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A kind of vat blue rsn preparation method

A raw material, aminoanthraquinone technology, applied in the field of preparation of vat blue RSN, can solve the problems of reduced total yield, darkening of dye hue, failure to meet quality requirements, etc., and achieves improved product quality, less impurity components, and production costs. low effect

Active Publication Date: 2016-07-13
安徽融创化工科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although the vat blue RSN obtained by the above method contains less unknown impurities than the previous process, these unknown impurities will darken the color of the dye and fail to meet the normal quality requirements
In order to remove these impurities, the product must be purified by hydrosulfite treatment, and the total yield after refining is reduced, up to 92%.

Method used

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  • A kind of vat blue rsn preparation method
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  • A kind of vat blue rsn preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 500mL four-necked flask, add 75g of DMS as a solvent, 0.23g of catalyst, and 50g of 1-aminoanthraquinone with a purity of 98.5%, stir, slowly raise the temperature to 125°C, and keep at 125-130°C for 1 hour to fully dissolve. After the dissolution, add 5g of water in 0.5h, adjust the temperature to 110-115°C, slowly and uniformly add 40g of potassium hydroxide aqueous solution with a concentration of 50% in 2.5h, and control the temperature at 110-115°C during the dropping process; , kept at 150-155°C for 5 hours, until the balance of 1-aminoanthraquinone reached 0.25%, the condensation reaction was completed; add 230g of dilution water (previous distillate water can be applied), press filter, the pH value of the filter cake is 7.2, wash until neutral, After drying, 49.5g vat blue RSN is obtained, with a yield of 99.0%. The appearance is a dark blue uniform powder, which is directly used for cloth printing and dyeing. The product is bright in color, and parameters s...

Embodiment 2

[0033] In a 500mL four-neck flask, add 90g of DMS as a solvent, 0.27g of catalyst, and 50g of 1-aminoanthraquinone with a purity of 98.5%, stir, slowly raise the temperature to 125°C, and keep at 125-130°C for 1 hour to fully dissolve. After the dissolution is completed, add 5g of water in 0.5h, adjust the temperature to 115-120°C, slowly and evenly add 60g of potassium hydroxide aqueous solution with a concentration of 50% dropwise for 3h, and control the temperature during the dropping process at 115-120°C; after the addition is completed, Incubate at 130-135°C for 5 hours, and the condensation reaction is complete when the balance of 1-aminoanthraquinone is 0.67%; add 270g of dilution water (previous distillate water can be applied), press filter, the pH value of the filter cake is 7.8, wash until neutral, and dry , to get 49.7g vat blue RSN, the yield is 99.4%, the appearance is dark blue uniform powder, directly used for cloth printing and dyeing, the product is bright in ...

Embodiment 3

[0036] In a 500mL four-neck flask, add solvent 110g DMS, 0.3g catalyst, 50g 1-aminoanthraquinone with a purity of 98.5%, stir, slowly raise the temperature to 125°C, keep at 125-130°C for 1 hour, and fully dissolve. After the dissolution, add 5g of water in 0.5h, adjust the temperature to 120-125°C, slowly and uniformly add 50g of potassium hydroxide aqueous solution with a concentration of 50% in 2.5h, and control the temperature at 120-125°C during the dropping process; , kept at 140-145°C for 5 hours, until the balance of 1-aminoanthraquinone reached 0.42%, the condensation reaction was completed; add 260g of dilution water (previous distillate water can be applied), press filter, the pH value of the filter cake is 7.5, wash until neutral, After drying, 48.9g vat blue RSN was obtained, with a yield of 97.8%. The appearance was a dark blue uniform powder, which was directly used for cloth printing and dyeing.

[0037] After the sodium hydroxide solution and hydrosulfite were...

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Abstract

The invention provides a method for preparing vat blue RSN. The method includes that the vat blue RSN is made of 1-amino-anthraquinone, the 1-amino-anthraquinone, alkaline condensing agents and air are subjected to condensation reaction under the effects of phase-transfer catalysts in solvent DMS (dimethyl sebacate) and are diluted, filtered, washed and dried to obtain the vat blue RSN, and the alkaline condensing agents and air are used as oxidizing agents. The method has the advantages that reactants are good in dispersibility in the solvent DMS and are high in reaction speed and good in selectivity, the prepared product has few impurity compositions and is low in impurity composition content, and the solvent is stable in performance and easy to recycle; the method is low in production cost and short in time, reaction can be carried out at one step, high-purity and high-yield vat blue RSN dyestuffs can be obtained without refining, the solvent can be recycled, accordingly, waste gas, waste water and solid waste pollution and emission can be reduced, and the yield can reach 99% at least.

Description

technical field [0001] The invention belongs to the technical field of dye preparation, and relates to a preparation method of vat blue RSN. Background technique [0002] Vat blue RSN, that is, dianthrone-N, N'-dihydroazine, is the earliest anthraquinone vat dye, and its structural formula is: [0003] [0004] According to dye nomenclature, Vat Blue RSN is expressed as a reddish vat blue dye with standard intensity, named C.I. Vat Blue 4 according to the "Dye Index". So far it is still the most important vat dye species with the largest output. Vat blue RSN has bright color and excellent fastness to light, alkali, washing and perspiration, but it is not resistant to chlorine bleaching. It is mainly used for dyeing cotton fiber, viscose fiber, vinylon, etc., and can also be used as an organic pigment. [0005] The traditional production process is to use 2-aminoanthraquinone as raw material, conduct condensation and closed ring in molten potassium hydroxide, sodium hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D241/38C07D241/36C07D241/00C09B5/48
Inventor 郭元王洪卫王方玉徐卉香李振张怀永高鸿宇
Owner 安徽融创化工科技股份有限公司