CN102321065A - Preparation method of water-soluble bromcresol green - Google Patents
Preparation method of water-soluble bromcresol green Download PDFInfo
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- CN102321065A CN102321065A CN201110226707A CN201110226707A CN102321065A CN 102321065 A CN102321065 A CN 102321065A CN 201110226707 A CN201110226707 A CN 201110226707A CN 201110226707 A CN201110226707 A CN 201110226707A CN 102321065 A CN102321065 A CN 102321065A
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Abstract
The invention relates to a preparation method of water-soluble bromcresol green. The preparation method comprises the following steps of: firstly preparing bromcresol green, then adding 500g of prepared bromcresol green to a sodium hydroxide solution for dissolving fully, stirring at the temperature of 80 DEG C for 2 hours, filtering the solution, and concentrating and drying the filtrate, thus obtaining a brownish red metal-luster crystal finished product namely the water-soluble bromcresol green. The indicator prepared by the preparation method provided by the invention has the advantages of narrow color change range, sensitive color change, high purity and few impurities; and the preparation method is simple to operate and is suitable for industrial application.
Description
Technical field
The invention belongs to the chemical tracer field, be specifically related to a kind of preparation method of water-soluble tetrabromo-mcresolsulfonphthalein.
Background technology
Acid typically refers to the one type of material that is accompanied by colour-change along with the change of pH value of solution value.Be the indispensable chemical substance of chemical analysis field, this tell-tale variation is actual to be the result of a kind of " tautomer " structural changes.
This tautomer has the character of conjugate acid-base pair, is in a kind of equilibrium state each other.The pH value just can influence their balance when changing, balance moves and be attended by the change of structure, the mutual conversion of the acid or the alkali formula of proton occurred losing or obtaining.The indicator of this moment is the pH indicator of our research just.
In practical application, hope that usually the transformation region of indicator is narrower good, even pH value of solution has less variation also can make indicator produce sharp variation like this.
In order to improve the sharp degree of indicator, what research made new advances forms complexing and produces the indicator of colour-change weak acid and weak base and some specific trace metal ion, becomes the emphasis of our research.
Water-soluble indicator is also referred to as sodium salt, and development research indicator sodium salt kind is a kind of change, also is a kind of needs of market.Water-soluble indicator for analytic process provides convenience, makes operation easier
Water-soluble tetrabromo-mcresolsulfonphthalein (C
21H
14Br
4O
5S mol698.04) the red-purple crystallization is water-soluble, and solution is blue red; Being slightly soluble in ethanol takes on a red color; Be dissolved in alkaline solution and be blue; Be insoluble to benzene, ether, chloroform.The preparation method is suspended in m-cresol sulphonyl phthalein in the Glacial acetic acid min. 99.5, under heating state, gets with bromine reaction.The sodium salt of its tetrabromo-mcresolsulfonphthalein is the red-brown crystallization, and is soluble in water, also is water-soluble tetrabromo-mcresolsulfonphthalein .pH3.8 (Huang)-5.4 (indigo plant).Tetrabromo-mcresolsulfonphthalein and water-soluble tetrabromo-mcresolsulfonphthalein are all acid.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of water-soluble tetrabromo-mcresolsulfonphthalein.
The technical scheme that realizes the object of the invention is following:
A kind of preparation method of water-soluble tetrabromo-mcresolsulfonphthalein is characterized in that comprising the steps:
(1) 1.5 kilograms of bromines is dissolved in 1.25 liters of glacial acetic acid solution, obtains bromo-glacial acetic acid mixed solution;
(2) 2 kilograms of pure m-cresol purples are dissolved in the solution of 2.5 liters of glacial acetic acids;
(3) the bromo-glacial acetic acid mixed solution that step (1) is obtained slowly splashes in step (2) the m-cresol purple solution; Temperature is no more than 80 ℃, adds that bromine is more than half to have yellow crystal constantly to separate out, and adds continued and stirs and kept 5 hours in 80～90 ℃; The cooling after-filtration; Deposition washes twice with glacial acetic acid, dries, in 50～60 ℃ of dry bullion tetrabromo-mcresolsulfonphthaleins that get.
(4) preparation of sodium salt: 57.3 gram sodium hydroxide are dissolved in 2000 ml distilled waters; Claim that the tetrabromo-mcresolsulfonphthalein that 500 gram steps (3) are processed adds in the sodium hydroxide solution; Make its whole dissolvings, stirred filtering solution two hours in 80 ℃; Filtrating concentrates evaporate to dryness, obtains red-brown and has the water-soluble tetrabromo-mcresolsulfonphthalein of metal light crystal product.
Advantage of the present invention and beneficial effect:
The color range of indicator of the present invention's preparation is narrow, and variable color is sharp; Purity is high, and impurity is few; Method is simple to operate, is fit to industrial application.
Embodiment
Below in conjunction with specific embodiments the present invention is further specified,, can not limit protection scope of the present invention with following illustrating to help understanding content of the present invention.
Equipment: flask with three necks,round bottom, beaker, electric mantle, electronic stirring, TM, tap funnel, prolong, suction filtration device.
Reagent: m-cresol purple, glacial acetic acid, bromine, sodium hydroxide.
A kind of preparation method of water-soluble tetrabromo-mcresolsulfonphthalein, step is following:
(1) 1.5 kilograms of bromines is dissolved in 1.25 liters of glacial acetic acid solution, obtains bromo-glacial acetic acid mixed solution;
(2) 2 kilograms of pure m-cresol purples are dissolved in the solution of 2.5 liters of glacial acetic acids;
(3) the bromo-glacial acetic acid mixed solution that step (1) is obtained slowly splashes in step (2) solution, and temperature is no more than 80 ℃, and adding more than halfly has a small amount of light yellow particle constantly to separate out; Add that continued stirs and kept 24 hours in 80～90 ℃, the cooling after-filtration, deposition is washed twice with glacial acetic acid; Dry, in 50～60 ℃ of dry bullion tetrabromo-mcresolsulfonphthaleins that get, bullion is with benzene or glacial acetic acid recrystallization; Crystallize into white, fusing point 218-9 ℃;
(4) preparation of sodium salt: 57.3 gram sodium hydroxide are dissolved in 2000 ml distilled waters; Claim that the tetrabromo-mcresolsulfonphthalein that 500 gram steps (3) are processed adds in the sodium hydroxide solution; Make its whole dissolvings, stirred filtering solution two hours in 80 ℃; Filtrating concentrates evaporate to dryness, obtains red-brown and has the water-soluble tetrabromo-mcresolsulfonphthalein of metal light crystal product.
The discussion of key problem in technology and problem
(1) adds the bromine temperature and must not surpass 80 ℃, otherwise can form brown crystallization.
(2) pure article are disodium salt, and excessive or a spot of alkali input all can influence pure article and use terminal point.
(3) the indicator sodium salt is prone to the moisture absorption, should under drying conditions, deposit.
(4) aqueous solution is comparatively stable.
Claims (1)
1. the preparation method of a water-soluble tetrabromo-mcresolsulfonphthalein is characterized in that: comprise the steps:
(1) 1.5 kilograms of bromines is dissolved in 1.25 liters of glacial acetic acid solution, obtains bromo-glacial acetic acid mixed solution;
(2) 2 kilograms of pure m-cresol purples are dissolved in the solution of 2.5 liters of glacial acetic acids;
(3) the bromo-glacial acetic acid mixed solution that step (1) is obtained slowly splashes in step (2) the m-cresol purple solution, and temperature is no more than 80 ℃, adds that continued stirs and keeps 5 hours in 80～90 ℃; The cooling after-filtration; Deposition washes twice with glacial acetic acid, dries, in 50～60 ℃ of dry bullion tetrabromo-mcresolsulfonphthaleins that get.
(4) preparation of sodium salt: 57.3 gram sodium hydroxide are dissolved in 2000 ml distilled waters; Claim that the tetrabromo-mcresolsulfonphthalein that 500 gram steps (3) are processed adds in the sodium hydroxide solution; Make its whole dissolvings, stirred filtering solution two hours in 80 ℃; Filtrating concentrates evaporate to dryness, obtains red-brown and has the water-soluble tetrabromo-mcresolsulfonphthalein of metal light crystal product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110226707A CN102321065A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromcresol green |
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| CN201110226707A CN102321065A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromcresol green |
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| CN102321065A true CN102321065A (en) | 2012-01-18 |
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| CN201110226707A Pending CN102321065A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromcresol green |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727359A (en) * | 2018-07-04 | 2018-11-02 | 山东朱氏药业集团有限公司 | Two (4- pyridines) cresol-purple sultones of one kind and preparation method thereof and application method |
| CN112759574A (en) * | 2020-11-27 | 2021-05-07 | 厦门大学 | Purification method of sulfophthalein acid-base indicator |
-
2011
- 2011-08-09 CN CN201110226707A patent/CN102321065A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727359A (en) * | 2018-07-04 | 2018-11-02 | 山东朱氏药业集团有限公司 | Two (4- pyridines) cresol-purple sultones of one kind and preparation method thereof and application method |
| CN112759574A (en) * | 2020-11-27 | 2021-05-07 | 厦门大学 | Purification method of sulfophthalein acid-base indicator |
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Application publication date: 20120118 |