CN102351839A - Preparation method of water-soluble bromophenol blue - Google Patents
Preparation method of water-soluble bromophenol blue Download PDFInfo
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- CN102351839A CN102351839A CN2011102266699A CN201110226669A CN102351839A CN 102351839 A CN102351839 A CN 102351839A CN 2011102266699 A CN2011102266699 A CN 2011102266699A CN 201110226669 A CN201110226669 A CN 201110226669A CN 102351839 A CN102351839 A CN 102351839A
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- glacial acetic
- water
- bromophenol blue
- acetic acid
- soluble
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Abstract
The invention relates to a preparation method of water-soluble bromophenol blue. The preparation method comprises the following steps of 1, weighing 5kg of phenol red, and dissolving the phenol red in 40L of glacial acetic acid, 2, dissolving 2L of bromine in 5L of glacial acetic acid to obtain a bromine-glacial acetic acid mixed solution, 3, heating the phenol red solution obtained by the step 1 for dissolution, adding dropwisely the bromine-glacial acetic acid mixed solution into the phenol red solution with stirring, filtering when all of the phenol red is dissolved gradually and yellow solids are precipitated, removing free bromine by glacial acetic acid, and placing the precipitate obtained by filtration in air to carry out drying to obtain crude bromophenol blue, and 4, weighing 1kg of the crude bromophenol blue, adding 2L of distilled water into 1kg of the crude bromophenol blue, adding 620g of 10% of a sodium hydroxide solution into the crude bromophenol blue solution at a temperature of 80 to 90 DEG C for neutralization until full dissolution, then adding a small quantity of active carbon into the neutral crude bromophenol blue solution, filtering, concentrating the filtrate to thick liquid, drying the thick liquid at a temperature below 80 DEG C, and crushing to obtain water-soluble bromophenol blue. The water-soluble bromophenol blue prepared by the preparation method has the advantages of narrow indicator color range, acute color transformation, high purity, and less impurity. The preparation method of the water-soluble bromophenol blue is easy for operation and is suitable for industrial application.
Description
Technical field
The invention belongs to the chemical indicator field, be specifically related to a kind of preparation method of water-soluble tetrabromophenol sulfonphthalein.
Background technology
Acid base indicator 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 color change interval 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 tetrabromophenol sulfonphthalein also is water-soluble tetrabromo phenol sulphonyl phthalein, and molecular formula is C
19H
10O
5Br
4Na S, molecular weight: 669.96.The breen powder, water-soluble be blue.This reagent is indicator commonly used.Color change interval is pH3.0 (Huang)～4.6 (purple).
The traditional preparation process method: phenolsulfonphthalein is dissolved in glacial acetic acid, adds the solution that bromine is dissolved in glacial acetic acid under stirring, in 60 ℃ of hot water of impouring, be cooled to room temperature behind the stirring several minutes, placement is spent the night.Filter, use glacial acetic acid, benzene washing leaching cake successively, dry, get tetrabromophenol sulfonphthalein.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of water-soluble tetrabromophenol sulfonphthalein.
The technical scheme that realizes the object of the invention is following:
A kind of preparation method of water-soluble tetrabromophenol sulfonphthalein is characterized in that comprising the steps:
(1) get 5 kilograms phenol red, be dissolved in 40 liters of glacial acetic acids;
(2) 2 liters of bromines are dissolved in 5 liters of glacial acetic acids, obtain bromine bromo-glacial acetic acid mixed solution;
(3) phenol red solution that step (1) is obtained is heated to whole dissolvings; Little backflow; And under agitation drip the bromo-glacial acetic acid mixed solution that step (2) obtains gradually; When all phenol red dissolve gradually and when being yellow solid and separating out; Filter; With glacial acetic acid flush away free bromine, place air drying promptly to get the crude product tetrabromophenol sulfonphthalein;
(4) get 1 kilogram of tetrabromophenol sulfonphthalein and add 2 liters of distilled water, be neutralized to dissolving fully in 80～90 ℃ with 620 grams, 10% sodium hydroxide, the dissolving back adds small amount of activated, filters, and filtrating is concentrated into pulpous state, in oven dry below 80 ℃, pulverize water-soluble tetrabromophenol sulfonphthalein.
And the crude product tetrabromophenol sulfonphthalein that step (3) is obtained obtains pure article tetrabromophenol sulfonphthalein with the glacial acetic acid purification.
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.
A kind of preparation method of water-soluble tetrabromophenol sulfonphthalein, step is following:
Instrument: flask with three necks,round bottom, beaker, electric mantle, electronic stirring, thermometer, dropping funnel, spherical condensation tube, suction filtration device.
Reagent: phenol red, glacial acetic acid, bromine, sodium hydroxide.
(1) get 5 kilograms phenol red, be dissolved in 40 liters of glacial acetic acids;
(2) 2 liters of bromines are dissolved in 5 liters of glacial acetic acids, obtain the bromine diluent;
(3) phenol red solution that step (1) is obtained is heated to whole dissolvings; Little backflow; And under agitation drip the bromine diluent that step (2) obtains gradually; When all phenol red dissolve gradually and when being yellow solid and separating out; Filter; With glacial acetic acid flush away free bromine, place air drying promptly to get the crude product tetrabromophenol sulfonphthalein;
(4) get 1 kilogram of tetrabromophenol sulfonphthalein and add 2 liters of distilled water, be neutralized to dissolving fully in 80～90 ℃ with 620 grams, 10% sodium hydroxide, the dissolving back adds small amount of activated, filters, and filtrating is concentrated into pulpous state, 80 ℃ of oven dry, pulverize water-soluble tetrabromophenol sulfonphthalein.The crude product tetrabromophenol sulfonphthalein that step (3) is obtained obtains pure article tetrabromophenol sulfonphthalein with the glacial acetic acid purification.
Key problem in technology and problem discussion
(1) water-soluble tetrabromophenol sulfonphthalein is a sodium salt, and the sodium of unnecessary amount directly influences the use emphasis.
(2) concentrating is a very long process, and temperature is unsuitable too high.
Claims (2)
1. the preparation method of a water-soluble tetrabromophenol sulfonphthalein is characterized in that: comprise the steps:
(1) get 5 kilograms phenol red, be dissolved in 40 liters of glacial acetic acids;
(2) 2 liters of bromines are dissolved in 5 liters of glacial acetic acids, obtain bromo-glacial acetic acid mixed solution;
(3) the phenol red heating for dissolving that step (1) is obtained; Little backflow; And under agitation drip the bromo-glacial acetic acid mixed solution that step (2) obtains gradually; When all phenol red dissolve gradually and when being yellow solid and separating out; Filter; With glacial acetic acid flush away free bromine, place air drying promptly to get the crude product tetrabromophenol sulfonphthalein;
(4) get 1 kilogram of tetrabromophenol sulfonphthalein and add 2 liters of distilled water, be neutralized to dissolving fully in 80～90 ℃ with 620 grams, 10% sodium hydroxide, the dissolving back adds small amount of activated, filters, and filtrating is concentrated into pulpous state, in oven dry below 80 ℃, pulverize water-soluble tetrabromophenol sulfonphthalein.
2. the preparation method of a kind of water-soluble tetrabromophenol sulfonphthalein according to claim 1 is characterized in that the crude product tetrabromophenol sulfonphthalein that step (3) is obtained obtains pure article tetrabromophenol sulfonphthalein with the glacial acetic acid purification.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102266699A CN102351839A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromophenol blue |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102266699A CN102351839A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromophenol blue |
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| CN102351839A true CN102351839A (en) | 2012-02-15 |
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| CN2011102266699A Pending CN102351839A (en) | 2011-08-09 | 2011-08-09 | Preparation method of water-soluble bromophenol blue |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196907A (en) * | 2013-01-21 | 2013-07-10 | 江南大学 | Acid-base indicator and preparation method thereof |
| CN112759574A (en) * | 2020-11-27 | 2021-05-07 | 厦门大学 | Purification method of sulfophthalein acid-base indicator |
-
2011
- 2011-08-09 CN CN2011102266699A patent/CN102351839A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196907A (en) * | 2013-01-21 | 2013-07-10 | 江南大学 | Acid-base indicator and preparation method thereof |
| CN103196907B (en) * | 2013-01-21 | 2016-12-28 | 江南大学 | A kind of acid-base indicator and preparation method thereof |
| 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: 20120215 |