CN103923036A - Preparation method of rod-shaped methylene blue crystal - Google Patents
Preparation method of rod-shaped methylene blue crystal Download PDFInfo
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- CN103923036A CN103923036A CN201410165084.4A CN201410165084A CN103923036A CN 103923036 A CN103923036 A CN 103923036A CN 201410165084 A CN201410165084 A CN 201410165084A CN 103923036 A CN103923036 A CN 103923036A
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- methylene blue
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D279/00—Heterocyclic compounds containing six-membered rings having one nitrogen atom and one sulfur atom as the only ring hetero atoms
- C07D279/10—1,4-Thiazines; Hydrogenated 1,4-thiazines
- C07D279/14—1,4-Thiazines; Hydrogenated 1,4-thiazines condensed with carbocyclic rings or ring systems
- C07D279/18—[b, e]-condensed with two six-membered rings
- C07D279/20—[b, e]-condensed with two six-membered rings with hydrogen atoms directly attached to the ring nitrogen atom
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Abstract
The invention provides a preparation method of a rod-shaped methylene blue crystal and belongs to the technical field of production of chemical raw materials. The preparation method comprises the following steps: firstly, respectively dissolving calcium nitrate and ammonium monoacid phosphate in de-ionized water so as to prepare a solution A and a solution B, wherein the mol ratio of calcium nitrate to ammonium monoacid phosphate in the two solutions is 5:3; respectively regulating the pH values of the two solutions by use of ammonia, then adding methylene blue into the solution B, and dropwise adding the solution A into the constantly-stirred solution B containing methylene blue; after dropwise adding the solution A, performing hydrothermal reaction for 4 hours under a stirring condition, and then standing and aging for 12 hours; and finally sieving a reaction solution, washing a methylene blue oversize product, and drying at a temperature of 40 DEG C for 12 hours, thereby obtaining the rod-shaped methylene blue crystal with the length of 0.2-5mm. The method is simple in process, low in raw material price and easy for industrial production.
Description
Technical field
The invention provides a kind of preparation method of bar-shaped methylene blue crystal, belong to industrial chemicals production technical field.
Background technology
Methylene blue is widely used in fields such as dyeing, photochemical reaction and disease treatments, its size and dimension has a certain impact to the production technique of methylene blue and physical and chemical performance, comprises synthesizing, collect, pack, transporting and the dissolution rate in application process, speed of response and medication effect etc. of product.When applied as oral pharmaceutical, methylene blue is allowed for access in blood after need being reduced in stomach, realizes its result for the treatment of, so the residence time of methylene blue in stomach becomes the key factor that its result for the treatment of of restriction improves.Than methylene blue solution, the methylene blue crystal residence time under one's belt will extend greatly, and the time that molecule discharges from crystals also extends greatly, can realize slow releasing effect.If adopt methylene blue crystal to be expected to realize the optimization of its result for the treatment of as oral pharmaceutical.Therefore, it is extremely important that the preparation of methylene blue crystal seems, and up to the present, the preparation method of methylene blue crystal has no report.
Summary of the invention
The object of the invention is to propose a kind of preparation method of bar-shaped methylene blue crystal, for achieving the above object, the technical solution adopted in the present invention step is as follows:
(1) nitrocalcite and Secondary ammonium phosphate are dissolved in respectively in deionized water and prepare A and B solution, the mol ratio that makes nitrocalcite and Secondary ammonium phosphate is 5:3, regulates respectively after the pH value of A and B solution with ammoniacal liquor, in B solution, adds methylene blue;
(2) A solution is added drop-wise to continuous stirring containing in the B solution of methylene blue, and after being added dropwise to complete the Water Under thermal response stirring 4 hours, more still aging 12 hours;
(3), by reaction soln sieving separating, washing screenings is also dried 12 hours at 40 ℃, prepares bar-shaped methylene blue crystal.
In step (1), in A solution, the concentration of nitrocalcite is 0.5 mole every liter, in B solution, the concentration of Secondary ammonium phosphate is 0.3 mole every liter, with ammoniacal liquor, regulating respectively the pH value of A and B two solution is 8 ~ 10, by regulating the size of the methylene blue crystal that the pH value of A and B solution can regulate and control to prepare.The concentration of B Methylene Blue in Solution is 0.027 ~ 0.053 mole every liter, and optimum concn is 0.053 mole every liter.
The hydrothermal temperature of A solution after being added dropwise to complete is 60 ~ 80 ℃ in step (2), can regulate and control the generative process of precipitation and crystallization reaction thing in solution by changing temperature of reaction, and optimal reaction temperature is 60 ℃.In hydro-thermal reaction and still aging process, methylene blue crystal is raw core growing up for rhabdolith gradually.Along with the raising of hydrothermal temperature, the size decreases of crystal.
In step (3), by the separated methylene blue crystal of method of screening, the methylene blue screenings obtaining, through washing and dry, prepares bar-shaped methylene blue crystal.
Beneficial effect of the present invention is:
1. the preparation of crystal is to utilize chemical reagent cheap and easy to get as reactant, and production cost is low, prepares required device simple and easy, is easy to suitability for industrialized production;
Selected chemical reagent can use safely, little to the toxicity of human body, environmental pollution is few;
3. the bar-shaped methylene blue crystal that obtained can regulate and control its size by changing pH value and the hydrothermal temperature of initial reaction solution, and its size range is 0.2 ~ 5 millimeter, can conveniently realize the granularity processing of methylene blue.
Accompanying drawing explanation
Fig. 1 is the optical microscope photograph of the bar-shaped methylene blue crystal of the embodiment of the present invention 1 preparation.
Fig. 2 is the optical microscope photograph of the bar-shaped methylene blue crystal of the embodiment of the present invention 2 preparations.
Embodiment
Below in conjunction with embodiment, further illustrate the present invention.
Embodiment 1:
(1) nitrocalcite and Secondary ammonium phosphate are dissolved in respectively in the deionized water of 60 milliliters and prepare A and B solution, the concentration of nitrocalcite and Secondary ammonium phosphate is respectively 0.5 and 0.3 mole every liter, then with ammoniacal liquor, regulating respectively the pH value of A and B solution is 10, then in B solution, add methylene blue, the concentration that makes methylene blue is 0.053 mole every liter;
(2) A solution is added drop-wise to continuous stirring containing in the B solution of methylene blue, stirring reaction 4 hours at 60 ℃ again after being added dropwise to complete, still aging 12 hours;
(3), by reaction soln sieving separating, washing screenings is also dried 12 hours at 40 ℃, prepares bar-shaped methylene blue crystal.
Opticmicroscope detects product pattern and sees Fig. 1.
Embodiment 2:
(1) nitrocalcite and Secondary ammonium phosphate are dissolved in respectively in the deionized water of 60 milliliters and prepare A and B solution, the concentration of nitrocalcite and Secondary ammonium phosphate is respectively 0.5 and 0.3 mole every liter, then with ammoniacal liquor, regulating respectively the pH value of A and B solution is 8, then in B solution, add methylene blue, the concentration that makes methylene blue is 0.053 mole every liter;
(2) A solution is added drop-wise to continuous stirring containing in the B solution of methylene blue, stirring reaction 4 hours at 60 ℃ again after being added dropwise to complete, still aging 12 hours;
(3), by reaction soln sieving separating, washing screenings is also dried 12 hours at 40 ℃, prepares bar-shaped methylene blue crystal.
Opticmicroscope detects product pattern and sees Fig. 2.
Claims (5)
1. a preparation method for bar-shaped methylene blue crystal, is characterized in that comprising the following steps:
Step 1. is dissolved in nitrocalcite and Secondary ammonium phosphate respectively in deionized water and prepares A and B solution, and the mol ratio that makes nitrocalcite and Secondary ammonium phosphate is 5:3, then with ammoniacal liquor, regulates respectively the pH value of A and B solution, then in B solution, adds methylene blue;
Step 2. by A solution be added drop-wise to continuous stirring containing in the B solution of methylene blue, after being added dropwise to complete the Water Under thermal response stirring 4 hours, more still aging 12 hours;
Step 3., by reaction soln sieving separating, is dried 12 hours after washing screenings and at 40 ℃, prepares bar-shaped methylene blue crystal.
2. the preparation method of a kind of bar-shaped methylene blue crystal according to claim 1, is characterized in that: in step 1, in A solution, the concentration of nitrocalcite is 0.5 mole every liter, and in B solution, the concentration of Secondary ammonium phosphate is 0.3 mole every liter.
3. the preparation method of a kind of bar-shaped methylene blue crystal according to claim 1, is characterized in that: in step 1, utilize ammoniacal liquor respectively the pH value of A and B solution to be adjusted to 8 ~ 10.
4. the preparation method of a kind of bar-shaped methylene blue crystal according to claim 1, is characterized in that: in step 1, the concentration of B Methylene Blue in Solution is 0.027 ~ 0.053 mole every liter.
5. the preparation method of a kind of bar-shaped methylene blue crystal according to claim 1, is characterized in that: in step 2, the temperature of hydro-thermal reaction is 60 ~ 80 ℃.
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| CN201410165084.4A CN103923036B (en) | 2014-04-24 | 2014-04-24 | A kind of preparation method of bar-shaped methylene blue crystal |
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| CN201410165084.4A CN103923036B (en) | 2014-04-24 | 2014-04-24 | A kind of preparation method of bar-shaped methylene blue crystal |
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| CN103923036A true CN103923036A (en) | 2014-07-16 |
| CN103923036B CN103923036B (en) | 2015-09-16 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370574A (en) * | 2018-12-11 | 2019-02-22 | 山东理工大学 | There is the method for the silicon/carbon dioxide composite particles containing methylene blue of high fluorescent using hydro-thermal method preparation |
| CN109456755A (en) * | 2018-12-11 | 2019-03-12 | 山东理工大学 | A method of there is the silica dioxide granule containing methylene blue of high fluorescent using hydro-thermal method preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109370574A (en) * | 2018-12-11 | 2019-02-22 | 山东理工大学 | There is the method for the silicon/carbon dioxide composite particles containing methylene blue of high fluorescent using hydro-thermal method preparation |
| CN109456755A (en) * | 2018-12-11 | 2019-03-12 | 山东理工大学 | A method of there is the silica dioxide granule containing methylene blue of high fluorescent using hydro-thermal method preparation |
| CN109370574B (en) * | 2018-12-11 | 2021-07-16 | 山东理工大学 | Method for preparing methylene blue-containing silicon dioxide/carbon composite particles with high fluorescence intensity by hydrothermal method |
| CN109456755B (en) * | 2018-12-11 | 2021-07-16 | 山东理工大学 | Method for preparing silicon dioxide particles containing methylene blue and having high fluorescence intensity by hydrothermal method |
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| CN103923036B (en) | 2015-09-16 |
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