Phenoxylation process for preparing disperse blue 2BLN

A technology of phenoxylation and disperse blue, which is applied in the field of disperse blue preparation, can solve problems such as slowing down the production progress, achieve the effects of reducing by-products, facilitating drying, and avoiding caking

Pending Publication Date: 2022-02-18
QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the application of this invention is small batch production. After increasing the amount of feed, this solution cannot avoid the occurrence of material hardening and other phenomena that greatly slow down the production progress.

Method used

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  • Phenoxylation process for preparing disperse blue 2BLN
  • Phenoxylation process for preparing disperse blue 2BLN

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] In this embodiment, a dispersed blue 2BLN phenoxylated product was prepared using the following method:

[0042] (1) The purification step is added to the product of sulfite after 醌 after a nitrification reaction, and the molar ratio of sodium sulfite and the sulfite primary nitrification product is 0.68: 1, and the system pH adjustment before joining sodium sulfite. 10.5;

[0043] (2) Potassium hydroxide and phenol are added to the phenoxylated reaction kettle, heated to 99 ° C, and heat it up to 145 ° C using the reaction heat, stirred at 145 ° C for 40 min, and the material is completely dissolved to 118 ° C The intermediate product obtained by adding step (1), allowing the molar ratio of phenol to the intermediate product to 2.65: 1, followed by warming to 147 ° C, and the insulation reaction is 4.5h;

[0044] (3) After the insulation reaction is completed in step (2), the mixed alkali is rapidly added to the reaction system under 95 ° C, stir mixed with 40 min, and the...

Embodiment 2

[0047] In this embodiment, a dispersed blue 2BLN phenoxylated product was prepared using the following method:

[0048] (1) The purification step is added to sodium sulfite in a product after hydrazine after a nitrification reaction, and the molar ratio of sodium sulfite and sulfite and the anthraquinone is 0.7: 1, and the system pH is adjusted before joining sodium sulfite. 12;

[0049] (2) Add potassium hydroxide and phenol, heated to 98 ° C, and heat it up to 143 ° C using the reaction heat, stirred at 143 ° C for 50 min, and cool down to 118 ° C after storage. The intermediate product obtained by adding step (1) so that the molar ratio of phenol and the intermediate product reaches 2.6: 1, followed by warming to 145 ° C, and the insulation reaction is 3.5 h;

[0050] (3) After the insulation reaction is completed in step (2), the mixed alkali is rapidly added to the reaction system under 97 ° C, and stir mixed with 35 min, and then the water of 95 ° C was diluted, and the mixt...

Embodiment 3

[0053] In this embodiment, a dispersed blue 2BLN phenoxylated product was prepared using the following method:

[0054] (1) The purification step is added to sodium sulfite in the product after after a nitrification reaction, and the molar ratio of sodium sulfite and the hydrazine primary nitrification product is 0.6: 1, and the system pH is adjusted before joining sodium sulfite. To 11;

[0055] (2) Add potassium hydroxide and phenol, heated to 95 ° C, and heat it up to 140 ° C using the reaction heat, stirred at 140 ° C for 45 min, and cool down to 120 ° C after storage. The intermediate product obtained by adding step (1) so that the molar ratio of phenol and the intermediate product reaches 2.7: 1, followed by warming to 142 ° C, and the reaction reaction is 6 h;

[0056] (3) After the insulation reaction is completed, the mixed alkali is rapidly added to the reaction system at 90 ° C, and the mixture is mixed at 90 ° C, and then the water of 90 ° C is diluted, and the dilutio...

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Abstract

The invention discloses a phenoxylation process for preparing disperse blue 2BLN. The process comprises the step of carrying out a phenoxylation reaction on an intermediate product having been subjected to primary nitration and refining. According to the process, the addition amount of sodium sulfite in the refining step is increased to make a molar ratio of sodium sulfite to a primary nitration product to reach (0.6-0.7): 1, and the addition amount of phenol in the phenoxylation reaction is increased to make a molar ratio of the phenol to the intermediate product to reach (2.6-2.8): 1. According to the process provided by the invention, by adjusting the reaction conditions and related parameters of the refining step and the phenoxylation reaction, the quality of the phenoxylation product is improved, a melting point is increased, the phenomenon of material caking generated in a subsequent drying process is avoided, the frequency of cleaning equipment is reduced while the equipment is protected from being damaged by a caked material, and production efficiency is greatly improved; and the process is suitable for promotion and application.

Description

Technical field [0001] The present invention belongs to the technical field of Disperse Blue prepared, in particular, relates to a dispersion of blue 2BLN phenoxy process for preparing. Background technique [0002] Disperse Blue 2BLN is one of the largest disperse blue dye yield two species, and the molecular structure and excellent application performance and dyeing anthraquinone type, occupy an important position in certain dye industry. In recent years, due to the growth of the market for Disperse Blue 2BLN demand, the general concern of the business, making it imperative to solve the technical problems Disperse Blue 2BLN produced in mass production. [0003] Currently, blue 2BLN dispersion preparation generally includes first nitrated, of phenoxy, second nitration, reduction, and hydrolysis reactions bromide process steps. Wherein the anthraquinone intermediate target after the first nitration obtained was 1,5-dinitro-anthraquinone or 1,8-dinitro anthraquinone, the intermedi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B1/503
CPCC09B1/503
Inventor 孙善起许佳伟王守满王永康王炳强李文青
Owner QINGDAO DOUBLE PEACH SPECIALTY CHEM GRP
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