CN109678984A - A method of Bismuth alginate is synthesized by mechanochemistry solid - Google Patents
A method of Bismuth alginate is synthesized by mechanochemistry solid Download PDFInfo
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- CN109678984A CN109678984A CN201910102359.2A CN201910102359A CN109678984A CN 109678984 A CN109678984 A CN 109678984A CN 201910102359 A CN201910102359 A CN 201910102359A CN 109678984 A CN109678984 A CN 109678984A
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
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Abstract
The present invention relates to the technology of preparing of bismuth-containing compound, specifically a kind of method that Bismuth alginate is synthesized by mechanochemistry solid.Alginic acid and bismuth alkali are realized into solid-state reaction by mechanical collision, obtain powdered Bismuth alginate.The mechanochemistry solid synthetic method of invention gained Bismuth alginate can not only reduce pollution, shorten the reaction time, reduce production cost, but also have many advantages, such as that high income, selectivity are strong, have extensive industrial application prospect.
Description
Technical field
The present invention relates to the technologies of preparing of bismuth-containing compound, specifically a kind of to synthesize seaweed by mechanochemistry solid
The method of sour bismuth.
Background technique
Bismuth organic compound, which has, inhibits and kills bacterium, virus or even trypanosome and conveyor screw etc..Bismuth preparation is alive
It is widely used in the treatment of enterogastric diseases within the scope of boundary.
Current clinically common anti-gastric-ulcer bismuth preparation mainly includes bismuth subcarbonate, bismuth citrate and bismuth subgallate
Deng the content of bismuth is above 46%.Since gastric ulcer is a kind of common disease, frequently-occurring disease, such as long term administration, its toxic side effect is not allowed
Ignore, such as headache and decrease of memory can be caused.Bismuth preparation truly has its unique advantage in the treatment of gastric ulcer.It can be straight
It connects and kills helicobacter pylori (Helicobacter pylori, Hp), overcome the initial drug-resistant of Hp and avoid secondary drug resistance
Property.
The national inventing patent (ZL 201210005970.1) authorized for 2014 using alginic acid as the carrier of bismuth,
Synthesize a kind of totally new kind of alginic acid bismuth salt, and through infrared spectrum analysis, its structure is characterized, it was demonstrated that this is one
The organic compound of the novel bismuth-containing of kind.Bismuth alginate has both the bioactivity of both bismuth preparation and alginic acid, has stomach lining
Protection reduces pepsin activity, kills Hp, promotes the multi-functionals such as peptic ulcer wound healing, has good new drug
Development volue；But that there are preparation methods is relative complex for the technology that is related to of this method, consumes a large amount of organic solvent ethyl alcohol, is produced into
The problems such as this is higher, is unfavorable for energy-saving.Therefore, this field need to develop it is a kind of it is easy to operate, process stabilizing, efficiently make
The method of standby Bismuth alginate.
Summary of the invention
The object of the present invention is to provide a kind of methods for synthesizing Bismuth alginate by mechanochemistry solid.
To achieve the above object, the invention adopts a technical scheme as:
A method of Bismuth alginate is synthesized by mechanochemistry solid, alginic acid and bismuth alkali are realized by mechanical collision
Solid-state reaction obtains powdered Bismuth alginate.
The bismuth alkali is bismuth hydroxide.
The solid-state reaction is to react 1-4h under 500-1000 revs/min of revolving speed using ball mill.
Further, the solid-state reaction is using planetary ball mill or oscillating ball mill, in revolving speed 700-800
1-2h is reacted under rev/min.
The alginic acid can be extracted by seaweed glue and be obtained, or be prepared by alginate.
The bismuth alkali can be prepared by bismuth salt.
Use the bismuth salt for bismuth nitrate, bismuth subnitrate, bismuth oxide, bismuth subcarbonate, bismuth trichloride or Basic Bismuth Chloride, chlorine
Bismuth oxide, bismuth acetate, bismuth and ammonium citrate, bismuth chloride or five water bismuth nitrates carry out preparing hydrogen-oxygen according to existing preparation method
Change bismuth.
According to Bismuth alginate (Bismuth alginate) obtained by the present invention, through infrared spectrum analysis, its chemistry knot is confirmed
Structure is as follows:
Assignment of Infrared Spectrum: infrared spectroscopy is surveyed on Thermo Scientific Nicolet iS50 infrared spectrometer
Fixed, infrared spectrogram is shown in Fig. 3, and the analysis of functional group the results are shown in Table 1.Analyze the metal carboxylate that result confirmation molecule is hydroxyl.
Advantage for present invention
The present invention is to pass through mechanochemistry solid synthesis Bismuth alginate (polyuronide bismuth), gained sea with alginic acid and bismuth alkali
Alginic acid bismuth can be used for treating gastritis, gastric ulcer, killing helicobacter pylori etc..
Specially
(1) operation of the present invention is simple, simplifies operation and last handling process, safety is good, process stabilizing；
(2) reaction temperature of the present invention is lower, less energy consumption；
(3) it is not necessarily to solvent and auxiliary agent in synthesis process of the present invention, reduces or eliminates to human health, the harmful chemistry of environment
Reaction dissolvent etc., and solvent free is avoided that and uses a large amount of toxics and volatile organic compounds.
To sum up the mechanochemistry solid synthetic method of present invention gained Bismuth alginate can not only reduce pollution, shorten reaction
Time reduces production cost, but also has many advantages, such as that high income, selectivity are strong, has extensive industrial application prospect.
Detailed description of the invention
Fig. 1 is the planetary high-energy ball mill working principle diagram that the present invention uses；Wherein, figure a. is planetary plate and ball grinder
The direction of motion schemes b. ball grinder cross section.
Fig. 2 is that mechanochemistry solid synthesis route provided in an embodiment of the present invention prepares Bismuth alginate flow chart.
Fig. 3 is the infrared spectrum that mechanochemistry solid synthesis route provided in an embodiment of the present invention prepares Bismuth alginate, wherein
A: alginic acid B: Bismuth alginate.
Specific embodiment
With reference to the accompanying drawings and examples the present invention is illustrated to illustrate.
The present invention is primary raw material with bismuth salt with alginic acid and its esters, by solid-state machinery chemosynthesis reaction, is generated
Bismuth alginate complex solid.Resulting Bismuth alginate can be used for killing helicobacter pylori, treatment gastritis, gastric ulcer etc..This hair
Bright mechanochemistry solid reaction method is easy to operate, simplifies operation and last handling process, safety is good, process stabilizing；
Reaction temperature is lower, less energy consumption；Can reduce pollution, shorten the reaction time, reduce production cost, but also have high income,
The advantages that selectivity is strong.
Embodiment 1:
As shown in Fig. 2, Bismuth alginate preparation method sequentially includes the following steps:
(1) food-grade sodium alginate 10g is first weighed, is added to the container, 1500ml distilled water is added, is stirred with blender straight
It is completely dissolved to sodium alginate.Then it with HCl tune pH to 1-3, is then separated by solid-liquid separation, it is 5 hours dry at 60 DEG C in an oven.With
High speed disintegrator crushes, and crosses 60 meshes.
(2) 30g bismuth nitrate crystal is weighed, adds deionized water 300ml, dilute nitric acid solution is added dropwise while stirring, until solution
Clarification.Then NaOH solution is added dropwise while stirring, until pH value of solution reaches 10-12, trivalent bismuth ion is made thoroughly to be converted into Bi
(OH)3Precipitating.Precipitating is filtered, and is washed with deionized three times, 45 DEG C of drying obtain faint yellow Bi (OH)3Powder.
(3) 5g alginic acid powder and 1g Bi (OH) are weighed3Yellow powder is placed in 100ml polytetrafluoroethylene (PTFE) ball grinder (ginseng
See Fig. 1), Φ 5mm zirconia ball is added, is fixed on planetary ball mill, revolving speed 700-800rpm, reacts 1 hour.It is made
Bismuth alginate powder (referring to Fig. 3 and table 1).
Above-mentioned acquisition Bismuth alginate powder is contained according to bismuth in the measurement sample of method described in 2015 editions " Chinese Pharmacopoeias "
Amount.
Method is as follows: this product about 0.5g is taken, it is accurately weighed, and after adding water 50mL to dissolve, then plus nitric acid solution 3mL and xylenol
Orange indicator solution 2 drips, and is titrated to solution displaing yellow with Calcium Disodium Versenate titrating solution (0.05mol/L).Every lmL ethylenediamine tetraacetic
Acetic acid disodium titrating solution (0.05mol/L) is equivalent to 10.45mg Bi.
It is measured by Calcium Disodium Versenate volumetric precipitation method, the Bismuth alginate compound bismuth-containing 15.8% is (by weight
Meter, the same below).
The ownership of 1 infrared spectroscopy main peaks of table
Embodiment 2:
As shown in Fig. 2, Bismuth alginate preparation method sequentially includes the following steps:
(1) food-grade potassium alginate 10g is first weighed, is added to the container, 2000ml distilled water is added, is stirred with blender straight
It is completely dissolved to potassium alginate.Then it with HCL aqueous solution tune pH to 1-3, is then separated by solid-liquid separation, it is dry in 50 DEG C of baking ovens, it uses
High speed disintegrator crushes, and crosses 60 meshes.
(2) 30g basic bismuth nitrate crystal is weighed, deionized water 500ml is added, under stiring, dilute nitric acid solution is added dropwise, until
Solution clarification, is then added dropwise NaOH solution while stirring, until pH value of solution reaches 12, makes Bi3+It is converted into Bi (OH)3Precipitating.It will
Precipitating is filtered and is washed with deionized three times, and 45 DEG C of drying obtain faint yellow Bi (OH)3Powder.
(3) 5g alginic acid powder and 0.5g Bi (OH) are weighed3Yellow powder in 100ml polytetrafluoroethylene (PTFE) ball grinder and
Φ 5mm zirconia ball, is fixed on planetary ball mill, revolving speed 800-900rpm, and ball milling 1 hour.Bismuth alginate white is made
Powder.
Above-mentioned acquisition Bismuth alginate powder is contained according to bismuth in the measurement sample of method described in 2015 editions " Chinese Pharmacopoeias "
Amount is 7.6% (by weight).
Embodiment 3:
As shown in Fig. 2, Bismuth alginate preparation method sequentially includes the following steps:
(1) food-grade ammonium alginate 10g is first weighed, is added to the container, 1500ml distilled water is added, is stirred with blender straight
It is completely dissolved to sodium alginate.Then it with HCL aqueous solution tune pH to 2 or so, is then separated by solid-liquid separation, it is dry in 50 DEG C of baking ovens,
It is crushed with high speed disintegrator, and crosses 60 meshes.
(2) 30g bismuth subnitrate crystal is weighed, deionized water 300ml is added, under stiring, nitric acid solution is added dropwise, until solution
Clarification, is then added dropwise NaOH solution while stirring, until pH value of solution reaches 12, to guarantee Bi3+Thoroughly it is converted into Bi (OH)3It is heavy
It forms sediment.Precipitating is filtered and is washed with deionized three times, 45 DEG C of drying obtain faint yellow Bi (OH)3Powder.
(3) 5g alginic acid powder and 0.8g Bi (OH) are weighed3Yellow powder in 100ml polytetrafluoroethylene (PTFE) ball grinder and
Φ 5mm zirconia ball, is fixed on planetary ball mill planetary plate, revolving speed 900-1000rpm, and ball milling 1 hour.Seaweed is made
Sour bismuth white powder.
Above-mentioned acquisition Bismuth alginate powder is contained according to bismuth in the measurement sample of method described in 2015 editions " Chinese Pharmacopoeias "
Amount is 12.5% (by weight).
Claims (7)
1. a kind of method for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: alginic acid and bismuth alkali are passed through machine
Solid-state reaction is realized in tool collision, obtains powdered Bismuth alginate.
2. the method according to claim 1 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: the bismuth alkali
For bismuth hydroxide.
3. the method as described in claim 1 or 2 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: described
Solid-state reaction is to react 1-4h under 500-1000 revs/min of revolving speed using ball mill.
4. the method according to claim 3 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: the solid-state
Reaction is to react 1-2h under 700-800 revs/min of revolving speed using planetary ball mill or oscillating ball mill.
5. the method according to claim 1 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: the seaweed
Acid can be extracted by seaweed glue and be obtained, or be prepared by alginate.
6. the method as described in claim 1 or 2 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: described
Bismuth alkali can be prepared by bismuth salt.
7. the method according to claim 6 for synthesizing Bismuth alginate by mechanochemistry solid, it is characterised in that: the bismuth salt
For bismuth nitrate, bismuth subnitrate, bismuth oxide, bismuth subcarbonate, bismuth trichloride or Basic Bismuth Chloride, bismuth oxychloride, bismuth acetate, citric acid
Bismuth ammonium, bismuth chloride or five water bismuth nitrates.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2350097A1 (en) * | 1976-05-05 | 1977-12-02 | Brothier Laboratoires | Micro-fibrillar calcium alginate powder compsn. - for treatment of erythematose dermatological lesions |
| JP3984402B2 (en) * | 1999-10-12 | 2007-10-03 | 株式会社マルイ物産 | Method for producing fucoidan-like polysaccharide complex and immunostimulant based on the same |
| JP2009149734A (en) * | 2007-12-19 | 2009-07-09 | Kao Corp | Production method for alginic acid of low molecular weight or derivative thereof |
| CN102558383A (en) * | 2012-01-10 | 2012-07-11 | 中国科学院海洋研究所 | Bismuth alginate and preparation method and application thereof |
| CN103360510A (en) * | 2013-07-31 | 2013-10-23 | 青岛海之林生物科技开发有限公司 | Production method for alginate specialized for welding |
| CN104844726B (en) * | 2014-02-13 | 2017-02-01 | 青岛海之林生物科技开发有限公司 | Production technology of magnesium alginate |
-
2019
- 2019-02-01 CN CN201910102359.2A patent/CN109678984B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2350097A1 (en) * | 1976-05-05 | 1977-12-02 | Brothier Laboratoires | Micro-fibrillar calcium alginate powder compsn. - for treatment of erythematose dermatological lesions |
| JP3984402B2 (en) * | 1999-10-12 | 2007-10-03 | 株式会社マルイ物産 | Method for producing fucoidan-like polysaccharide complex and immunostimulant based on the same |
| JP2009149734A (en) * | 2007-12-19 | 2009-07-09 | Kao Corp | Production method for alginic acid of low molecular weight or derivative thereof |
| CN102558383A (en) * | 2012-01-10 | 2012-07-11 | 中国科学院海洋研究所 | Bismuth alginate and preparation method and application thereof |
| CN103360510A (en) * | 2013-07-31 | 2013-10-23 | 青岛海之林生物科技开发有限公司 | Production method for alginate specialized for welding |
| CN104844726B (en) * | 2014-02-13 | 2017-02-01 | 青岛海之林生物科技开发有限公司 | Production technology of magnesium alginate |
Non-Patent Citations (2)
| Title |
|---|
| 李进军 等: "《绿色化学导论 2版》", 31 August 2015, 武汉：武汉大学出版社 * |
| 沈玉龙 等: "《绿色化学 3版》", 30 April 2016, 北京：中国环境出版社 * |
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