CN102411002A - Preparation method of bromophenol blue indicator - Google Patents
Preparation method of bromophenol blue indicator Download PDFInfo
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- CN102411002A CN102411002A CN2011102267066A CN201110226706A CN102411002A CN 102411002 A CN102411002 A CN 102411002A CN 2011102267066 A CN2011102267066 A CN 2011102267066A CN 201110226706 A CN201110226706 A CN 201110226706A CN 102411002 A CN102411002 A CN 102411002A
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- glacial acetic
- acetic acid
- bromophenol blue
- bromine
- preparation
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Abstract
The invention relates to a preparation method of bromophenol blue, which comprises the following steps: dissolving 1kg of phenol red in 3L of glacial acetic acid; dissolving 0.64L of bromine in 0.8L of the glacial acetic acid to get bromine diluent; heating phenol red solution to 60 DEG C under a stirring condition, slowly dropwise adding the bromine diluent, continuously heating up to 100-105 DEG C after the bromine diluent is added completely, maintaining the reaction for 2 hours and filtering at the temperature of 80-100 DEG C so as to get a sandy pink bromophenol blue crude product; and drying, then further purifying with the glacial acetic acid so as to get a pure bromophenol blue product. The indicator prepared by the preparation method is narrow in color change interval and sensitive in color change; the purity is high and impurities are few; and the method is simple to operate and suitable for industrial applications.
Description
Technical field
The invention belongs to the chemical indicator field, be specifically related to a kind of preparation method of bromophenol blue indicator.
Background technology
Acid base indicator typically refers to the one type of material that is accompanied by change color 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 " dynamic isomer " structural change.
This dynamic isomer has the character of Conjugate Acid-Base Pairs, 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 change color weak acid and weak base and some specific trace metal ion, becomes the emphasis of our research.
Bromophenol blue also is tetrabromo phenol sulphonyl phthalein (C
19H
10O
5Br
4S, mol 669.96).Be close to colourless or the tiny crystallization of misty rose, be slightly soluble in water and make the WS be yellow, be soluble in ether and ethanol, can be dissolved in diluted alkaline and the ammonia solution and au bleu is brown after putting for a long time.This reagent is indicator commonly used.Color change interval is pH3.0～4.6; Also can be used as the reagent of measuring mercury ion.
The traditional preparation process method: phenol red is dissolved in glacial acetic acid, stirs and to add the solution that bromine is dissolved in glacial acetic acid down, stir after a few minutes in 60 ℃ of hot water of impouring, be cooled to room temperature, placement is spent the night.Filter, use glacial acetic acid, benzene washing leaching cake successively, dry, get bromophenol blue.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of bromophenol blue indicator.
The technical scheme that realizes the object of the invention is following:
A kind of preparation method of bromophenol blue indicator is characterized in that: comprise the steps:
(1) get 1 kilogram phenol red, be dissolved in 3 liters of glacial acetic acids;
Said phenol red and w/v glacial acetic acid are: 0.3-1: 1-3;
(2) 0.64 liter of bromine is dissolved in 0.8 liter of glacial acetic acid, obtains bromo-glacial acetic acid mixed liquor;
The volume ratio of said bromine and glacial acetic acid is: 1-4: 5-4;
(3) phenol red solution that step (1) is obtained with stir under be heated to 60 ℃; Slowly drip the bromo-glacial acetic acid mixed liquor that step (2) obtains, add continued and heat up 100～105 ℃, keep reaction two hours; In 80～100 ℃ of filtrations, go out sand-like pink bullion bromophenol blue.
And the bullion bromophenol blue of said step (3) is further purified with glacial acetic acid after drying, gets pure article bromophenol blue.
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 commercial 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.
Instrument: flask with three necks,round bottom, beaker, electric jacket, electronic stirring, thermometer, tap funnel, spherical condensation tube, suction filtration device.
Reagent: phenol red, glacial acetic acid, bromine.
Embodiment 1:
A kind of preparation method of bromophenol blue indicator, step is following:
(1) get 1 kilogram phenol red, be dissolved in 3 liters of glacial acetic acids;
(2) 0.64 liter of bromine is dissolved in 0.8 liter of glacial acetic acid, obtains bromo-glacial acetic acid mixed liquor;
(3) phenol red solution that step (1) is obtained with stir under be heated to 60 ℃; Slowly drip the bromo-glacial acetic acid mixed liquor that step (2) obtains, add continued and heat up 100～105 ℃, keep reaction two hours; In 80～100 ℃ of filtrations, go out sand-like pink bullion bromophenol blue.
The bullion bromophenol blue is further purified with glacial acetic acid after drying, gets pure article bromophenol blue 1.3～1.4kg.
Embodiment 2:
A kind of preparation method of bromophenol blue indicator, step is following:
(1) get 300 the gram phenol red, be dissolved in 1000 milliliters of glacial acetic acids;
(2) 200 milliliters of bromines are dissolved in 500 milliliters of glacial acetic acids, obtain bromo-glacial acetic acid mixed liquor;
(3) the bromo-glacial acetic acid mixed liquor that step (2) is obtained under agitation adds in the phenol red solution that step (1) obtains, and after the stirred for several minute, moves in 60 ℃ the hot water; Be cooled to room temperature, placement is spent the night, and filters; Earlier with 200 milliliters of glacial acetic acid washings; Use 400 milliliters of benzene washing precipitations again, airing in air gets bullion bromophenol blue 400g.
Dried bullion bromophenol blue obtains pure article bromophenol blue with acetone-glacial acetic acid recrystallization.
Points for attention are the discussion of problem both
(1) adding bromine liquid should slowly carry out, owing to emit a small amount of bromize hydrogen gas, reaction should be carried out under ventilation condition.
(2) elaboration is answered the remaining bromide of Ex-all, otherwise terminal point is used in influence.
Claims (2)
1. the preparation method of a bromophenol blue indicator is characterized in that: comprise the steps:
(1) get 1 kilogram phenol red, be dissolved in 3 liters of glacial acetic acids;
Said phenol red and w/v glacial acetic acid are: 0.3-1: 1-3;
(2) 0.64 liter of bromine is dissolved in 0.8 liter of glacial acetic acid, obtains bromo-glacial acetic acid mixed liquor;
The volume ratio of said bromine and glacial acetic acid is: 1-4: 5-4;
(3) phenol red solution that step (1) is obtained with stir under be heated to 60 ℃; Slowly drip the bromo-glacial acetic acid mixed liquor that step (2) obtains, add continued and heat up 100～105 ℃, keep reaction two hours; In 80～100 ℃ of filtrations, go out sand-like pink bullion bromophenol blue.
2. the preparation method of a kind of bromophenol blue indicator according to claim 1 is characterized in that: the bullion bromophenol blue of said step (3) is further purified with glacial acetic acid after drying, gets pure article bromophenol blue.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102267066A CN102411002A (en) | 2011-08-09 | 2011-08-09 | Preparation method of bromophenol blue indicator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102267066A CN102411002A (en) | 2011-08-09 | 2011-08-09 | Preparation method of bromophenol blue indicator |
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| CN102411002A true CN102411002A (en) | 2012-04-11 |
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| CN2011102267066A Pending CN102411002A (en) | 2011-08-09 | 2011-08-09 | Preparation method of bromophenol blue indicator |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278498A (en) * | 2013-05-17 | 2013-09-04 | 无锡中德伯尔生物技术有限公司 | Detecting method and kit of sibutramine hydrochloride |
| CN103411969A (en) * | 2013-08-22 | 2013-11-27 | 上海市闵行第二中学 | Preparation method of pH indicator |
| CN105928943A (en) * | 2016-05-20 | 2016-09-07 | 浙江同兴技术股份有限公司 | Preparation method of photo-sensitive material for detecting sulfur dioxide concentration |
-
2011
- 2011-08-09 CN CN2011102267066A patent/CN102411002A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103278498A (en) * | 2013-05-17 | 2013-09-04 | 无锡中德伯尔生物技术有限公司 | Detecting method and kit of sibutramine hydrochloride |
| CN103411969A (en) * | 2013-08-22 | 2013-11-27 | 上海市闵行第二中学 | Preparation method of pH indicator |
| CN105928943A (en) * | 2016-05-20 | 2016-09-07 | 浙江同兴技术股份有限公司 | Preparation method of photo-sensitive material for detecting sulfur dioxide concentration |
| CN105928943B (en) * | 2016-05-20 | 2019-03-15 | 浙江同兴技术股份有限公司 | It is a kind of for detecting the preparation method of the optical sensitive material of sulfur dioxide concentration |
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Application publication date: 20120411 |