CN102911155A - Method for preparing water-soluble bromochlorophenol blue - Google Patents
Method for preparing water-soluble bromochlorophenol blue Download PDFInfo
- Publication number
- CN102911155A CN102911155A CN 201210451698 CN201210451698A CN102911155A CN 102911155 A CN102911155 A CN 102911155A CN 201210451698 CN201210451698 CN 201210451698 CN 201210451698 A CN201210451698 A CN 201210451698A CN 102911155 A CN102911155 A CN 102911155A
- Authority
- CN
- China
- Prior art keywords
- solution
- soluble
- bromochlorophenol
- red
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing water-soluble bromochlorophenol blue. The method includes the following steps of (1) synthetizing bromochlorophenol red, dissolving chlorphenol red in a glacial acetic acid of 20L, slowly adding a glacial acetic acid solution with bromine dissolved in under stirring, then increasing the temperature to 65 DEG C to 75 DEG C, performing thermal insulation for 4 to 7 hours, cooling, filtering, washing for 2 to 5 times, and crystallizing until the color is faded; and (2) dissolving a filter cake in a sodium hydroxide solution, adding activated carbon to decolor and filter, subjecting the solution to reduced pressure distillation until the volume of the solution is 1/3 of the original volume, pouring the solution in ethanol, precipitating crystals, filtering out the crystals, and drying the crystals at the temperature of 60 DEG C to 80 DEG C to obtain a finished product. According to the method for preparing the water-soluble bromochlorophenol blue, o-benzenesulfonic anhydride is condensed with chlorophenol under the catalysis of zinc chloride anhydrous to obtain the chlorphenol red, the chlorphenol red is directly bromized to obtain the bromochlorophenol red, the bromochlorophenol red is reacted with alkali to obtain the bromochlorophenol blue sodium salt, and prior methods which are long in cycle, highly toxic in raw materials, and low in yield are abandoned.
Description
Technical field
The invention belongs to pH indicator preparation field, particularly a kind of preparation method of water-soluble bromchlorphenol blue.
Background technology
Acid base indicator normally is accompanied by a class material of colour-change along with the change of pH, be that chemistry and chemical analysis field must inadvisable few chemical articles, 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 each other a kind of equilibrium state.The pH value just can affect 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, and namely 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, what research made new advances forms complexing and produces the emphasis that colour-change becomes present the sector research weak acid and weak base and some specific trace metal ion.
Bromchlorphenol blue sodium salt brown ceramic powder (C
19H
9Br
2CL
2NaO
5S mol 603.04) soluble in water, be slightly soluble in ethanol, acetic acid is not dissolved in ether, chloroform, and solution takes on a red color in alcohol, alkali; PH value 3.2(is yellow)-4.8(is purple), acid base indicator made.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, water-soluble bromchlorphenol blue that a kind of method is more simple, productive rate is higher and preparation method thereof is provided.
The present invention realizes that the technical scheme of purpose is as follows:
A kind of preparation method of water-soluble bromchlorphenol blue, step is as follows
⑴ the synthetic of bromine dichlorophenol sulfonphthalein is dissolved in dichlorophenol sulfonphthalein in the 20L Glacial acetic acid, under agitation slowly adds the glacial acetic acid solution that has dissolved in bromine, adds rear intensification 65-75 ℃ and be incubated 4-7 hour, cooled and filtered, and washing 2-5 time, and the crystallization color shoals;
⑵ be dissolved in filter cake in the sodium hydroxide solution, adds activated carbon decolorizing and filter, and solution, is poured in the ethanol during to original volume 1/3 through underpressure distillation, and crystallization leaches crystallization, in 60-80 ℃ of drying, gets finished product.
And described raw material weight is than being dichlorophenol sulfonphthalein: bromine: sodium hydroxide=1:0.8:0.1.
And the massfraction of described sodium hydroxide solution is 10%.
Advantage of the present invention and beneficial effect are:
1, bromchlorphenol blue sodium salt of the present invention synthetic be by adjacent Phenylsulfonic acid acid anhydride under Zinc Chloride Anhydrous catalysis with the chlorophenol condensation, the dichlorophenol sulfonphthalein of making, the direct bromination of dichlorophenol sulfonphthalein can obtain bromine dichlorophenol sulfonphthalein, obtain sodium salt with alkali reaction again, abandoned by contrast the route that the cycle is long, raw material is hypertoxic, yield is low.
The more common easy row of the preparation method of the water-soluble bromchlorphenol blue that 2, the present invention relates to, raw material easy, the cycle is short, easy and simple to handle, the product yield of preparation is high, in preparation process first the system finished product, then finished product has been carried out again the purification steps such as further washing, the finished product purity of acquisition is higher.
Embodiment
Below in conjunction with embodiment, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The per-cent of following examples volume all is weight percentage, have special indicate except.
Instrument and equipment: three bottles, thermometer, electric stirring, prolong, electric mantle, filtration unit.
A kind of preparation method of water-soluble bromchlorphenol blue, step is as follows
⑴ the synthetic of bromine dichlorophenol sulfonphthalein is dissolved in 5kg dichlorophenol sulfonphthalein in the 20L Glacial acetic acid, under agitation slowly adds the glacial acetic acid solution that 5L has dissolved in the 4kg bromine, adds rear intensification 65-75 ℃ and be incubated 6 hours, the control temperature is unsuitable too high, cooled and filtered, and washing is repeatedly, the crystallization color shoals;
⑵ be dissolved in filter cake in 5kg 10% sodium hydroxide solution, adds a small amount of activated carbon decolorizing and filter, and solution, is poured in the ethanol during to original volume 1/3 through underpressure distillation, and crystallization leaches crystallization, in 60-80 ℃ of drying, gets finished product.
The weight ratio that feeds intake dichlorophenol sulfonphthalein: bromine: sodium hydroxide=1:0.8:0.1.
Operate very easy, will be in the past bromine dichlorophenol sulfonphthalein and sodium salt stepwise synthesis be reduced to a step and carry out, but the resistates of bromine must Ex-all, so filter through repeatedly washing.
Claims (3)
1. the preparation method of a water-soluble bromchlorphenol blue, step is as follows
⑴ the synthetic of bromine dichlorophenol sulfonphthalein is dissolved in dichlorophenol sulfonphthalein in the 20L Glacial acetic acid, under agitation slowly adds the glacial acetic acid solution that has dissolved in bromine, adds rear intensification 65-75 ℃ and be incubated 4-7 hour, cooled and filtered, and washing 2-5 time, and the crystallization color shoals;
⑵ be dissolved in filter cake in the sodium hydroxide solution, adds activated carbon decolorizing and filter, and solution, is poured in the ethanol during to original volume 1/3 through underpressure distillation, and crystallization leaches crystallization, in 60-80 ℃ of drying, gets finished product.
2. the preparation method of water-soluble bromchlorphenol blue according to claim 1 is characterized in that: described raw material weight is than being dichlorophenol sulfonphthalein: bromine: sodium hydroxide=1:0.8:0.1.
3. the preparation method of water-soluble bromchlorphenol blue according to claim 1, it is characterized in that: the massfraction of described sodium hydroxide solution is 10%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210451698 CN102911155A (en) | 2012-11-12 | 2012-11-12 | Method for preparing water-soluble bromochlorophenol blue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210451698 CN102911155A (en) | 2012-11-12 | 2012-11-12 | Method for preparing water-soluble bromochlorophenol blue |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102911155A true CN102911155A (en) | 2013-02-06 |
Family
ID=47609761
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201210451698 Pending CN102911155A (en) | 2012-11-12 | 2012-11-12 | Method for preparing water-soluble bromochlorophenol blue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102911155A (en) |
-
2012
- 2012-11-12 CN CN 201210451698 patent/CN102911155A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112679420B (en) | Preparation method of 2,5-dibromopyridine | |
| CN103435632B (en) | A kind of preparation method of cefuroxime axetil | |
| CN106349245A (en) | Sitagliptin phosphate impurities, method for preparing same and application of sitagliptin phosphate impurities | |
| CN101817989A (en) | Method for preparing disperse blue 60 and homologues thereof | |
| CN106008290A (en) | Method for preparing tembotrions | |
| WO2022166442A1 (en) | Preparation method for 2-acetyl-1,10-phenanthroline | |
| CN102295536B (en) | Preparation method of high-content trimethylhydroquinone | |
| CN105461622A (en) | Method for preparing 4-amino-3,6-dichloropicolinic acid by reducing 4-amino-3,5,6-trichloropicolinic acid | |
| CN101270124B (en) | Novel method for purifying and preparing high-purity fluorandiol and fluorandiol salt | |
| CN106892803B (en) | Preparation method of 2, 6-dichloro-3-fluorobenzaldehyde and preparation method of fluoroquinolone compound | |
| CN102911155A (en) | Method for preparing water-soluble bromochlorophenol blue | |
| CN101955415B (en) | Method for preparing 2-hydroxyl biphenyl compound | |
| CN102911154A (en) | Preparation method of water-soluble bromocresol purple | |
| CN103804187B (en) | Synthesis method of diethylstilbestrol compound pigeon pea ketonic acid A | |
| CN103360394B (en) | 8-chlorotheophylline preparation method | |
| CN105418507A (en) | Preparation method for 1-(3-methyl-1-phenyl-1H-pyrazole-5-yl)piperazine | |
| CN102267976A (en) | Preparation method for m-cresol purple | |
| CN103360323A (en) | Preparation method of triclabendazole | |
| CN103508883B (en) | Method for synthesizing roflumilast intermediate | |
| CN102924369A (en) | Method for synthesizing 3,5-dibromo-4-iodopyridine by one step | |
| CN103396388A (en) | Preparation method of tetrabromophenolphthalein indicator | |
| CN102276578A (en) | Method for preparing phenol red complexing agent | |
| CN102924468A (en) | Preparing method of fluorescein complexing agents | |
| CN102936614A (en) | Synthesis method of 7-alpha-methoxy-3-deacetylcephalothin benzathine | |
| CN103058896A (en) | Preparation method of water-soluble sodium alizarin sulfonate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20130206 |