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Improved method for preparing c.i. Vat Blue 4

A technology of aminoanthraquinone and pyridazine, applied in the field of preparing C.I. Vat blue 4, can solve the problems of high viscosity of reactants, high reaction temperature, low yield and the like

Active Publication Date: 2017-05-24
NANTONG HENGSHENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] (1) The melting condensation reaction temperature of 2-aminoanthraquinone is higher, causes condensation product: the yield of 6,15-dihydrodianthracene pyridazine-5,9,14,18-tetraketone is on the low side (about 50 %about);
[0007] (2) Although the temperature of the melting and condensation reaction is higher, the viscosity of the reactant is still very large, in order to strengthen the stirring effect, special reaction equipment is required;

Method used

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  • Improved method for preparing c.i. Vat Blue 4
  • Improved method for preparing c.i. Vat Blue 4
  • Improved method for preparing c.i. Vat Blue 4

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preparation example Construction

[0025] Compared with the preparation method of traditional C.I. Vat Blue 4, the present invention has the following advantages:

[0026] (1) The reaction temperature of the condensation reaction of aminoanthraquinone (1-aminoanthraquinone or 2-aminoanthraquinone) is reduced, and the reaction temperature of 6,15-dihydrodianthracene pyridazine-5,9,14,18-tetra The yield of ketone (about 80%);

[0027] (2) No need to use hydrosulfite to reduce and refine 6,15-dihydrodianthracene pyridazine-5,9,14,18-tetraketone;

[0028] (3) Since the condensation reaction of aminoanthraquinone (1-aminoanthraquinone or 2-aminoanthraquinone) is carried out in an aprotic polar organic solvent (reducing the viscosity of the reaction material), a common reactor can be used (no need to use special reaction equipment).

Embodiment 1

[0035] Add cesium hydroxide (134.9g, 0.90mol), 1,5-diazabicyclo[4.3.0]non-5-ene (148.7, 1.20mol) and o-dichlorobenzene (180g ), under nitrogen protection, heated to 100°C under stirring, and then added 1-aminoanthraquinone (66.9g, 0.30mol) when the solid was completely dissolved. The raw material point disappeared (about 12h), stopped heating, cooled naturally to room temperature, diluted with methanol and filtered, the filter cake was washed with methanol until there was no obvious smell, and 54g of dark blue solid was obtained after drying, with a yield of 80%.

Embodiment 2

[0037] Add cesium hydroxide (134.9g, 0.90mol), 1,5-diazabicyclo[4.3.0]non-5-ene (148.7g, 1.20mol) and o-dichlorobenzene ( 180g), under nitrogen protection, heated to 100°C under stirring, and then added 2-aminoanthraquinone (66.9g, 0.30mol) when the solid was completely dissolved. Stop heating until the raw material point disappears, cool naturally to room temperature, add methanol to dilute and filter, the filter cake is washed with methanol until there is no obvious smell, and after drying, 55 g of dark blue solid is obtained, with a yield of 81%.

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Abstract

The invention relates to a method for preparing C.I.vat blue 4.The method comprises the steps of preparing 6,15-dihydro-5,9,14,18-anthrazinetetrone and dying 6,15-dihydro-5,9,14,18-anthrazinetetrone.The method is characterized in that according to the main steps of the step 1, on the condition of existence of a mixture of inorganic base and organic base and inert gas, 2-amino anthraquinone or 1-amino anthraquinone react in non-proton polarity organic solvent at the temperature of 140-180 DEG C so that a target object can be obtained, and the target object does not need to be reduced or refined with sodium dithionite and is directly used in the step 2.The yield of the 6,15-dihydro-5,9,14,18-anthrazinetetrone is increased, the steps of preparing the C.I.vat blue 4 are more concise, and the method for preparing the C.I.vat blue 4 has higher commercial value.

Description

technical field [0001] The present invention relates to a kind of preparation method of blue vat dye, specifically, relate to a kind of method of preparation C.I. vat blue 4. Background technique [0002] C.I. Vat Blue 4 (chemical composition is 6,15-dihydrodianthracene pyridazine-5,9,14,18-tetraketone (its structure is shown in formula Ⅰ), trade name: Vat Blue RSN, commonly known as "blue Anthrone") is one of the most widely used varieties of vat dyes, mainly used for dyeing cotton fabrics with light resistance, washing resistance and perspiration fastness. [0003] [0004] The traditional method for preparing C.I. Vat Blue 4 is: use 2-aminoanthraquinone as a raw material, and undergo fusion condensation of an inorganic mixed alkali (such as potassium hydroxide-sodium hydroxide) (the melting condensation reaction temperature is 220°C to 230°C) to obtain 6 , 15-dihydrodianthracene pyridazine-5,9,14,18-tetraketone, which becomes a dye after being refined with sodium bica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B5/48C09B5/50
CPCC09B5/48C09B5/50
Inventor 沈永嘉邹盼盼周长凯陶雪松候嘉祺
Owner NANTONG HENGSHENG FINE CHEM
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