CN105597692A - Preparation method of cellulose derivative gydrogel microspheres - Google Patents
Preparation method of cellulose derivative gydrogel microspheres Download PDFInfo
- Publication number
- CN105597692A CN105597692A CN201510978698.9A CN201510978698A CN105597692A CN 105597692 A CN105597692 A CN 105597692A CN 201510978698 A CN201510978698 A CN 201510978698A CN 105597692 A CN105597692 A CN 105597692A
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- cellulose derivative
- preparation
- ethylenediamine
- microspheres
- cellulose
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- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28019—Spherical, ellipsoidal or cylindrical
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Water Supply & Treatment (AREA)
- Hydrology & Water Resources (AREA)
- Soil Sciences (AREA)
- Dispersion Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Biological Depolymerization Polymers (AREA)
Abstract
The invention provides a preparation method of cellulose derivative gydrogel microspheres. The preparation method comprises the following steps: adding a sodium hydroxide solution into microcrystalline cellulose, then adding an ethylenediamine tetraacetic dianhydride solution, reacting for 2h at 50 DEG C while stirring is carried out, washing and drying to obtain an ethylenediamine tetraacetic acid-esterified cellulose derivative; adding an epichlorohydrin crosslinker and polyvinyl alcohol into an aqueous solution of the ethylenediamine tetraacetic acid-esterified cellulose derivative, and then dropwise adding into 50 DEG C liquid paraffin, and stirring for 2h to prepare the ethylenediamine tetraacetic acid-esterified cellulose derivative gydrogel microspheres. The gydrogel microspheres prepared according to the preparation method not only has the characteristics of biodegradability, strong water absorption and the like of cellulose, and but also has good metal ion adsorption; the synthesized hydrogel microspheres are expected to be applied to treatment and recycle of heavy metal in sewage and soil, and has a wide application prospect.
Description
Technical field
Patent of the present invention provides a kind of preparation method of vitamin derivative hydrogel microsphere.
Background technology
The environmental problem of heavy metal pollution becomes increasingly conspicuous, and synthetic economic adsorbent reliable, that adsorption efficiency is high and adsorption capacity is large is imperative.
Cellulose has the advantages such as mechanical strength is high, renewable, bio-compatibility is good, inexpensive and biodegradable. Cellulosic structure is the linear polymer chemistry thing being formed by connecting by 1,4 glucosides by glucose construction unit, in cellulosic each glucose unit, there is active hydroxyl, can with ethylenediamine tetra-acetic acid in carboxyl generation esterification generate cellulose derivative. The cellulose derivative of esterification not only has the performances such as cellulosic degradability, biocompatibility and water imbibition, has introduced carboxyl and the amido of ethylenediamine tetra-acetic acid simultaneously, and metal is had to good chelating performance.
Hydrogel has the characteristics such as low cost, porous, good biocompatibility and biodegradable, and synthetic water gel has the features such as good mechanical strength and porous. The present invention, taking ethylenediamine tetra-acetic acid and cellulose as raw material, carries out esterification synthetic chemistry modified cellulose derivative, then taking esterified cellulose derivative as raw material, synthetic water gel micro-ball. The hydrogel microsphere of preparation have cellulosic biodegradable, water imbibition strong, metal is there is to the advantages such as good adsorptivity, can be applicable to during heavy metal in waste water, soil processes and reclaim.
Summary of the invention
The invention provides a kind of preparation method of cellulose derivative hydrogel microsphere.
The preparation method of cellulose derivative hydrogel microsphere is as follows: be 5% sodium hydroxide solution by adding mass concentration in microcrystalline cellulose, be uniformly mixed 1h, adding mass concentration is 30% ethylenediamine tetra-acetic acid two anhydride solutions again, stirring reaction 2h at 50 DEG C, the cellulose esterification product of synthesis of ethylenediamine tetraacethyl dianhydride, respectively clean 2 times with ethanol, acetone successively, dry 5h at 80 DEG C, obtain the cellulose derivative of ethylenediamine tetraacetate.
The cellulose derivative of ethylenediamine tetraacetate is dissolved in the water, in the above-mentioned aqueous solution, add 5% epoxychloropropane crosslinking agent, 2% polyvinyl alcohol, above-mentioned solution is added drop-wise in atoleine, temperature is 50 DEG C, stir 2h, filter, prepare the cellulose derivative hydrogel microsphere that ethylenediamine tetraacetateization is modified.
The invention has the beneficial effects as follows: the hydrogel microsphere of preparation not only has cellulosic biodegradable, the feature such as water imbibition is strong, simultaneously owing to having multiple carboxyls and amido in structure, metal is had to good chelating; The porous of hydrogel microsphere has been strengthened the adsorption capacity to metal ion, and can be by performances such as the mechanical strengths of regulation and control hydrogel microsphere, and the heavy metal that synthetic hydrogel microsphere is expected to be applied in waste water, soil is processed recovery.
Brief description of the drawings
Fig. 1 is the preparation flow figure of the cellulose derivative hydrogel microsphere of patent of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, the preparation process of cellulose derivative hydrogel microsphere in the present invention is further described.
As shown in the figure, be 5% sodium hydroxide solution by adding mass concentration in microcrystalline cellulose, be uniformly mixed 1h, adding mass concentration is 30% ethylenediamine tetra-acetic acid two anhydride solutions again, stirring reaction 2h at 50 DEG C, the cellulose esterification product of synthesis of ethylenediamine tetraacethyl dianhydride, respectively cleans 2 times with ethanol, acetone successively, at 80 DEG C, dry 5h, obtain the cellulose derivative of ethylenediamine tetraacetate. The cellulose derivative of ethylenediamine tetraacetate is dissolved in the water, in the above-mentioned aqueous solution, add 5% epoxychloropropane crosslinking agent, 2% polyvinyl alcohol, above-mentioned solution is added drop-wise in atoleine, temperature is 50 DEG C, stir 2h, filter, prepare the cellulose derivative hydrogel microsphere that ethylenediamine tetraacetateization is modified.
Claims (5)
1. the preparation method of a cellulose derivative hydrogel microsphere, it is characterized in that: be 5% sodium hydroxide solution by adding mass concentration in microcrystalline cellulose, be uniformly mixed 1h, add again ethylenediamine tetra-acetic acid two anhydride solutions, stirring reaction 2h at 50 DEG C, the cellulose esterification product of synthesis of ethylenediamine tetraacethyl dianhydride, use successively ethanol, acetone is each to be cleaned 2 times, at 80 DEG C, dry 5h, obtain the cellulose derivative of ethylenediamine tetraacetate, the cellulose derivative of ethylenediamine tetraacetate is dissolved in the water, in the above-mentioned aqueous solution, add respectively epoxychloropropane crosslinking agent, polyvinyl alcohol, above-mentioned solution is added drop-wise in atoleine, stir 2h, filter, prepare the cellulose derivative hydrogel microsphere that ethylenediamine tetraacetateization is modified.
2. preparation method according to claim 1, is characterized in that: the mass concentration of ethylenediamine tetra-acetic acid two anhydride solutions that add is 30%.
3. preparation method according to claim 1, is characterized in that: the epoxychloropropane crosslinking agent volume ratio adding is 5%.
4. preparation method according to claim 1, is characterized in that: the polyvinyl alcohol agent volume ratio adding is 2%.
5. preparation method according to claim 1, is characterized in that: by adding respectively epoxychloropropane crosslinking agent, polyvinyl alcohol in the cellulose derivative aqueous solution, be added drop-wise in atoleine, reaction temperature is 50 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510978698.9A CN105597692A (en) | 2015-12-24 | 2015-12-24 | Preparation method of cellulose derivative gydrogel microspheres |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510978698.9A CN105597692A (en) | 2015-12-24 | 2015-12-24 | Preparation method of cellulose derivative gydrogel microspheres |
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| Publication Number | Publication Date |
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| CN105597692A true CN105597692A (en) | 2016-05-25 |
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| CN201510978698.9A Pending CN105597692A (en) | 2015-12-24 | 2015-12-24 | Preparation method of cellulose derivative gydrogel microspheres |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108554389A (en) * | 2018-05-14 | 2018-09-21 | 中国人民大学 | A kind of bacteria cellulose membrane adsorbent and the preparation method and application thereof that EDTA is modified |
| CN109225170A (en) * | 2018-09-27 | 2019-01-18 | 陕西科技大学 | A kind of cellulose base adsorbent material and its preparation method and application of casein crosslinking |
| CN110003356A (en) * | 2019-04-12 | 2019-07-12 | 南京理工大学 | Thermal gels-EDTA derivative and preparation method and the application in adsorption of metal ions |
| CN113501886A (en) * | 2021-08-17 | 2021-10-15 | 中南大学 | Anhydride esterification modified cellulose, cellulose nano-silver composite material, and preparation method and application thereof |
| CN114605664A (en) * | 2020-12-17 | 2022-06-10 | 赣南师范大学 | Hydrogel and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910393A (en) * | 2015-06-10 | 2015-09-16 | 华南理工大学 | Cellulose sulfate hydrogel and preparation method thereof |
-
2015
- 2015-12-24 CN CN201510978698.9A patent/CN105597692A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910393A (en) * | 2015-06-10 | 2015-09-16 | 华南理工大学 | Cellulose sulfate hydrogel and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| OSVALDO KARNITZ JÚNIOR ET AL.: "Adsorption of Cu(II), Cd(II), and Pb(II) from aqueous single metal solutions by mercerized cellulose and mercerized sugarcane bagasse chemically modified with EDTA dianhydride (EDTAD)", 《CARBOHYDRATE POLYMERS》 * |
| SHAOPING YANG ET AL.: "Hydrogel Beads Based on Carboxymethyl Cellulose for Removal Heavy Metal Ions", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108554389A (en) * | 2018-05-14 | 2018-09-21 | 中国人民大学 | A kind of bacteria cellulose membrane adsorbent and the preparation method and application thereof that EDTA is modified |
| CN108554389B (en) * | 2018-05-14 | 2020-09-01 | 中国人民大学 | EDTA (ethylene diamine tetraacetic acid) -modified bacterial cellulose membrane adsorbent as well as preparation method and application thereof |
| CN109225170A (en) * | 2018-09-27 | 2019-01-18 | 陕西科技大学 | A kind of cellulose base adsorbent material and its preparation method and application of casein crosslinking |
| CN109225170B (en) * | 2018-09-27 | 2021-06-29 | 陕西科技大学 | Casein crosslinked cellulose-based adsorption material and preparation method and application thereof |
| CN110003356A (en) * | 2019-04-12 | 2019-07-12 | 南京理工大学 | Thermal gels-EDTA derivative and preparation method and the application in adsorption of metal ions |
| CN114605664A (en) * | 2020-12-17 | 2022-06-10 | 赣南师范大学 | Hydrogel and preparation method thereof |
| CN114605664B (en) * | 2020-12-17 | 2023-07-04 | 赣南师范大学 | Hydrogel and preparation method thereof |
| CN113501886A (en) * | 2021-08-17 | 2021-10-15 | 中南大学 | Anhydride esterification modified cellulose, cellulose nano-silver composite material, and preparation method and application thereof |
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