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Method of preparing solvent blue 14

A solvent, stirring and dissolving technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of many by-products, low conversion rate, low yield, etc., and achieve high product yield and complete reaction , The effect of high solvent recovery rate

Inactive Publication Date: 2018-10-16
JIANGSU DAOBO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The conversion rate of the process product is low; the yield is low; there are many by-products

Method used

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  • Method of preparing solvent blue 14
  • Method of preparing solvent blue 14
  • Method of preparing solvent blue 14

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 204g of water and 23.1g of caustic soda into a 500mL four-necked bottle, stir to dissolve and cool down to room temperature, add 60g of 1,4-dihydroxyanthraquinone, stir for 15 minutes; then add 9g of hydrosulfite, stir and heat up to 55-60 ℃ insulation 1h;

[0023] After the heat preservation is over, add 138g of n-pentylamine, heat up to 88-90°C and heat for 6-12 hours; the yield is 89%, the chromaticity value (DC: 0.5, DH: 0.36, DE: 1.37) is excellent, and the weighted intensity: 101.23 , fully meet customer needs.

Embodiment 2

[0025] Put 204g of water and 23.1g of caustic soda into a 500mL four-necked bottle, stir to dissolve and cool down to room temperature, add 60g of 1,4-dihydroxyanthraquinone, stir for 15 minutes; then add 9g of hydrosulfite, stir and heat up to 55-60 ℃ insulation 1h;

[0026] After the heat preservation is over, add 138g of n-pentylamine, raise the temperature to 88-90°C and heat the reaction for 6-12h; the yield is 90.20%, the chromaticity value (DC: 0.56, DH: 0.45, DE: 1.88) is excellent, and the weighted intensity: 101.33 , fully meet customer needs.

Embodiment 3

[0028] Put 204g of water and 23.1g of caustic soda into a 500mL four-necked bottle, stir to dissolve and cool down to room temperature, add 60g of 1,4-dihydroxyanthraquinone, stir for 15 minutes; then add 9g of hydrosulfite, stir and heat up to 55-60 ℃ insulation 1h;

[0029] After the heat preservation is over, add 138g of n-pentylamine, raise the temperature to 88-90°C and heat the reaction for 6-12h; the yield is 88.90%, the chromaticity value (DC: 0.60, DH: 0.63, DE: 1.90) is excellent, and the weighted intensity: 102.17 , fully meet customer needs.

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Abstract

The invention discloses a method of preparing solvent blue 14. The method comprises the following steps of: feeding water and an caustic soda flake into a container, stirring for dissolution, coolingto a room temperature, adding 1,4-dihydroxy anthraquinone, performing uniform stirring, adding sodium hydrosulfite, stirring and heating to 55-60 DEG C, performing thermal insulation for reaction forabove 1h, generating a leuco body through an oxidoreduction reaction, continuing adding n-amylamine, heating to 88-90 DEG C, performing thermal insulation for reaction for 6-12h, and generating a target product through a condensation reaction. According to the method, reaction time is shortened; the reaction is relatively thorough; a solvent recovery rate is high; a product yield is increased by approximately 5%; almost no byproduct is generated in the reaction; and the target product is excellent in color light and strength.

Description

technical field [0001] The invention relates to a method for synthesizing solvent blue 14, in particular to a method for synthesizing solvent blue 14, which belongs to the field of organic chemical synthesis. Background technique [0002] Solvent blue 14, the chemical name is 1,4-bis(amylamino)anthraquinone; CAS number: 2646-15-3, its structural formula is: [0003] [0004] In the prior art, solvent blue 14 is mainly obtained by reacting 1,4-dihydroxyanthraquinone and n-pentylamine as raw materials, and its reaction formula is as follows: [0005] Main response: [0006] [0007] side effects: [0008] [0009] The conversion rate of the product of this process is low; the yield is low; there are many by-products. Contents of the invention [0010] In order to overcome defects such as low product yield and long reaction time occurring in the above-mentioned process, the present invention proposes a new synthesis method of solvent blue 14. [0011] In order to...

Claims

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Application Information

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IPC IPC(8): C07C221/00C07C225/34
CPCC07C221/00C07C2603/24C07C225/34
Inventor 徐松刘学峰汪港王亚君
Owner JIANGSU DAOBO CHEM