CN104652127A - Synthetic method of [beta]-cyclodextrin - Google Patents
Synthetic method of [beta]-cyclodextrin Download PDFInfo
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- CN104652127A CN104652127A CN201310584502.9A CN201310584502A CN104652127A CN 104652127 A CN104652127 A CN 104652127A CN 201310584502 A CN201310584502 A CN 201310584502A CN 104652127 A CN104652127 A CN 104652127A
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- distilled water
- viscose
- suction filtration
- beta
- epoxychloropropane
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Abstract
A synthetic method of [beta]-cyclodextrin belongs to the technical field of chemical engineering. In particular, the invention relates to the synthetic method of [beta]-cyclodextrin and provides a synthetic method of cellulosic fiber grafted [beta]-cyclodextrin, wherein the synthetic method is characterized by comprising following steps: (1) weighing 1g of viscose cellulosic fiber and placing the viscose cellulosic fiber in a 300-350 ml conical flask with addition of 250-1000 ml of distillated water and 4-16ml of a 0.1 mol/ml NaOH solution; (2) adding 55-88 ml of distillated water, 7-20 ml of epoxy chloropropane and 7-20 ml of a NaOH solution to the viscose cellulosic fiber after swelling; (3) adding a proper amount of distillated water, washing a product to neutral, detecting the epoxy chloropropane in an effluent liquid with sodium thiosulfate and phenolphthalein indicator until the epoxy chloropropane is washed-out, and then performing suction filtration; (4) directly feeding the epoxy viscose after the suction filtration into a 40% NaOH solution in which [beta]-cyclodextrin is dissolved, performing a vibrating reaction at 45 DEG C in water bath for 3-8 h, stopping vibration, adding a proper amount of distillated water into a triangular flask to wash a product, performing suction filtration until an effluent liquid is neutral, and drying the product at 50-80 DEG C.
Description
Technical field
The invention belongs to chemical technology field, specifically, the present invention relates to a kind of beta-schardinger dextrin-synthetic method.
Background technology
Along with the world is to the attention of environmental protection, water treatment technology is subject to the growing interest of people.But the water treatment of China research is started late, and technical merit still has larger gap compared with advanced international standard.The method for treating water governance efficiencies such as traditional bioanalysis, flocculent precipitation, absorption method are low, and have secondary pollution, and therefore developing the water treatment agent of new generation with advanced level becomes the task of top priority.Beta-schardinger dextrin-is the cyclic oligosaccharide formed by α-Isosorbide-5-Nitrae-2 glycosidic bond by 7 glucose molecules, and its most significant feature is that to have a ring outer hydrophilic, hydrophobic and have the three-dimensional chirality cavity microenvironment of certain size in ring.Its molecular surface distributes the identical hydroxyl of numerous chemical reactivity, has taper tubular structure.Sticking with paste special hydrophobic cavity due to β-ring can the suitable organic molecule of envelope size, and outside it, hydrophilic hydroxyl has chelation to high volence metal ion, therefore has certain solid and selects and recognition performance.β just-ring sticks with paste this special structures and characteristics, makes it have a wide range of applications at field of environment protection.
Summary of the invention
The present invention is exactly for above-mentioned technical problem, provides a kind of cellulose fibre graft beta-cyclodextrin synthetic method.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme: beta-schardinger dextrin-synthetic method of the present invention, it is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 300-350mL, and add the distilled water of 250-1000mL, add the NaOH solution 4-16mL of 0.1mol/mL, swelling 1-4h.The distilled water of 55-88mL is added, the NaOH solution of 7-20mL epoxychloropropane and 7-20mL in the viscose after swelling.Put into water-bath shaker 40-60 DEG C of constant temperature 3-6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 3-8h, stops concussion, and add appropriate distilled water in the middle of triangular flask.Wash, suction filtration, until eluate is neutral.Product is in 50-80 DEG C of oven dry.
Beneficial effect of the present invention: production method of the present invention is simple, reaction condition is gentle, and appropriate experimental indoor are configured, and is also applicable to factory mass and produces, have wide range of applications, have very strong practicality.
In addition, productive rate of the present invention is high, good product quality, and after testing, product indices all can reach standard.
Detailed description of the invention
Beta-schardinger dextrin-synthetic method of the present invention, is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 300-350mL, and add the distilled water of 250-1000mL, add the NaOH solution 4-16mL of 0.1mol/mL, swelling 1-4h.The distilled water of 55-88mL is added, the NaOH solution of 7-20mL epoxychloropropane and 7-20mL in the viscose after swelling.Put into water-bath shaker 40-60 DEG C of constant temperature 3-6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 3-8h, stops concussion, and add appropriate distilled water in the middle of triangular flask.Wash, suction filtration, until eluate is neutral.Product is in 50-80 DEG C of oven dry.
Embodiment 1: take 1g viscose cellulose fiber, put into the conical flask of 300mL, and add the distilled water of 250mL, add the NaOH solution 4mL of 0.1mol/mL, swelling 1h.The distilled water of 55mL is added, the NaOH solution of 7mL epoxychloropropane and 7mL in the viscose after swelling.Put into water-bath shaker 40 DEG C of constant temperature 3-6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 3h, stops concussion, and add appropriate distilled water in the middle of triangular flask.Wash, suction filtration, until eluate is neutral.Product is in 50 DEG C of oven dry.
Embodiment 2: take 1g viscose cellulose fiber, put into the conical flask of 350mL, and add the distilled water of 1000mL, add the NaOH solution 16mL of 0.1mol/mL, swelling 4h.The distilled water of 88mL is added, the NaOH solution of 20mL epoxychloropropane and 20mL in the viscose after swelling.Put into water-bath shaker 60 DEG C of constant temperature 6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 8h, stops concussion, and add appropriate distilled water in the middle of triangular flask.Wash, suction filtration, until eluate is neutral.Product is in 80 DEG C of oven dry.
Embodiment 3: take 1g viscose cellulose fiber, put into the conical flask of 325mL, and add the distilled water of 700mL, add the NaOH solution 10mL of 0.1mol/mL, swelling 3h.The distilled water of 75mL is added, the NaOH solution of 15mL epoxychloropropane and 15mL in the viscose after swelling.Put into water-bath shaker 50 DEG C of constant temperature 4h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 6h, stops concussion, and add appropriate distilled water in the middle of triangular flask.Wash, suction filtration, until eluate is neutral.Product is in 70 DEG C of oven dry.
Claims (4)
1. beta-schardinger dextrin-synthetic method, it is characterized in that: beta-schardinger dextrin-synthetic method of the present invention, it is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 300-350mL, and add the distilled water of 250-1000mL, add the NaOH solution 4-16mL of 0.1mol/mL, swelling 1-4h; The distilled water of 55-88mL is added, the NaOH solution of 7-20mL epoxychloropropane and 7-20mL in the viscose after swelling; Put into water-bath shaker 40-60 DEG C of constant temperature 3-6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 3-8h, stops concussion, and add appropriate distilled water in the middle of triangular flask; Wash, suction filtration, until eluate is neutral; Product is in 50-80 DEG C of oven dry.
2. beta-schardinger dextrin-synthetic method according to claim 1, is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 300mL, and add the distilled water of 250mL, add the NaOH solution 4mL of 0.1mol/mL, swelling 1h; The distilled water of 55mL is added, the NaOH solution of 7mL epoxychloropropane and 7mL in the viscose after swelling; Put into water-bath shaker 40 DEG C of constant temperature 3-6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 3h, stops concussion, and add appropriate distilled water in the middle of triangular flask; Wash, suction filtration, until eluate is neutral; Product is in 50 DEG C of oven dry.
3. beta-schardinger dextrin-synthetic method according to claim 1, is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 350mL, and add the distilled water of 1000mL, add the NaOH solution 16mL of 0.1mol/mL, swelling 4h; The distilled water of 88mL is added, the NaOH solution of 20mL epoxychloropropane and 20mL in the viscose after swelling; Put into water-bath shaker 60 DEG C of constant temperature 6h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 8h, stops concussion, and add appropriate distilled water in the middle of triangular flask; Wash, suction filtration, until eluate is neutral; Product is in 80 DEG C of oven dry.
4. beta-schardinger dextrin-synthetic method according to claim 1, is characterized in that: take 1g viscose cellulose fiber, put into the conical flask of 325mL, and add the distilled water of 700mL, add the NaOH solution 10mL of 0.1mol/mL, swelling 3h; The distilled water of 75mL is added, the NaOH solution of 15mL epoxychloropropane and 15mL in the viscose after swelling; Put into water-bath shaker 50 DEG C of constant temperature 4h after being shaken by triangular flask, stop reaction, add appropriate distilled water, product washing is to neutral, and the epoxychloropropane detected with sodium thiosulfate and phenolphthalein indicator in efflux, until clean epoxychloropropane, suction filtration; Directly dropped into by epoxidation viscose after suction filtration in the sodium hydroxide solution of dissolve beta-schardinger dextrin-40%, reaction temperature is 45 DEG C, and water-bath concussion reaction 6h, stops concussion, and add appropriate distilled water in the middle of triangular flask; Wash, suction filtration, until eluate is neutral; Product is in 70 DEG C of oven dry.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310584502.9A CN104652127A (en) | 2013-11-20 | 2013-11-20 | Synthetic method of [beta]-cyclodextrin |
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| CN201310584502.9A CN104652127A (en) | 2013-11-20 | 2013-11-20 | Synthetic method of [beta]-cyclodextrin |
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| CN104652127A true CN104652127A (en) | 2015-05-27 |
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| CN201310584502.9A Pending CN104652127A (en) | 2013-11-20 | 2013-11-20 | Synthetic method of [beta]-cyclodextrin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271505A (en) * | 2017-06-01 | 2017-10-20 | 赵云飞 | Composite electrode and preparation method thereof, Quercetin sensor |
| CN109444123A (en) * | 2018-10-26 | 2019-03-08 | 宁夏然尔特工业产业研究院（有限公司） | Application and detection method in beta-cyclodextrin-micro benzaldehyde of phenolphthalein probe in detecting |
| CN112739723A (en) * | 2018-10-15 | 2021-04-30 | 国立大学法人大阪大学 | Cyclic oligosaccharide and process for producing the same |
-
2013
- 2013-11-20 CN CN201310584502.9A patent/CN104652127A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107271505A (en) * | 2017-06-01 | 2017-10-20 | 赵云飞 | Composite electrode and preparation method thereof, Quercetin sensor |
| CN112739723A (en) * | 2018-10-15 | 2021-04-30 | 国立大学法人大阪大学 | Cyclic oligosaccharide and process for producing the same |
| CN112739723B (en) * | 2018-10-15 | 2023-02-17 | 国立大学法人大阪大学 | Cyclic oligosaccharide and process for producing the same |
| CN109444123A (en) * | 2018-10-26 | 2019-03-08 | 宁夏然尔特工业产业研究院（有限公司） | Application and detection method in beta-cyclodextrin-micro benzaldehyde of phenolphthalein probe in detecting |
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