A kind of crosslinked starch and preparation method thereof |
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Application publication date: 20170426 |
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