CN103923036B - A kind of preparation method of bar-shaped methylene blue crystal - Google Patents
A kind of preparation method of bar-shaped methylene blue crystal Download PDFInfo
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- CN103923036B CN103923036B CN201410165084.4A CN201410165084A CN103923036B CN 103923036 B CN103923036 B CN 103923036B CN 201410165084 A CN201410165084 A CN 201410165084A CN 103923036 B CN103923036 B CN 103923036B
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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 kind of preparation method of bar-shaped methylene blue crystal, belong to technical field of chemical raw material production.First nitrocalcite and Secondary ammonium phosphate are dissolved in deionized water respectively and prepare A and B solution, make the mol ratio of nitrocalcite and Secondary ammonium phosphate in two solution be 5:3; Then regulate the pH value of two solution with ammoniacal liquor respectively, then in B solution, add methylene blue, and solution A is added drop-wise to constantly stirred containing methylene blue B solution in.After being added dropwise to complete, the Water Under thermal response 4 hours stirred, more still aging 12 hours.Finally sieved by reaction soln, washing methylene blue screenings at 40 DEG C dry 12 hours, namely prepare bar-shaped methylene blue crystal, length is 0.2 ~ 5 millimeter.The technique that present method adopts is simple, cost of material is low and be easy to suitability for industrialized production.
Description
Technical field
The invention provides a kind of preparation method of bar-shaped methylene blue crystal, belong to technical field of chemical raw material production.
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 the synthesis of product, collection, packaging, transport and the dissolution rate in application process, speed of response and medication effect etc.During as 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, and therefore the residence time of methylene blue in stomach becomes the key factor that its result for the treatment of of restriction improves.Compared to 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 as oral pharmaceutical the optimization realizing its result for the treatment of.Therefore, the preparation of methylene blue crystal seems abnormal important, 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 the preparation method proposing a kind 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 deionized water respectively prepare A and B solution, make the mol ratio of nitrocalcite and Secondary ammonium phosphate be 5:3, regulate the pH value of A and B solution respectively with ammoniacal liquor after, in B solution, add methylene blue;
(2) solution A is added drop-wise to constantly stirred containing in the B solution of methylene blue, and the Water Under thermal response 4 hours stirred after being added dropwise to complete, more still aging 12 hours;
(3) by reaction soln sieving separating, washing screenings at 40 DEG C dry 12 hours, namely prepare bar-shaped methylene blue crystal.
In step (1), in solution A, the concentration of nitrocalcite is 0.5 mole often liter, in B solution, the concentration of Secondary ammonium phosphate is 0.3 mole often liter, the pH value of A and B two solution is regulated to be 8 ~ 10 respectively with ammoniacal liquor, the size of the methylene blue crystal that can regulate and control to prepare by regulating the pH value of A and B solution.The concentration of B solution Methylene Blue is 0.027 ~ 0.053 mole often liter, and optimum concn is 0.053 mole often liter.
Hydrothermal temperature after the middle solution A of step (2) is added dropwise to complete is 60 ~ 80 DEG C, and can regulate and control the generative process of precipitation and crystallization reaction thing in solution by changing temperature of reaction, optimal reaction temperature is 60 DEG C.In hydro-thermal reaction and still aging process, methylene blue crystal is given birth to core gradually and is grown up for rhabdolith.Along with the raising of hydrothermal temperature, the size of crystal diminishes.
Be separated methylene blue crystal by the method for screening in step (3), the methylene blue screenings obtained, through washing and drying, namely prepares bar-shaped methylene blue crystal.
Beneficial effect of the present invention is:
1. the preparation of crystal utilizes chemical reagent cheap and easy to get as reactant, and production cost is low, and the device needed for preparation is simple and easy, is easy to suitability for industrialized production;
2. the chemical reagent selected by can be used safely, little to the toxicity of human body, environmental pollution is few;
3. obtained bar-shaped methylene blue crystal regulates and controls its size by the pH value and hydrothermal temperature changing initial reaction solution, and its size range is 0.2 ~ 5 millimeter, conveniently can realize the granularity processing of methylene blue.
Accompanying drawing explanation
Fig. 1 is the optical microscope photograph of bar-shaped methylene blue crystal prepared by the embodiment of the present invention 1.
Fig. 2 is the optical microscope photograph of bar-shaped methylene blue crystal prepared by the embodiment of the present invention 2.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1:
(1) nitrocalcite and Secondary ammonium phosphate are dissolved in the deionized water of 60 milliliters respectively prepare A and B solution, the concentration of nitrocalcite and Secondary ammonium phosphate is respectively 0.5 and 0.3 mole often liter, then the pH value of A and B solution is regulated to be 10 respectively with ammoniacal liquor, then in B solution, add methylene blue, make the concentration of methylene blue be 0.053 mole often liter;
(2) solution A is added drop-wise to constantly stirred containing in the B solution of methylene blue, stirring reaction 4 hours at 60 DEG C again after being added dropwise to complete, still aging 12 hours;
(3) by reaction soln sieving separating, washing screenings at 40 DEG C dry 12 hours, namely prepare bar-shaped methylene blue crystal.
Opticmicroscope detects product pattern and sees Fig. 1.
Embodiment 2:
(1) nitrocalcite and Secondary ammonium phosphate are dissolved in the deionized water of 60 milliliters respectively prepare A and B solution, the concentration of nitrocalcite and Secondary ammonium phosphate is respectively 0.5 and 0.3 mole often liter, then the pH value of A and B solution is regulated to be 8 respectively with ammoniacal liquor, then in B solution, add methylene blue, make the concentration of methylene blue be 0.053 mole often liter;
(2) solution A is added drop-wise to constantly stirred containing in the B solution of methylene blue, stirring reaction 4 hours at 60 DEG C again after being added dropwise to complete, still aging 12 hours;
(3) by reaction soln sieving separating, washing screenings at 40 DEG C dry 12 hours, namely prepare bar-shaped methylene blue crystal.
Opticmicroscope detects product pattern and sees Fig. 2.
Claims (1)
1. a preparation method for bar-shaped methylene blue crystal, is characterized in that comprising the following steps:
Nitrocalcite and Secondary ammonium phosphate are dissolved in deionized water and prepare A and B solution by step 1. respectively, the concentration of nitrocalcite in solution A is made to be 0.5 mole often liter, in B solution, the concentration of Secondary ammonium phosphate is 0.3 mole often liter, the mol ratio of nitrocalcite and Secondary ammonium phosphate is 5:3, then pH value to 8 ~ 10 of A and B solution are regulated respectively with ammoniacal liquor, then in B solution, add methylene blue, make the concentration of B solution Methylene Blue be 0.027 ~ 0.053 mole often liter;
Step 2. solution A is added drop-wise to constantly stirred containing in the B solution of methylene blue, the Water Under thermal response 4 hours stirred after being added dropwise to complete, the temperature of hydro-thermal reaction is 60 ~ 80 DEG C, more still aging 12 hours;
Step 3., by reaction soln sieving separating, after washing screenings and at 40 DEG C dry 12 hours, namely prepares bar-shaped methylene blue crystal.
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| Application Number | Priority Date | Filing Date | Title |
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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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| CN103923036B true CN103923036B (en) | 2015-09-16 |
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| 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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| WO2009044127A1 (en) * | 2007-10-03 | 2009-04-09 | Wista Laboratories Ltd. | Therapeutic use of diaminophenothiazines |
| CN101624182A (en) * | 2008-07-11 | 2010-01-13 | 北京化工大学 | Method for preparing hydroxylapatite ultrafine powder |
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| CN103071447A (en) * | 2013-02-05 | 2013-05-01 | 东华大学 | Method for preparing strontium-doped hydroxyapatite through supersound |
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