CN103288794A - Preparation method of bromcresol purple - Google Patents
Preparation method of bromcresol purple Download PDFInfo
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- CN103288794A CN103288794A CN 201310188951 CN201310188951A CN103288794A CN 103288794 A CN103288794 A CN 103288794A CN 201310188951 CN201310188951 CN 201310188951 CN 201310188951 A CN201310188951 A CN 201310188951A CN 103288794 A CN103288794 A CN 103288794A
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- glacial acetic
- acetic acid
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- bromcresol purple
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Abstract
The invention relates to a preparation method of bromcresol purple. The method comprises the following steps of: (1) mixing cresol red with glacial acetic acid according to the mass ratio of the cresol red to the glacial acetic acid being 5: (1 to 2) and adding the mixture into a reaction kettle; heating to the temperature of 80 to 85 DEG C in a stirring manner; dripping a bromate mixture into the reaction kettle by using a funnel under the condition that the temperature is controlled within 80 DEG C to 85 DEG C, wherein the white smoke generated by a reaction escapes from a condensation pipe and flows back; after adding the bromate mixture, heating to the temperature of 100 DEG C to 102 DEG C and maintaining for 2 hours; and (2) standing for the night; filtering light red crystals and drying the light read crystals in the air, thereby obtaining a crude bromcresol purple product; and purifying the crude bromcresol purple product with glacial acetic acid, thereby obtaining the pure bromcresol purple. The method is convenient and simple, general and easy to implement, short in preparation period and simple and easy to operate; raw materials are easy to obtain, and the yield of the bromcresol purple is high; and thus the production cost of an enterprise is lowered, and the economic benefit of the enterprise is increased.
Description
Technical field
The invention belongs to the chemical analysis reagent field, relate to acid base indicator, especially a kind of preparation method of purpurum bromocresolis.
Background technology
Acid base indicator only is accompanied by a class material of colour-change usually along with the change of pH value of solution value.Be chemical with the inadvisable few chemical substance of 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 acid or the alkali formula of proton occurred losing or obtaining.Just we study the pH indicator to the indicator of this moment.
In actual applications, wish 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, research makes new advances produces colour-change to the specific trace metal ion formation complexing of weak acid and weak base and some and becomes to attach most importance to.
Purpurum bromocresolis is called toluene bromide phenol violet (C again
21H
16O
5SBr2mol540.22) water insoluble, be slightly soluble in ethanol, be dissolved in diluted alkaline and be blue, pH value 5.2-6.8(color is by the xanthochromia purple);Mainly as acid base indicator, chromatographic analysis reagent.
Summary of the invention
The objective of the invention is to overcome existing deficiency, provide a kind of method general easy row, raw material is easy to get, the cycle lacks, the preparation method of purpurum bromocresolis easy and simple to handle, and is narrow by the preparation-obtained purpurum bromocresolis color change interval of this method, variable color is sharp.
The present invention solves its technical problem and takes following technical scheme to realize:
A kind of preparation method of purpurum bromocresolis, step is as follows:
With o-cresolsulfonphthalein and glacial acetic acid by quality than o-cresolsulfonphthalein: glacial acetic acid is that the mixed of 5:1～2 adds in the reactor, be warming up to the 80-85 degree under stirring, dripping bromine acid mixture in the still, temperature control is at the 80-85 degree, the white cigarette that reaction produces is overflowed by prolong and backflow is arranged, and is warming up to the 100-102 degree after adding and keeps 2 hours;
⑵ sinking is spent the night, and the crystallization of filtering light red is dried, and gets the purpurum bromocresolis crude product, and crude product is purified with Glacial acetic acid, namely gets purpurum bromocresolis.
And o-cresolsulfonphthalein among the described step ⑴: the mass ratio of glacial acetic acid is 5:1.5.
And the bromic acid mixture is bromine and glacial acetic acid mixture among the described step ⑴, bromine: the volume ratio of glacial acetic acid is 1.7:2.
Advantage of the present invention and beneficial effect are:
1, convenient and simple, the general easy row of preparation method of the present invention, raw material is easy to get, and preparation cycle is short, and is easy and simple to handle, and the productive rate of purpurum bromocresolis is also higher, has reduced the production cost of enterprise, has improved economic benefit of enterprises.
2, the purpurum bromocresolis color change interval for preparing of the inventive method is narrow, even pH value of solution has less variation also can make indicator produce sensitive variation, and the variable color acumen, thereby can be widely used in the actual production.
Embodiment
Be further described below in conjunction with embodiment, following examples are descriptive, are not determinate, can not limit protection scope of the present invention with this.
Employed reagent among the present invention if no special instructions, is commercially available conventional reagent; Employed method among the present invention if no special instructions, is the ordinary method of using in the art.
Instrument used in the present invention and equipment:
There-necked flask long-tail dropping funnel, electronic stirring mixed electric mantle, return line (recovery acetic acid), B and filter flask;
Raw material used in the present invention: o-cresolsulfonphthalein, bromine, glacial acetic acid.
Embodiment 1
A kind of preparation method of purpurum bromocresolis, step is as follows:
⑴ put into 5 kilograms of o-cresolsulfonphthaleins to have and stir the reactor that has added 1.5 kilograms of glacial acetic acids, stir and slowly be warming up to the 80-85 degree down, be solidliquid mixture this moment in the bottle, with funnel dripping bromine acid mixture (1.7 liters of bromine+2 liter glacial acetic acids) in the still, drip and want slow, temperature control is between the 80-85 degree, and reaction has a large amount of white cigarette prolongs to overflow and with backflow, adds back intensification 100-102 degree and keeps 2 hours;
⑵ liquid blackening stops to heat and keeps after 2 hours sinking and spend the night, and the crystallization of filtering light red is dried, and gets crude product, and crude product can further be purified with Glacial acetic acid, namely gets the pure product of purpurum bromocresolis.
After testing, obtain 4.3 kilograms of products.
Embodiment 2
A kind of preparation method of purpurum bromocresolis, step is as follows:
⑴ put into 5 kilograms of o-cresolsulfonphthaleins to have and stir the reactor that has added 1 kilogram of glacial acetic acid, stir and slowly be warming up to the 80-85 degree down, be solidliquid mixture this moment in the bottle, with funnel dripping bromine acid mixture (1.7 liters of bromine+2 liter glacial acetic acids) in the still, drip and want slow, temperature control is between the 80-85 degree, and reaction has a large amount of white cigarette prolongs to overflow and with backflow, adds back intensification 100-102 degree and keeps 2 hours;
⑵ liquid blackening stops to heat and keeps after 2 hours sinking and spend the night, and the crystallization of filtering light red is dried, and gets crude product, and elaboration can further be purified with Glacial acetic acid, namely gets the pure product of purpurum bromocresolis.
After testing, obtain 4.2 kilograms of products.
Embodiment 3
A kind of preparation method of purpurum bromocresolis, step is as follows:
⑴ put into 5 kilograms of o-cresolsulfonphthaleins to have and stir the reactor that has added 2 kilograms of glacial acetic acids, stir and slowly be warming up to the 80-85 degree down, be solidliquid mixture this moment in the bottle, with funnel dripping bromine acid mixture (1.7 liters of bromine+2 liter glacial acetic acids) in the still, drip and want slow, temperature control is between the 80-85 degree, and reaction has a large amount of white cigarette prolongs to overflow and with backflow, adds back intensification 100-102 degree and keeps 2 hours;
⑵ liquid blackening stops to heat and keeps after 2 hours sinking and spend the night, and the crystallization of filtering light red is dried, and gets crude product, and elaboration can further be purified with Glacial acetic acid, namely gets the pure product of purpurum bromocresolis.
After testing, obtain 4.4 kilograms of products.
Annotate: it is very simple, easy to operate that preparation method of the present invention is characterized in comparing other method through experiment for many years, but should note following phenomenon:
Raw band is corrosive and should have worn safety appliance, and reaction produces bromize hydrogen gas, should operation under ventilating.
Bromo-reaction is a slower process, need to carry out under the acidic conditions, otherwise yield reduces.
Strict control temperature of reaction, otherwise crystallization deepens the yield reduction.
Claims (3)
1. the preparation method of a purpurum bromocresolis, it is characterized in that: step is as follows:
With o-cresolsulfonphthalein and glacial acetic acid by quality than o-cresolsulfonphthalein: glacial acetic acid is that the mixed of 5:1～2 adds in the reactor, be warming up to the 80-85 degree under stirring, dripping bromine acid mixture in the still, temperature control is at the 80-85 degree, the white cigarette that reaction produces is overflowed by prolong and backflow is arranged, and is warming up to the 100-102 degree after adding and keeps 2 hours;
⑵ sinking is spent the night, and the crystallization of filtering light red is dried, and gets the purpurum bromocresolis crude product, and crude product is purified with Glacial acetic acid, namely gets purpurum bromocresolis.
2. the preparation method of purpurum bromocresolis according to claim 1, it is characterized in that: o-cresolsulfonphthalein among the described step ⑴: the mass ratio of glacial acetic acid is 5:1.5.
3. the preparation method of purpurum bromocresolis according to claim 1, it is characterized in that: the bromic acid mixture is bromine and glacial acetic acid mixture among the described step ⑴, bromine: the volume ratio of glacial acetic acid is 1.7:2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310188951 CN103288794A (en) | 2013-05-21 | 2013-05-21 | Preparation method of bromcresol purple |
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| CN 201310188951 CN103288794A (en) | 2013-05-21 | 2013-05-21 | Preparation method of bromcresol purple |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608619A (en) * | 2020-12-18 | 2021-04-06 | 袁新华 | Preparation method of tar violet |
-
2013
- 2013-05-21 CN CN 201310188951 patent/CN103288794A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112608619A (en) * | 2020-12-18 | 2021-04-06 | 袁新华 | Preparation method of tar violet |
| CN112608619B (en) * | 2020-12-18 | 2022-04-29 | 袁新华 | Preparation method of tar violet |
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Application publication date: 20130911 |