A kind of preparation method of chromium o-hydroxybenzoate containing substituent

A technology of o-hydroxybenzoic acid and substituent, applied in the field of organic compound preparation, can solve the problems of generating sticky agglomerates, low equipment efficiency and high production cost, achieve easy separation and washing, solve the problem of large equipment investment, and protect production equipment Effect

Active Publication Date: 2018-09-21
GUANGXI RES INST OF CHEM IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional process of industrially producing chromium o-hydroxybenzoate is to prepare inorganic chromium salts such as chromium sulfate and sodium o-hydroxybenzoate through metathesis reaction in aqueous solution. This kind of preparation method has the following problems: (1) The product is viscous and difficult to Solid-liquid separation, and various impurities in the product bring obstacles to purification; (2) In the subsequent processing steps, the product crystallizes multiple times, and crystallization equipment needs to be added. The equipment investment is too large, the production process is complicated, and the production cost is high; (3) Heavy metal pollution in waste liquid is not conducive to the development of enterprises and the improvement of economic benefits, and also has great hidden dangers to the natural environment polluted by heavy metals
However, the equipment efficiency of this method is low, and the subsequent purification and washing are complicated
[0005] As can be seen from the above, in the existing process for synthesizing chromium o-hydroxybenzoate, there are problems such as generation of viscous agglomerates in the reaction process, difficult separation and purification of products, and heavy metal pollution of chromium ions in the waste liquid after the reaction

Method used

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  • A kind of preparation method of chromium o-hydroxybenzoate containing substituent
  • A kind of preparation method of chromium o-hydroxybenzoate containing substituent
  • A kind of preparation method of chromium o-hydroxybenzoate containing substituent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Measure 270ml of deionized water, weigh 5mol of chromium formate and 5mol of 3-nitro-o-hydroxybenzoic acid, pour deionized water into a 500ml reaction kettle, add chromium formate into water for dispersion treatment, and add all 3 -Nitro o-hydroxybenzoic acid and start to heat up slowly, control the temperature rise rate of the entire material mixing system to 0.2°C / min until the system boils, let the system react in the boiling state for 2 hours, then take a sample and filter, observe that the filtrate is colorless, chromium When the test paper detects that the chromium ion in the filtrate is lower than 0.5ppm, stop the reaction, filter, then wash and dry the product to obtain final product.

Embodiment 2

[0032] Measure 270ml of deionized water, weigh 5mol of chromium sulfate and 7mol of 5-methyl o-hydroxybenzoic acid, pour deionized water into a 500ml reaction kettle, add chromium sulfate into water for dispersion treatment, and add all 5 -Methyl o-hydroxybenzoic acid and start to heat up slowly, control the heating rate of the entire material mixing system to 0.25°C / min until the system boils, make the system react in a boiling state for 2.5h, then sample and filter, observe that the filtrate is colorless, When the chromium test paper detects that the chromium ion in the filtrate is lower than 0.5ppm, the reaction is stopped, filtered, and then the product is washed and dried to obtain final product.

Embodiment 3

[0034] Prepare 270ml of mixed solvent of water and ethanol, wherein the mass fraction of water is 80%, and the mass fraction of ethanol is 20%; weigh 3 mol of chromium acetate, 2 mol of chromium chloride and 10 mol of 3-ethyl-5-methoxy-o-hydroxybenzene Formic acid: Pour the mixed solvent into a 500ml reaction kettle, then add chromium acetate and chromium chloride to the mixed solvent for dispersion treatment, add all 3-ethyl-5-methoxy o-hydroxybenzoic acid while stirring and start Slowly heat up, control the temperature rise rate of the entire material mixing system to 0.3°C / min until the system boils, let the system react in a boiling state for 3 hours, then take a sample and filter, observe that the filtrate is colorless, and the chromium ion in the filtrate is lower than 0.5ppm by chromium test paper , stop the reaction, filter, then wash and dry the product to obtain the product.

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Abstract

The invention provides a preparation method of substituent-containing chromium o-hydroxybenzoate. The substituent-containing chromium o-hydroxybenzoate is prepared from a chromium salt and substituent-containing o-hydroxybenzoic acid. The preparation method comprises adding a chromium salt into a water-solvent mixed system, carrying out dispersion treatment, adding substituent-containing o-hydroxybenzoic acid into the solution in batch or carrying out slow heating until the system is boiling, carrying out a reaction process in a boiling state for 2h or more, then washing the product and then drying the product. Through effective measures in the reaction process, binder production in the reaction process is reduced and the finished product has a high yield, high purity and no viscidity and is easy to separate and wash. The reaction waste liquid has low chromium ion content and can be directly discharged so that heavy metal pollution hidden danger is avoided, environmental friendliness is improved and a wide promotion prospect is realized.

Description

technical field [0001] The invention belongs to the field of organic compound preparation, and in particular relates to a preparation method of chromium o-hydroxybenzoate containing substituents. Background technique [0002] Chromium o-hydroxybenzoate complex is an organic chromium mineral additive, which can be used as medicine and health care products or feed additives, electroplating and leather tanning aids, chromium-imparting agents for complexation reactions, and metal anti-corrosion agents, etc. It has broad application prospects , so it is getting more and more attention. [0003] The traditional process of industrially producing chromium o-hydroxybenzoate is to prepare inorganic chromium salts such as chromium sulfate and sodium o-hydroxybenzoate through metathesis reaction in aqueous solution. This kind of preparation method has the following problems: (1) The product is viscous and difficult to Solid-liquid separation, and various impurities in the product bring...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F11/00
CPCC07F11/005
Inventor 余慧群莫友彬周海廖艳芳彭初和
Owner GUANGXI RES INST OF CHEM IND CO LTD
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