Preparation method of bromaminic acid sodium salt and intermediate of bromaminic acid sodium salt and solvent recovery method

A recovery method and a solvent technology, which are applied in the field of preparation of bromine sodium salt and its intermediates and solvent recovery, can solve the problem of incomplete dilution and stratification of dilute sulfuric acid, reduced conversion rate of sulfonation reaction, and low yield of sulfonated products and other problems, to achieve the effect of reducing cost, unaffected purity, and high purity of solvent

Inactive Publication Date: 2017-04-19
YANTAI ANOKY FINE CHEM CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the incomplete dilution and stratification with dilute sulfuric acid in the process of preparing bromonic acid in the prior art, which leads to a low yield of sulfonated products and the recovered ortho-dichloro Direct recycling of benzene will reduce the conversion rate of the sulfonation reaction, thus providing a preparation method for bromine sodium salt and its intermediates, which uses o-dichloride that is completely separated and recycled during concentrated sulfuric acid extraction. Benzene can be directly applied to produce bromic acid and its sodium salt with higher yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046]The preparation method of the bromine sodium salt of the present embodiment comprises the steps:

[0047] (1) Sulfonation reaction: Add 259.0g of o-dichlorobenzene and 29.60g (0.13mol) of 1-aminoanthraquinone into a 500mL four-necked flask, stir and heat up to 115-120°C, dehydrate for 1.5-2h, and cool down to 70°C , slowly add 21.14g (0.18mol) of chlorosulfonic acid dropwise, finish adding 1.5h, keep warm for 1h, raise the temperature to 135°C, keep warm for 2h, take a sample test to the end, the main production is 1-aminoanthraquinone-2-sulfonic acid by HPLC test The purity is 96.25%.

[0048] (2) Extraction and stratification: after the end of sulfonation, cool to 55°C, add 133.2g of concentrated sulfuric acid, stir for 30min, pour into a separatory funnel and stand for 3-4h for extraction and separation, the upper layer is 249.9g o-dichlorobenzene, and the lower layer is The sulfonated material layer was 181.91 g, and the yield of 1-aminoanthraquinone-2-sulfonic acid...

Embodiment 2

[0053] The preparation method of the bromine sodium salt of the present embodiment comprises the steps:

[0054] (1) Sulfonation reaction: Add 249.9 g of o-dichlorobenzene obtained in step (5) of Example 1 to a 500 mL four-necked flask, add 9.1 g of neo-o-dichlorobenzene, 29.60 g of 1-aminoanthraquinone, and stir Heat up to 115-120°C for dehydration, keep warm for 1.5-2h, cool down to 70°C, slowly add 21.14g of chlorosulfonic acid dropwise, finish adding 1.5h, keep warm for 1h, heat up to 135°C, keep warm for 2h, the main product is 1- The purity of aminoanthraquinone-2-sulfonic acid is 96.58%.

[0055] (2) Extraction and stratification: After the end point of sulfonation, cool to 55°C, add 133.2g of concentrated sulfuric acid, stir for 30min, pour it into a separatory funnel and let it stand for 3-4h for extraction and separation. The upper layer is 248.9g o-dichlorobenzene, and the lower layer is The sulfonated material layer was 180.35 g, and the yield of 1-aminoanthraquin...

Embodiment 3

[0060] The preparation method of the bromine sodium salt of the present embodiment comprises the steps:

[0061] (1) Sulfonation reaction: Add 246.41 o-dichlorobenzene obtained in step (3) of Example 2 to a 500mL four-necked flask, add 12.59g new o-dichlorobenzene, 29.60g 1-aminoanthraquinone, and stir Heat up to 115-120°C for dehydration, keep warm for 1.5-2h, cool down to 70°C, slowly add 21.14g of chlorosulfonic acid dropwise, finish adding 1.5h, keep warm for 1h, heat up to 135°C, keep warm for 2h, the main product is 1- The purity of aminoanthraquinone-2-sulfonic acid is 96.22%.

[0062] (2) Extraction and stratification: after the end of sulfonation, cool to 55°C, add 133.2g of concentrated sulfuric acid, stir for 30min, pour into a separatory funnel and stand for 3-4h for extraction and separation, the upper layer is 248.6g o-dichlorobenzene, and the lower layer is The sulfonated material layer was 181.35 g, and the yield of 1-aminoanthraquinone-2-sulfonic acid in the ...

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PUM

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Abstract

The invention discloses a preparation method of bromaminic acid sodium salt and an intermediate of the bromaminic acid sodium salt and a solvent recovery method. The preparation method of 1-aminoanthraquinone-2-sulfonic acid comprises the following steps that (1) in an inert solvent, a sulfonation reaction is conducted on 1-aminoanthraquinone and chlorosulfonic acid; (2) secondly, after the sulfonation reaction in the step (1) is ended, layered extraction is conducted with concentrated sulfuric acid, the upper layer is a solvent organic phase layer, and the lower layer is a material layer containing the 1-aminoanthraquinone-2-sulfonic acid and sulfuric acid. By the adoption of the preparation method of the 1-aminoanthraquinone-2-sulfonic acid, the extraction layering is complete, and the yield of the 1-aminoanthraquinone-2-sulfonic acid is high. Meanwhile, a method of recycling the solvent with water is adopted, the recycled solvent can be directly used for preparation of bromamine acid and sodium slat of the bromamine acid, and the bromamine acid is high in yield.

Description

technical field [0001] The invention relates to a preparation method and a solvent recovery method of bromine sodium salt and its intermediate. Background technique [0002] Bromine sodium salt, the chemical name is 1-amino-4-bromoanthraquinone-2-sodium sulfonate, and the CAS number is 116-81-4. Bromine sodium salt is an important dye intermediate, which is mainly used in the production of important dyes such as disperse, acid and reactive dyes. The bromination process for preparing bromine sodium salt is to replace 1-amino-anthraquinone-2-sulfonic acid with bromine, and then neutralize with alkali to obtain sodium salt. [0003] 1-Amino-4-bromoanthraquinone-2-sulfonic acid, commonly known as bromic acid, has a red needle-like crystal appearance, is easily soluble in water, and is in the form of orange-red paste or powder. It is mainly used in dye intermediates to manufacture acid anthraquinone dyes, and is widely used in the preparation of anthraquinone acid dyes and disp...

Claims

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Application Information

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IPC IPC(8): C07C303/08C07C309/47C07C17/38C07C25/08C07C201/16C07C205/06C07C303/22C07C309/48C07C303/32
CPCC07C303/08C07C17/38C07C201/16C07C303/22C07C303/32C07C309/47C07C25/08C07C205/06C07C309/48
Inventor 曲美君李诗杰刘祥庆尹程琳
Owner YANTAI ANOKY FINE CHEM CO LTD
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