Method for catalytically synthesizing bromamine acid condensation product by using heterogeneous system

A technology of condensation product, bromo-acid, applied in the direction of organic chemistry, sulfonate preparation, etc., can solve problems such as influence, difficult separation of condensation product and by-product copper bromide, etc., and achieve the effect of high yield and purity

Inactive Publication Date: 2017-12-12
TIANJIN CHENGJIAN UNIV
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Problems solved by technology

However, this method has certain limitations. During the reaction process, copper powder catalyzes the by-product copper bromide, which has high solubility in both ethanol and water, making it difficult to separate the condensation product and the by-product copper bromide in the reaction system. , which in turn affects the purity of the condensation product and the quality of the C.I. Pigment Red 177 prepared by the desulfonation process

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  • Method for catalytically synthesizing bromamine acid condensation product by using heterogeneous system

Examples

Experimental program
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Effect test

Embodiment 1

[0030] At room temperature, according to the solid-to-liquid ratio (w / v) of 1:4, the strongly acidic ion exchange resin was stirred and soaked for 5 hours with 0.5mol / L NaOH solution and 0.5mol / L HCl solution in turn, and then suction filtered. The filter cake was washed with water until it was neutral, and then air-dried at 75°C to obtain a pretreated strong acidic ion exchange resin, ready for use;

[0031] At room temperature, according to the solid-to-liquid ratio (w / v) of 1:3, use 0.5mol / L HCl solution to stir and soak the copper powder for 4 hours, then filter with suction, wash the filter cake with water until neutral, and dry it in vacuum at 50°C , cross 200 mesh sieves to obtain pretreated copper powder, stand-by;

[0032] Weigh 1mol of bromine and add it to a reaction flask equipped with a thermometer, a stirrer and a reflux condenser, then add 50mL of mixed solvent (methanol:water=10:1, V / V) to soak for 30min, and then pour Continue to add 60mL of mixed solvent, an...

Embodiment 2

[0034] The mixed solvent in Example 1 was replaced with ethanol:water=10:1 (V / V), the reaction temperature was increased to 75° C., and other reaction conditions remained unchanged. The yield of the condensation product calculated by weighing was 96.24%, and its purity was found to be 95.50% by high performance liquid chromatography (HPLC).

Embodiment 3

[0036] Adopt 50mL mixed solvent (methanol:water=9:1, V / V) to carry out immersion treatment to bromic acid raw material as embodiment example 1, other reaction conditions remain unchanged. The yield of the condensation product calculated by weighing was 96.19%, and its purity was found to be 97.62% by high performance liquid chromatography (HPLC).

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Abstract

The invention discloses a novel method for catalytically synthesizing a bromamine acid condensation product by using a heterogeneous system. A strong-acidic ion exchange resin-mixed solvent-copper powder catalytic system is used for substituting a traditional thick sulfuric acid-water-copper powder catalytic system to perform the bromamine condensation reaction, and by utilizing the difference of solubility of the reaction raw material bromamine acid and the reaction condensation product in a mixed solvent in the reaction, and by selecting an organic solvent type in the mixed solvent, adjusting a volume ratio of the organic solvent and water and controlling the total consumption of the mixed solvent, a condensation product is separated from the reaction solution into a solid mixture of the heterogeneous system, so that the separation of the condensation product from a byproduct copper bromide can be realized, and a condensation product with higher purity and yield can be prepared. Under the condition that the consumption of the bromamine acid raw material is 1mol, by controlling the volume ratio of the organic solvent (methanol or ethanol) in the mixed solvent to the water to be (10 to 1) to (9 to 2) and the consumption of the mixed solvent to be 110 to 200 mL, the yield of the prepared condensation product can reach 95 percent above, and the spectral (HPLC) purity is 95.50 percent to 98.88 percent.

Description

technical field [0001] The invention belongs to the synthesis method of catalytic dyeing pigment intermediates in the field of fine chemical industry, and particularly relates to a method for catalytically synthesizing a bromic acid condensation product by using a strong acid ion exchange resin-copper powder-mixed solvent system instead of the traditional concentrated sulfuric acid-copper powder-water system Methods. Background technique [0002] With the rapid development of the chemical industry, fine chemicals are playing an increasingly important role in the development of my country's national economy. However, with the rapid development of fine chemical industry, the problem of environmental pollution is becoming more and more serious. 4,4'-diamino-1,1'-dianthraquinone-3,3'-sodium disulfonate is an important intermediate for the preparation of high-grade organic pigment C.I Pigment Red 177, and its traditional synthesis method is based on bromic acid The raw material...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/32C07C309/53
Inventor 费学宁曹凌云朱森赵洪宾
Owner TIANJIN CHENGJIAN UNIV
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