CN110642795A - Preparation method for synthesizing nano sulfadiazine copper - Google Patents
Preparation method for synthesizing nano sulfadiazine copper Download PDFInfo
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- CN110642795A CN110642795A CN201911019298.XA CN201911019298A CN110642795A CN 110642795 A CN110642795 A CN 110642795A CN 201911019298 A CN201911019298 A CN 201911019298A CN 110642795 A CN110642795 A CN 110642795A
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- sulfadiazine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
- C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
- C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
- C07D239/69—Benzenesulfonamido-pyrimidines
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Abstract
The invention relates to a preparation method for synthesizing nano sulfadiazine copper, which solves the problem of large particle size of the existing nano sulfadiazine copper and adopts the technical scheme that a copper ammonia complex solution is slowly added into a sulfadiazine ammonia salt solution in a mode of feeding and stirring for reaction, the reaction temperature is controlled to be 20 ~ 30 ℃, the filtration is carried out immediately after the reaction is carried out for 3-5 minutes, the filtered sulfadiazine copper is added into distilled water and repeatedly cleaned until the PH of the filtrate is 7, then the washed sulfadiazine copper powder is pre-frozen to be below the eutectic point temperature, the pre-frozen sulfadiazine copper is placed into a drying chamber of a vacuum freeze dryer for drying, and a sample is taken out after the pre-frozen sulfadiazine copper is completely dried and is packaged in vacuum.
Description
Technical Field
The invention relates to a preparation method for synthesizing nano sulfadiazine copper.
Background
Copper sulfadiazine is tasteless and green crystalline powder obtained by reacting sulfadiazine ammonium salt with copper complex. Copper sulfadiazine is insoluble in water, ethanol, chloroform and ether, and is soluble in dilute hydrochloric acid and ammonia solution.
The existing preparation method of copper sulfadiazine is mainly a hot air drying method, the obtained copper sulfadiazine powder has relatively large particle size and is easy to agglomerate, so that the absorption effect of a human body on drugs is poor, and high-temperature drying can cause certain influence on the activity of the drugs, thereby greatly limiting the absorption of the human body on drug properties.
Disclosure of Invention
In view of the above, the invention provides a preparation method for synthesizing nano copper sulfadiazine, which solves the problem of large particle size of the existing nano copper sulfadiazine.
In order to solve the problems in the prior art, the technical scheme of the invention is as follows: a preparation method for synthesizing nano sulfadiazine copper is characterized by comprising the following steps:
slowly adding a copper-ammonia complex solution into a sulfadiazine ammonia salt solution in a mode of feeding and stirring at the same time for reaction, controlling the reaction temperature to be 20 ~ 30 ℃, immediately filtering after reacting for 3-5 minutes, adding distilled water into the filtered sulfadiazine copper, repeatedly cleaning until the pH of filtrate is 7, then pre-freezing the washed sulfadiazine copper powder to be below the eutectic temperature, placing the pre-frozen sulfadiazine copper in a drying chamber of a vacuum freeze dryer for drying, taking out a sample after completely drying, and carrying out vacuum packaging.
The pre-freezing method is divided into 3 methods,
the first one is: pre-freezing in a refrigerator at the temperature of minus 20 ℃;
the second method comprises pre-freezing at-50 deg.C ~ -60 deg.C in cold trap;
the third is: vacuumizing and freezing.
The sulfadiazine ammonia salt solution is obtained by dissolving sulfadiazine in dilute ammonia water.
The copper ammonia complex solution is obtained by the reaction of copper sulfate solution and dilute ammonia water.
Compared with the prior art, the invention has the following advantages:
1. the invention controls the pre-freezing rate, and the prepared nano sulfadiazine copper powder has small particle size and can not generate agglomeration;
2. the invention adopts low-temperature freeze drying, so that the prepared sulfadiazine copper powder has good biological activity and the drug effect is ensured;
3. the drying of the material is finished in a frozen state, so that the physical structure and the molecular structure of the material are changed little, and the organization structure and the appearance form of the material are completely preserved.
Description of the drawings:
FIGS. 1(a) (b) show TEM micrographs of copper sulfadiazine powder prepared in example 1;
FIG. 2(a) (b) shows TEM electron micrographs of copper sulfadiazine powder prepared in example 2;
FIGS. 3(a) (b) show TEM micrographs of copper sulfadiazine powder prepared in example 3.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The first embodiment is as follows:
the preparation method for synthesizing the nano sulfadiazine copper comprises the following steps:
step 1: preparation of sulfadiazine ammonia salt solution
Weighing 10g of sulfadiazine powder, dissolving the sulfadiazine powder in 25ml of 10% dilute ammonia water at the reaction temperature of 25 ℃ to obtain light yellow transparent liquid, namely sulfadiazine ammonia salt;
step 2: preparation of copper ammine complex solution
Weighing 5g of blue vitriol, dissolving with distilled water to obtain a blue vitriol solution, adding about 20ml of 10% diluted ammonia water, and reacting at 25 deg.C to obtain a clear solution, i.e. a copper ammonia complex solution;
and step 3: synthesis of copper sulfadiazine
Slowly adding the copper-ammonia complex solution into the sulfadiazine ammonium salt solution in a manner of feeding and stirring at 25 ℃, and immediately filtering after reacting for 4 minutes;
and 4, step 4: washing, precipitating and pre-freezing
Adding filtered copper sulfadiazine into distilled water, repeatedly washing until the pH value of the filtrate is 7, placing the washed copper sulfadiazine in a refrigerator at the temperature of-20 ℃ for pre-freezing for about 90 minutes (the freezing standard is that the temperature of the experimental materials is lower than the eutectic point);
and 5: drying
And then placing the sulfadiazine copper which is pre-frozen in the refrigerator into a drying chamber of a vacuum freeze dryer for drying, wherein the pressure of the drying chamber is about 3Pa, and the drying time is 12 hours.
The TEM electron micrographs of the nano copper sulfadiazine powder prepared by the method are shown in figures 1(a) and (b).
Example two:
step 1: preparation of sulfadiazine ammonia salt solution
Weighing 10g of sulfadiazine powder, dissolving in 25ml of 10% dilute ammonia water, and reacting at 30 ℃ to obtain light yellow transparent liquid, namely sulfadiazine ammonia salt.
Step 2: preparation of copper ammine complex solution
Weighing 5g of blue vitriol, dissolving with distilled water to obtain a blue vitriol solution, adding about 20ml of 10% diluted ammonia water, and reacting at 30 deg.C to obtain a clear solution, i.e. a copper ammonia complex solution.
And step 3: synthesis of copper sulfadiazine
Slowly adding the copper-ammonia complex solution into the sulfadiazine ammonium salt solution while stirring, controlling the reaction temperature at 30 ℃, and immediately filtering after reacting for 3 minutes;
and 4, step 4: washing, precipitating and pre-freezing
Adding filtered copper sulfadiazine into distilled water, repeatedly cleaning until the pH value of the filtrate is about 7, placing the washed copper sulfadiazine in a cold trap at-55 ℃ for pre-freezing for about 1 hour (the freezing standard is that the temperature of experimental materials is lower than the eutectic point);
and 5: vacuum drying
And then placing the sulfadiazine copper which is pre-frozen in the cold trap into a drying chamber of a vacuum freeze dryer for drying, wherein the pressure of the drying chamber is about 3Pa, and the drying time is 12 hours.
The TEM electron micrographs of the nano copper sulfadiazine powder prepared by the method are shown in FIGS. 2(a) and (b).
Example three:
step 1: preparation of sulfadiazine ammonia salt solution
Weighing 10g of sulfadiazine powder, dissolving in 25ml of 10% dilute ammonia water, and reacting at 20 ℃ to obtain light yellow transparent liquid, namely sulfadiazine ammonia salt.
Step 2: preparation of copper ammine complex solution
Weighing 5g of blue vitriol, dissolving with distilled water to obtain a blue vitriol solution, adding about 20ml of 10% diluted ammonia water, and reacting at 20 ℃ to obtain a clear solution, namely the copper ammonia complex solution.
And step 3: synthesis of copper sulfadiazine
Slowly adding the copper-ammonia complex solution into the sulfadiazine ammonium salt solution while stirring, controlling the reaction temperature at 20 ~ 30 ℃, and immediately filtering after reacting for 5 minutes;
and 4, step 4: washing the precipitate with water
Adding the filtered sulfadiazine copper into distilled water, and repeatedly cleaning until the pH value of the filtrate is about 7;
and 5: vacuum-pumping freezing and vacuum drying
And (3) reducing the temperature of a cold trap of a vacuum refrigerator to-55 ℃, and then placing the washed sulfadiazine copper in a drying chamber of a vacuum freeze dryer for vacuumizing, freeze drying, wherein the pressure of the drying chamber is about 3Pa, and the drying time is 12 hours.
The TEM electron micrographs of the nano copper sulfadiazine powder prepared by the method are shown in FIGS. 3(a) and (b).
The electron microscope images show that the sulfadiazine copper powder prepared by the method is square flaky particles, the thickness of each flaky particle is about 50-100nm, the length of each flaky particle is 500nm-2 mu m, strip-shaped linear particles are vertically arranged on a copper film in the images, and the deeper particles in the images are electron microscope images generated by thicker flakes or stacked flakes. The method can prepare nano powder, and compared with the powder prepared by the traditional hot air drying method, the nano powder has smaller particle size and relatively better dispersity and is not easy to agglomerate and agglomerate.
The sulfadiazine powder used in the invention is produced by Shanghai Aladdin Biotechnology GmbH.
The copper sulfate used in the present invention is produced by the maotai chemical reagent factory in Tianjin.
The ammonia water used in the invention is produced by Dacron chemical reagent factory in Tianjin.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the scope of the present invention, and it should be noted that those skilled in the art should make modifications and variations without departing from the principle of the present invention.
Claims (4)
1. A preparation method for synthesizing nano sulfadiazine copper is characterized by comprising the following steps:
slowly adding a copper-ammonia complex solution into a sulfadiazine ammonia salt solution in a mode of feeding and stirring at the same time for reaction, controlling the reaction temperature to be 20 ~ 30 ℃, immediately filtering after reacting for 3-5 minutes, adding distilled water into the filtered sulfadiazine copper, repeatedly cleaning until the pH of filtrate is 7, then pre-freezing the washed sulfadiazine copper powder to be below the eutectic temperature, placing the pre-frozen sulfadiazine copper in a drying chamber of a vacuum freeze dryer for drying, taking out a sample after completely drying, and carrying out vacuum packaging.
2. The preparation method of the synthetic nano sulfadiazine copper according to claim 1, is characterized in that: the pre-freezing method is divided into 3 methods,
the first one is: pre-freezing in a refrigerator at the temperature of minus 20 ℃;
the second method comprises pre-freezing at-50 deg.C ~ -60 deg.C in cold trap;
the third is: vacuumizing and freezing.
3. The preparation method of the synthetic nano sulfadiazine copper according to the claim 1 or 2, is characterized in that: the sulfadiazine ammonia salt solution is obtained by dissolving sulfadiazine in dilute ammonia water.
4. The preparation method of the synthetic nano sulfadiazine copper according to claim 3, is characterized in that: the copper ammonia complex solution is obtained by the reaction of copper sulfate solution and dilute ammonia water.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203229A (en) * | 1998-05-29 | 1998-12-30 | 郑州铁路局武汉中心医院 | Sulfadiazine copper and its preparing process and medicine thereof |
| CN102552968A (en) * | 2012-02-13 | 2012-07-11 | 江苏天麟生物医药科技有限公司 | Method for preparing hyaluronic acid and collagen compound burn biomembrane |
| CN105949134A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfadiazine iron palladium nano-composite particle and preparation method thereof |
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- 2019-10-24 CN CN201911019298.XA patent/CN110642795A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1203229A (en) * | 1998-05-29 | 1998-12-30 | 郑州铁路局武汉中心医院 | Sulfadiazine copper and its preparing process and medicine thereof |
| CN102552968A (en) * | 2012-02-13 | 2012-07-11 | 江苏天麟生物医药科技有限公司 | Method for preparing hyaluronic acid and collagen compound burn biomembrane |
| CN105949134A (en) * | 2016-04-29 | 2016-09-21 | 宁波大学 | Sulfadiazine iron palladium nano-composite particle and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 张友智等: "磺胺嘧啶铜的合成与质量控制", 《中国药房》 * |
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