CN104403011A - Preparation method of pH responsive material - Google Patents
Preparation method of pH responsive material Download PDFInfo
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- CN104403011A CN104403011A CN201410734965.3A CN201410734965A CN104403011A CN 104403011 A CN104403011 A CN 104403011A CN 201410734965 A CN201410734965 A CN 201410734965A CN 104403011 A CN104403011 A CN 104403011A
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Abstract
The invention discloses a preparation method of a pH responsive material. The method comprises the following steps: adding a certain mass of starch and TEMPO (Tetramethylpiperidinooxy), NaClO2 and NaClO solutions into a sodium phosphate buffer solution, stirring and reacting for 24 hours under certain conditions, adding anhydrous ethanol to terminate the reaction, pouring the solution into a conical flask to stand and layer, pouring away supernatant liquid, replacing with ethanol with a volume concentration of 50 percent and water, obtaining a clean and thick gelatinous carboxyl modified starch solution, drying and finally obtaining a product. The preparation method has the benefits that 1, the starch is taken as a raw material in the preparation method, is wide in source and low in cost, still returns to the nature in a form of carbon dioxide and water after degradation and is a natural renewable material which is zero-pollution; 2, the preparation process is simple, the product biocompatibility is optimal, the degradation is complete or a degradation product has no harm to bodies, and the preparation method can be widely applied to the fields of material science, biology and medicine.
Description
Technical field
The present invention relates to the preparation field of macromolecular material, particularly a kind of preparation method of pH responsive materials.
Background technology
Starch is the carbohydrate that plant is formed through photosynthesis, its wide material sources, cheap, degraded after still get back to the Nature with the form of carbonic acid gas and water, be considered to the material of the natural reproducible do not polluted completely, obtain in non-edible field and research and develop widely.PH responsive materials, refers to the change because of pH value, and material molecule can with the H in solution
+in conjunction be separated, this combination be separated, the change of its micro molecule structure can cause the change of its volume or form, this change is the stimulating responsive based on molecular level and macromolecular level.Due to this special character, cause the attention of Chinese scholars, and prepare a series of type material with pH responsiveness.But the pH responsive materials prepared at present or preparation process be complicated, have potential threat to environment, or when being used as biomaterial, biocompatibility is not good, degraded not exclusively or degraded product health is harmful to.
Summary of the invention
The object of this invention is to provide a kind of preparation method of pH responsive materials.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for pH responsive materials, operates according to following steps:
Take quality 1g starch, 0.024 ~ 0.24g TEMPO (2,2,6,6-tetramethyl piperidine-nitrogen-oxyradical), 1.06 ~ 2.52g NaClO
2(Textone) and 4 ~ 16ml mass concentration be 15% NaClO (clorox) solution to join volume be in the buffer solution of sodium phosphate of pH5.7 ~ 8.0 of 40 ~ 500ml, stirring reaction 24 hours under 35 DEG C ~ 60 DEG C conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, retain lower floor's thing, be 50% ethanol by volumetric concentration successively, water displacement lower floor thing, obtain clean, the starch solution of dense gelatinous carboxylated modification, the product obtained after drying is the starch of pH responsive materials-carboxylated modification.
Getting above-mentioned carboxylated treated starch 0.1g makes it be scattered in 20ml water, regulates the pH of dispersion liquid, when pH lower than 1 time, described starch molecule can be wadded a quilt with cotton and be gathered in the bottom; When pH raises gradually, described starch molecule can disperse gradually, when pH higher than 5.6 time, dispersion liquid is homogeneous transparent.
The invention has the beneficial effects as follows:
1. the present invention uses starch as raw material, wide material sources, cheap, degraded after still get back to the Nature with the form of carbonic acid gas and water, be the material of the natural reproducible do not polluted completely.
2. preparation process of the present invention is simple, and product biocompatibility is good, and degraded is complete or degraded product is harmless to health, can be widely used in the fields such as materialogy, biology, medical science.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
A preparation method for pH responsive materials, operates according to following steps:
Take quality 1g starch, 0.024g TEMPO, 1.06g NaClO
2joining volume with the 4ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of the pH5.7 of 40ml, stirring reaction 24 hours under 35 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, retain lower floor's thing, be 50% ethanol, water displacement lower floor thing by volumetric concentration successively, obtain starch solution that is clean, dense gelatinous carboxylated modification, the product obtained after drying is the starch of pH responsive materials-carboxylated modification.
Embodiment 2
A preparation method for pH responsive materials, operates according to following steps:
Take quality 1g starch, 0.12g TEMPO, 1.56g NaClO
2joining volume with the 10ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of the pH6.8 of 200ml, stirring reaction 24 hours under 40 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, retain lower floor's thing, be 50% ethanol, water displacement lower floor thing by volumetric concentration successively, obtain starch solution that is clean, dense gelatinous carboxylated modification, the product obtained after drying is the starch of pH responsive materials-carboxylated modification.
Embodiment 3
A preparation method for pH responsive materials, operates according to following steps:
Take quality 1g starch, 0.24g TEMPO, 2.52g NaClO
2joining volume with the 16ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of the pH8.0 of 500ml, stirring reaction 24 hours under 60 DEG C of conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, retain lower floor's thing, be 50% ethanol, water displacement lower floor thing by volumetric concentration successively, obtain starch solution that is clean, dense gelatinous carboxylated modification, the product obtained after drying is the starch of pH responsive materials-carboxylated modification.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. a preparation method for pH responsive materials, is characterized in that, operates according to following steps:
Take quality 1g starch, 0.024 ~ 0.24g TEMPO, 1.06 ~ 2.52g NaClO
2joining volume with 4 ~ 16ml mass concentration NaClO solution that is 15% is in the buffer solution of sodium phosphate of pH5.7 ~ 8.0 of 40 ~ 500ml, stirring reaction 24 hours under 35 DEG C ~ 60 DEG C conditions, add dehydrated alcohol termination reaction, solution is poured into stratification in Erlenmeyer flask, outwell supernatant liquid, retain lower floor's thing, be 50% ethanol, water displacement lower floor thing by volumetric concentration successively, obtain starch solution that is clean, dense gelatinous carboxylated modification, the product obtained after drying is the starch of pH responsive materials-carboxylated modification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410734965.3A CN104403011A (en) | 2014-12-05 | 2014-12-05 | Preparation method of pH responsive material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410734965.3A CN104403011A (en) | 2014-12-05 | 2014-12-05 | Preparation method of pH responsive material |
Publications (1)
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| CN104403011A true CN104403011A (en) | 2015-03-11 |
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| CN201410734965.3A Pending CN104403011A (en) | 2014-12-05 | 2014-12-05 | Preparation method of pH responsive material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017020237A1 (en) * | 2015-08-04 | 2017-02-09 | 江南大学 | Triple-response type starch-based microgel and preparation method therefor |
| CN106699911A (en) * | 2017-01-20 | 2017-05-24 | 青岛大学 | Method for ultrasonic-assisted preparation of high carboxyl content oxidized starch |
| CN106832018A (en) * | 2017-01-20 | 2017-06-13 | 青岛大学 | A kind of preparation method of high-carboxyl-content oxidized starch |
| CN108774315A (en) * | 2018-06-27 | 2018-11-09 | 湖南华腾制药有限公司 | PEGylated Norfloxacin and its antibacterial application |
| CN114191601A (en) * | 2021-11-25 | 2022-03-18 | 华南理工大学 | Starch gel hemostatic material based on 3D printing technology and preparation method and application thereof |
-
2014
- 2014-12-05 CN CN201410734965.3A patent/CN104403011A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| NAOYUKI TAMURA等: "Oxidation of curdlan and other polysaccharides by 4-acetamide-TEMPO/NaClO/NaClO2 under acid conditions", 《CARBOHYDRATE POLYMERS》 * |
| 桑显葵等: "《中国造纸学会第十六届学术年会论文集》", 22 May 2014 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017020237A1 (en) * | 2015-08-04 | 2017-02-09 | 江南大学 | Triple-response type starch-based microgel and preparation method therefor |
| US9956536B2 (en) | 2015-08-04 | 2018-05-01 | Jiangnan University | Triple-responsive starch-based microgel and preparation method thereof |
| CN106699911A (en) * | 2017-01-20 | 2017-05-24 | 青岛大学 | Method for ultrasonic-assisted preparation of high carboxyl content oxidized starch |
| CN106832018A (en) * | 2017-01-20 | 2017-06-13 | 青岛大学 | A kind of preparation method of high-carboxyl-content oxidized starch |
| CN108774315A (en) * | 2018-06-27 | 2018-11-09 | 湖南华腾制药有限公司 | PEGylated Norfloxacin and its antibacterial application |
| CN114191601A (en) * | 2021-11-25 | 2022-03-18 | 华南理工大学 | Starch gel hemostatic material based on 3D printing technology and preparation method and application thereof |
| CN114191601B (en) * | 2021-11-25 | 2022-05-24 | 华南理工大学 | Starch gel hemostatic material based on 3D printing technology and preparation method and application thereof |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20150311 |