CN106700092A - Microwave-assisted method for preparing silver fulvate - Google Patents
Microwave-assisted method for preparing silver fulvate Download PDFInfo
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- CN106700092A CN106700092A CN201611216158.8A CN201611216158A CN106700092A CN 106700092 A CN106700092 A CN 106700092A CN 201611216158 A CN201611216158 A CN 201611216158A CN 106700092 A CN106700092 A CN 106700092A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a microwave-assisted method for preparing silver fulvate, belonging to the technical field of medicine preparation. The method comprises the following steps: a) preparing a fulvic acid solution and a Gemini surfactant solution, dissolving silver nitrate in deionized water to prepare a silver nitrate solution, and adding the silver nitrate solution into aqua ammonia while stirring, thereby forming a diammine silver solution; b) dropwisely adding the fulvic acid solution and Gemini surfactant solution into the diammine silver solution under microwave conditions, and mixing to react; and c) after the reaction finishes, carrying out solid-liquid separation, and carrying out freeze-drying on the obtained solid precipitate to obtain the silver fulvate. The method disclosed by the invention has the advantages of simple technique, low cost and high production efficiency, and is a novel preparation method of silver fulvate. The obtained product can slowly release silver, the silver has the effects of killing germs and accelerating wound healing and has the actions of alleviating pain, arresting bleeding and diminishing inflammation, and thus, the product has wide application prospects in industries of medicine, health products and cosmetics.
Description
Technical field
The present invention relates to a kind of method that microwave radiation technology prepares fulvic acid silver, belong to technical field of medicine preparation.
Background technology
People have just recognized the bioactivity of humic acid substance very early, and have certain at the aspect such as agricultural and medical treatment
Using.Fulvic acid is active stronger composition in humic acid substance.The 1950's external beginning system research, 20th century
At the end of the seventies, China worker begins one's study fulvic acid bioactivity and its application.Fulvic acid is clinically either as controlling
The main pharmacodynamics composition of medicine is treated still as the stabilizer of effective ingredient, synergist and sustained release agent etc., there is exploitation to answer
With value and development prospect.And fulvic acid silver products can slowly discharge silver, silver has functions that sterilized, quickening wound healing, together
When fulvic acid there is analgesic, convergence, the effect of anti-inflammatory, therefore fulvic acid silver is before medicine, health products and cosmetic industry application
Scape is more wide.
The content of the invention
In view of this, the method that a kind of microwave radiation technology of the invention prepares fulvic acid silver, process is simple, low cost, production
Efficiency high, is a kind of preparation method of new fulvic acid silver, and the product for obtaining can slowly discharge silver, and silver has sterilized, quickening
Effect of wound healing, while there is the effect of analgesic, convergence, anti-inflammatory, in medicine, health products and cosmetic industry application prospect
It is wide.
The present invention solves above-mentioned technical problem by following technological means：
The method that a kind of microwave radiation technology of the invention prepares fulvic acid silver, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 10-20%, double lauryl alcohol polyethylene glycol oxide (9) esters of oxalamide butanedioic acid in fulvic acid solution
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 1-10%, silver nitrate in sodium sulfonate solution
The mass fraction of silver nitrate is 5-10% in solution.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 3-10mol/L, reaction temperature
It it is 10-50 DEG C, mixing speed is 200-500 r/min, ammonia is 3-6 with the mol ratio of silver ion:1, final two amminos silver solution
The concentration of middle free ammonia is 1-4mol/L, and the two amminos silver solution for obtaining after filtering by using.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 200-500r/min, two amminos
The rate of addition of silver is 5-50ml/min, and the pH value of two amminos silver solution is 8-13, microwave power 100-200w, reaction temperature
70-90 DEG C, time 10-20min.
In step c) separation of solid and liquid uses centrifugation, and 2000-3000rpm is reported in centrifugation, during freeze-drying
Between 24-48h, temperature be-10-20 DEG C, pressure is 1-20Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Beneficial effects of the present invention：
1）Preparation process is simple, low cost, production efficiency is high.Fulvic acid solution and Gemini surface active agent solution are mixed, so
After prepare two amminos silver solution, both mix can prepare fulvic acid silver, be prepared using conventional liquid phase synthesis process, work
Skill is simple, low cost, while being prepared into nitrate solution again after a small amount of unprecipitated silver ion is recyclable, reduce further into
This, using freeze-drying, dries fulvic acid silver, it is to avoid the thermal decomposition under high temperature, while also improving drying efficiency at low temperature.
2）The fulvic acid silver products country there is no relevant report, due to the fulvic acid silver characteristic of itself, can slowly discharge silver,
Silver has functions that sterilized, quickening wound healing, while fulvic acid has analgesic, convergence, the effect of anti-inflammatory, therefore fulvic acid silver exists
Medicine, health products and cosmetic industry have a extensive future.
3）Because silver ion is added in the form of silver ammonia complex, so that the combination of fulvic acid and silver ion is very slow
Slowly, while introducing surfactant, the precipitation particle for obtaining is closely knit and particle is big, and good dispersion can slowly discharge silver, effect
Persistently.
Brief description of the drawings
The invention will be further described with reference to the accompanying drawings and examples.
Fig. 1 is process chart of the invention.
Specific embodiment
Below with reference to accompanying drawing, the present invention is described in detail, as shown in Figure 1：A kind of microwave radiation technology prepares fulvic acid silver
Method, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 10-20%, double lauryl alcohol polyethylene glycol oxide (9) esters of oxalamide butanedioic acid in fulvic acid solution
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 1-10%, silver nitrate in sodium sulfonate solution
The mass fraction of silver nitrate is 5-10% in solution.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 3-10mol/L, reaction temperature
It it is 10-50 DEG C, mixing speed is 200-500 r/min, ammonia is 3-6 with the mol ratio of silver ion:1, final two amminos silver solution
The concentration of middle free ammonia is 1-4mol/L, and the two amminos silver solution for obtaining after filtering by using.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 200-500r/min, two amminos
The rate of addition of silver is 5-50ml/min, and the pH value of two amminos silver solution is 8-13, microwave power 100-200w, reaction temperature
70-90 DEG C, time 10-20min
In step c) separation of solid and liquid uses centrifugation, and 2000-3000rpm, sublimation drying 24- are reported in centrifugation
48h, temperature is-10-20 DEG C, and pressure is 1-20Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Embodiment one
A kind of method that microwave radiation technology prepares fulvic acid silver, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 20% in fulvic acid solution, double lauryl alcohol polyethylene glycol oxide (9) the ester sulphurs of oxalamide butanedioic acid
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 1%, silver nitrate solution in acid sodium solution
The mass fraction of middle silver nitrate is 5%.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 4mol/L, and reaction temperature is
30 DEG C, mixing speed is 200 r/min, and ammonia is 6 with the mol ratio of silver ion:1, free ammonia is dense in final two amminos silver solution
It is 4mol/L to spend, and the two amminos silver solution for obtaining after filtering by using.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 200r/min, two amminos silver
Rate of addition is 5ml/min, and the pH value of two amminos silver solution is 9, microwave power 100w, 80 DEG C of reaction temperature, time 15min
In step c) separation of solid and liquid uses centrifugation, and 2000rpm, sublimation drying 36h, temperature are reported in centrifugation
It it is -15 DEG C, pressure is 10Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Embodiment two
A kind of method that microwave radiation technology prepares fulvic acid silver, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 20% in fulvic acid solution, double lauryl alcohol polyethylene glycol oxide (9) the ester sulphurs of oxalamide butanedioic acid
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 1%, silver nitrate solution in acid sodium solution
The mass fraction of middle silver nitrate is 5%.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 4mol/L, and reaction temperature is
30 DEG C, mixing speed is 300 r/min, and ammonia is 4 with the mol ratio of silver ion:1, free ammonia is dense in final two amminos silver solution
It is 2mol/L to spend, and the two amminos silver solution for obtaining after filtering by using.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 200r/min, two amminos silver
Rate of addition is 10ml/min, and the pH value of two amminos silver solution is 9, microwave power 200w, 70 DEG C of reaction temperature, time 20min
In step c) separation of solid and liquid uses centrifugation, and 2000rpm, sublimation drying 24h, temperature are reported in centrifugation
It it is -18 DEG C, pressure is 15Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Embodiment three
A kind of method that microwave radiation technology prepares fulvic acid silver, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 10% in fulvic acid solution, double lauryl alcohol polyethylene glycol oxide (9) the ester sulphurs of oxalamide butanedioic acid
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 1%, silver nitrate solution in acid sodium solution
The mass fraction of middle silver nitrate is 10%.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 5mol/L, and reaction temperature is
35 DEG C, mixing speed is 300 r/min, and ammonia is 5 with the mol ratio of silver ion:1, free ammonia is dense in final two amminos silver solution
It is 3mol/L to spend, and the two amminos silver solution for obtaining after filtering by using.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 200r/min, two amminos silver
Rate of addition is 5ml/min, and the pH value of two amminos silver solution is 10, microwave power 200w, 90 DEG C of reaction temperature, time 10min
In step c) separation of solid and liquid uses centrifugation, and 3000rpm, sublimation drying 32h, temperature are reported in centrifugation
It it is -12 DEG C, pressure is 12Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Example IV
A kind of method that microwave radiation technology prepares fulvic acid silver, it comprises the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid in the step a)
Solution, the mass fraction of fulvic acid is 15% in fulvic acid solution, double lauryl alcohol polyethylene glycol oxide (9) the ester sulphurs of oxalamide butanedioic acid
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of oxalamide butanedioic acid is 5.5% in acid sodium solution, and silver nitrate is molten
The mass fraction of silver nitrate is 7.5% in liquid.
The preparation process of two amminos silver solution in the step a), the concentration of ammonia spirit is 6.5mol/L, reaction temperature
It it is 30 DEG C, mixing speed is 350 r/min, ammonia is 4.5 with the mol ratio of silver ion:1, free ammonia in final two amminos silver solution
Concentration be 2.5mol/L, obtain two amminos silver solution by being used after filtering.
Hybrid reaction is stirred using agitator in the step b), and mixing speed is 350r/min, two amminos silver
Rate of addition is 27ml/min, and the pH value of two amminos silver solution is 12, microwave power 150w, 75 DEG C of reaction temperature, time
15min
In step c) separation of solid and liquid uses centrifugation, and 2500rpm, sublimation drying 36h, temperature are reported in centrifugation
It it is -17 DEG C, pressure is 11Pa.
Filtrate after centrifugation in step c) adds sulfide precipitation filtering, and the sediment for obtaining after roasting by adding
Enter nitric acid dissolving, so as to obtain silver nitrate solution, used in return to step a).
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to skill of the invention
Art scheme is modified or equivalent, and without deviating from the objective and scope of technical solution of the present invention, it all should cover at this
In the middle of the right of invention.
Claims (6)
1. a kind of method that microwave radiation technology prepares fulvic acid silver, it is characterised in that comprise the following steps：
A) fulvic acid solution and Gemini surface active agent solution are prepared, silver nitrate is dissolved in into deionized water, and to be configured to silver nitrate molten
, be added to silver nitrate solution in ammonia spirit under agitation by liquid, forms two amminos silver solution；
B) fulvic acid solution, Gemini surface active agent solution are added drop-wise in two amminos silver solution under microwave condition, hybrid reaction；
C) reaction terminates rear separation of solid and liquid, and the solids of sedimentation for obtaining obtains fulvic acid silver by freeze-drying.
2. the method that a kind of microwave radiation technology as claimed in claim 1 prepares fulvic acid silver, it is characterised in that：In the step a)
Gemini surface active agent is double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonate solutions of oxalamide butanedioic acid, rich in fulvic acid solution
In the mass fraction of acid be 10-20%, oxalyl in double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonate solutions of oxalamide butanedioic acid
The mass fraction of double lauryl alcohol polyethylene glycol oxide (9) the ester sodium sulfonates of amine butanedioic acid is 1-10%, the quality of silver nitrate in silver nitrate solution
Fraction is 5-10%.
3. the method that a kind of microwave radiation technology as claimed in claim 1 prepares fulvic acid silver, it is characterised in that：In the step a)
The preparation process of two amminos silver solution, the concentration of ammonia spirit is 3-10mol/L, and reaction temperature is 10-50 DEG C, and mixing speed is
200-500 r/min, ammonia is 3-6 with the mol ratio of silver ion:1, the concentration of free ammonia is 1- in final two amminos silver solution
4mol/L, the two amminos silver solution for obtaining after filtering by using.
4. the method that a kind of microwave radiation technology as claimed in claim 1 prepares fulvic acid silver, it is characterised in that：In the step b)
Hybrid reaction is stirred using agitator, and mixing speed is 200-500r/min, and the rate of addition of two amminos silver is 5-50ml/
Min, the pH value of two amminos silver solution is 8-13, microwave power 100-200w, 70-90 DEG C of reaction temperature, time 10-20min.
5. the method that a kind of microwave radiation technology as claimed in claim 1 prepares fulvic acid silver, it is characterised in that：It is solid in step c)
Liquid is separated and uses centrifugation, and 2000-3000rpm is reported in centrifugation, sublimation drying 24-48h, and temperature is-10-
20 DEG C, pressure is 1-20Pa.
6. the method that a kind of microwave radiation technology as claimed in claim 1 prepares fulvic acid silver, it is characterised in that：In step c) from
Filtrate after the heart is separated adds sulfide precipitation filtering, and the sediment for obtaining dissolves by addition nitric acid after roasting, so as to obtain
Silver nitrate solution, uses in return to step a).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511015271 | 2015-12-31 | ||
| CN2015110152715 | 2015-12-31 |
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| Publication Number | Publication Date |
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| CN106700092A true CN106700092A (en) | 2017-05-24 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611216158.8A Pending CN106700092A (en) | 2015-12-31 | 2016-12-26 | Microwave-assisted method for preparing silver fulvate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021090038A1 (en) * | 2019-11-06 | 2021-05-14 | Ioi Investment Zrt. | Process for production of formic acid and acetic acid by absorbing co2 via photocatalytic reduction, improved catalyst and apparatus |
| CN115627069A (en) * | 2022-10-22 | 2023-01-20 | 营口理工学院 | Modified nano magnesium hydroxide composite flame-retardant nylon 66 and preparation method thereof |
-
2016
- 2016-12-26 CN CN201611216158.8A patent/CN106700092A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021090038A1 (en) * | 2019-11-06 | 2021-05-14 | Ioi Investment Zrt. | Process for production of formic acid and acetic acid by absorbing co2 via photocatalytic reduction, improved catalyst and apparatus |
| CN115627069A (en) * | 2022-10-22 | 2023-01-20 | 营口理工学院 | Modified nano magnesium hydroxide composite flame-retardant nylon 66 and preparation method thereof |
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Application publication date: 20170524 |