Technology for preparing semi-xylenol orange by one-step method

A technology for semi-xylenol orange and preparation process, which is applied in the field of one-step preparation of semi-xylenol orange, can solve the problems of complex process, cumbersome steps and high cost, and achieves the effects of simple process, improved conversion rate and low cost

Inactive Publication Date: 2009-04-01
TIANJIN CHEM REAGENT RES INST
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  • Description
  • Claims
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Problems solved by technology

The whole process is relatively complicated, the steps

Method used

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Embodiment Construction

[0015] The technical content of the present invention will be further described below in conjunction with the embodiments. The following examples are illustrative, not restrictive, and the protection scope of the present invention cannot be limited by the following examples.

[0016] (1). Put 1 kg of cresol red, 0.46 kg of iminodiacetic acid disodium salt and 2L of glacial acetic acid into a 5L three-necked flask, stir well, heat at 60-65°C until all of them dissolve, and cool to 30°C to form a cooling mixture;

[0017] (2). Add 0.3L, 37% formaldehyde solution to the cooling mixture, let it stand for 8 hours, and then stir continuously at 60-65°C for 8 hours;

[0018] (3). Remove the excess solvent (hydrous acetic acid) by reducing pressure, and pour the remaining black thick substance into an evaporation tank to evaporate to dryness at a temperature of 70-80°C to form crystals;

[0019] (4). Crush the crystals to obtain 2.5 kg of orange-red solid—semi-xylenol orange finishe...

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Abstract

The invention relates to a method for preparing semixylenol orange by one-step operation, including the following steps: (1) cresol red, iminodiacetic acid disodium salt and glacial acetic acid are mixed and stirred evenly, the mixture is heated till full dissolving at the temperature of 60 to 65 DEG C and then is cooled to 25 to 30 DEG C to obtain a cooled mixed liquid; (2) 37 percent of formaldehyde solution is added into the cooled mixture which is rested for 7 to 8 hours and then is constantly stirred for 7 to 8 hours at the temperature of 60 to 65 DEG C; (3) the unwanted solution is removed by decompression and the remaining black thick matter is poured into an evaporation tank to be steamed to be dry at the steaming temperature of 70 to 80 DEG C to form crystals; and (4) the crystals are crushed to obtain the orange-red solid-semixylenol orange finished products. The one-step synthesizing method adopted by the invention greatly enhances the conversion rate; the yield is higher; the sensitivity reaches the standard of similar products; the method is suitable for the large-scale industrial production.

Description

technical field [0001] The invention belongs to the field of chemical reagents, and relates to a process for preparing semi-xylenol orange in one step. Background technique [0002] Semi-xylenol orange is a complex indicator for titrating iron, aluminum, and lead. It can complex with various metal ions. Its sodium salt is in the form of red powder. It is used for colorimetric determination of bismuth, zirconium, hafnium, and thorium. It is usually produced by using cresyl red, iminodiacetic acid, formaldehyde, etc. as raw materials. Semi-xylenol orange is generated in steps due to the reaction, and the generated product is a mixed form of xylenol orange and semi-xylenol orange, so it needs to be purified and separated by different methods. The commonly used method is to first make the semi-xylenol orange crude product with the above-mentioned raw materials, and then react the obtained crude product with sodium acetate to generate the semi-xylenol orange disodium salt, and t...

Claims

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Application Information

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IPC IPC(8): C07D327/04
Inventor 石开丁
Owner TIANJIN CHEM REAGENT RES INST
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