CN103387505A - Preparation method of nitrilotriacetic acid - Google Patents
Preparation method of nitrilotriacetic acid Download PDFInfo
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- CN103387505A CN103387505A CN2013102797362A CN201310279736A CN103387505A CN 103387505 A CN103387505 A CN 103387505A CN 2013102797362 A CN2013102797362 A CN 2013102797362A CN 201310279736 A CN201310279736 A CN 201310279736A CN 103387505 A CN103387505 A CN 103387505A
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Abstract
The invention relates to a preparation method of nitrilotriacetic acid. The preparation method comprises the following steps: (1) dissolving chloroacetic acid in water, adding anhydrous sodium carbonate with stirring to neutralize the pH value to 6-7; (2) adding ammonium chloride, heating and raising temperature to 60-70 DEG C, then adding a sodium hydroxide solution with stirring, keeping warm at 90-95 DEG C for 4 h with a pH value of 9; (3) neutralizing the pH value to 6-7 with dilute hydrochloric acid, adding water accounting for 1-3 times by volume to dilute, adding active carbon for decolouring, and filtering; and (4) neutralizing the pH value of the filtrate to 1-2 with dilute hydrochloric acid to precipitate a white precipitate which is nitrilotriacetic acid, performing filtering, water washing, centrifuge dewatering, and drying at 80-90 DEG C to obtain nitrilotriacetic acid. The nitrilotriacetic acid prepared by the preparation method is insoluble in water, soluble in dilute alkali solution and shows blue, and is mainly applied to complexing agents and organic synthesis. By selecting a synthetic method of a water-soluble sodium salt, the preparation method is universal and practicable, easily available in raw materials, short in period and simple to operate.
Description
Technical field
The invention belongs to the chemical reagent field, relate to a kind of indicator, especially a kind of preparation method of nitrilotriacetic acid.
Background technology:
Acid base indicator is often referred to a class material that is accompanied by colour-change along with the change of pH, is the indispensable chemical substance of chemistry and analysis field, and this tell-tale variation is actual is 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 while changing, and 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.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of nitrilotriacetic acid is provided, this indicator can form complexing and produce colour-change weak acid and weak base and some specific trace metal ion.
The present invention solves its technical problem and takes following technical scheme to realize:
A kind of preparation method of nitrilotriacetic acid, step is as follows:
⑴ soluble in water with Mono Chloro Acetic Acid, adds anhydrous sodium carbonate under stirring, and being neutralized to the pH value is 6～7, controls temperature of reaction below 10 ℃;
⑵ add ammonium chloride, is heated to 60-70 ℃, and then add sodium hydroxide solution under stirring, and makes temperature rise to 80-100 ℃, and 90-95 ℃ of insulation 4 hours, pH was 9;
⑶ be neutralized to the pH value with dilute hydrochloric acid is 6-7, adds 1-3 times of volume water dilution, adds activated carbon decolorizing and filters;
⑷ be neutralized to pH1-2 with dilute hydrochloric acid in filtrate, separating out white precipitate is nitrilotriacetic acid, and washing,, in centrifuge dehydration and in 80-90 ℃ of oven dry, obtain nitrilotriacetic acid after filtration;
Described Mono Chloro Acetic Acid: anhydrous sodium carbonate: the mass ratio of ammonium chloride is 5.25:2.92:1.
And the massfraction of described sodium hydroxide solution is 40%.
Advantage of the present invention and beneficial effect are:
It is water insoluble that the nitrilotriacetic acid of the present invention's preparation is called again nitrilotriacetic acid (C6H9NO6), is dissolved in diluted alkaline and is blue, is mainly used in complexometric reagent and organic synthesis.The present invention selects the synthetic method of water-soluble sodium salt, and more common easy row, raw material are easy to get, the cycle is short, easy and simple to handle.
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.
All per-cents are mass percent.
A kind of preparation method of nitrilotriacetic acid, step is as follows:
⑴ be dissolved in the 31.5kg Mono Chloro Acetic Acid in 80L water, more slowly add the 17.5kg anhydrous sodium carbonate under stirring, and being neutralized to the pH value is 6～7, controls temperature of reaction below 10 ℃,
⑵ add 6kg ammonium chloride, is heated to 60-70 ℃, and then add 40% sodium hydroxide solution 35kg under stirring, and makes temperature rise to 90 ℃, and 90-95 ℃ of insulation 4 hours, pH was 9,
⑶ be neutralized to the pH value with dilute hydrochloric acid is 6-7, and the volume water that doubles dilution adds the heat decoloring filtration slightly of 100g gac;
⑷ continue in filtrate to be neutralized to pH1-2 with dilute hydrochloric acid, should separate out white precipitate this moment is nitrilotriacetic acid, and washing,, in centrifuge dehydration and in 80-90 ℃ of oven dry, obtain finished product 16kg after filtration.Output is 75.5% of theoretical yield.
Described Mono Chloro Acetic Acid: anhydrous sodium carbonate: the mass ratio of ammonium chloride is 5.25:2.92:1.
Claims (2)
1. the preparation method of a nitrilotriacetic acid, it is characterized in that: step is as follows:
⑴ soluble in water with Mono Chloro Acetic Acid, adds anhydrous sodium carbonate under stirring, and being neutralized to the pH value is 6～7, controls temperature of reaction below 10 ℃;
⑵ add ammonium chloride, is heated to 60-70 ℃, and then add sodium hydroxide solution under stirring, and makes temperature rise to 80-100 ℃, and 90-95 ℃ of insulation 4 hours, pH was 9;
⑶ be neutralized to the pH value with dilute hydrochloric acid is 6-7, adds 1-3 times of volume water dilution, adds activated carbon decolorizing and filters;
⑷ be neutralized to pH1-2 with dilute hydrochloric acid in filtrate, separating out white precipitate is nitrilotriacetic acid, and washing,, in centrifuge dehydration and in 80-90 ℃ of oven dry, obtain nitrilotriacetic acid after filtration;
Described Mono Chloro Acetic Acid: anhydrous sodium carbonate: the mass ratio of ammonium chloride is 5.25:2.92:1.
2. the preparation method of nitrilotriacetic acid according to claim 1, it is characterized in that: the massfraction of described sodium hydroxide solution is 40%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2013102797362A CN103387505A (en) | 2013-07-05 | 2013-07-05 | Preparation method of nitrilotriacetic acid |
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| CN2013102797362A CN103387505A (en) | 2013-07-05 | 2013-07-05 | Preparation method of nitrilotriacetic acid |
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| CN2013102797362A Pending CN103387505A (en) | 2013-07-05 | 2013-07-05 | Preparation method of nitrilotriacetic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909047A (en) * | 2020-08-20 | 2020-11-10 | 苏州亚科科技股份有限公司 | Preparation process of N- (2-acetamido) -2-iminodiacetic acid |
-
2013
- 2013-07-05 CN CN2013102797362A patent/CN103387505A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909047A (en) * | 2020-08-20 | 2020-11-10 | 苏州亚科科技股份有限公司 | Preparation process of N- (2-acetamido) -2-iminodiacetic acid |
| CN111909047B (en) * | 2020-08-20 | 2023-01-31 | 苏州亚科科技股份有限公司 | Preparation process of 2- [ (2-amino-2-oxyethyl) - (carboxymethyl) amino ] acetic acid |
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Application publication date: 20131113 |