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A kind of environment-friendly preparation method of solvent blue 104 dye

A dyestuff and environmental protection technology, applied in the field of environmental protection preparation of solvent blue 104 dyes, can solve the problems of pollution, low reaction purity, long reaction time, etc., and achieve the effects of reducing emissions, reducing pollution, and improving conversion rate and yield.

Active Publication Date: 2019-04-02
中关村科技租赁股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing solvent blue 104 production process has a long reaction time, low reaction purity, and a large amount of washing wastewater for production, which is easy to cause pollution to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The present embodiment provides a kind of environment-friendly preparation method of solvent blue 104 dyestuff, and it comprises the following steps:

[0014] (a) 1,500kg of mesitidine, which has been accurately measured manually, is vacuum pumped into a 2000L reactor, and 425kg of 1,4-dihydroxyanthraquinone, 175kg of 1,4-dihydroxyanthraquinone leuco, Put in 75kg of boric acid and 75kg of catalyst (salicylic acid), and then heat up to 125°C for condensation reaction under normal pressure for 18 hours; install a condensate receiving tank in the secondary freezing and condensing device for the tail gas of the reactor, and the receiving liquid is mainly water and homogeneous Trimethylaniline, after layered separation, the mesitidine in the upper layer is reused, and the wastewater in the lower layer enters the sewage treatment station;

[0015] (b) Cool the material in the reactor to 60°C, add 1000kg of methanol for isolation, and then cool down to 40°C; transport it to a ...

Embodiment 2

[0017] The present embodiment provides a kind of environment-friendly preparation method of solvent blue 104 dyestuff, and it comprises the following steps:

[0018] (a) Vacuum pump 1200 kg of mesitidine accurately measured manually into the 2000L reactor, and put in 300 kg of 1,4-dihydroxyanthraquinone, 150 kg of 1,4-dihydroxyanthraquinone leucosome, Put in 80kg of boric acid and 100kg of catalyst (acetic acid), and then heat up to 130°C for condensation reaction under normal pressure for 15 hours; install a condensate receiving tank in the secondary freezing and condensing device for the tail gas of the reactor, and the receiving liquid is mainly water and mesitylene , after layered separation, the mesitidine in the upper layer is reused, and the wastewater in the lower layer enters the sewage treatment station;

[0019] (b) Cool the material in the reactor to 50°C, add 1000kg of methanol to isolate, then cool down to 30°C; transport it to a closed suction filter tank throug...

Embodiment 3

[0021] The present embodiment provides a kind of environment-friendly preparation method of solvent blue 104 dyestuff, and it comprises the following steps:

[0022] (a) Vacuum pump 1800kg of mesitidine accurately measured manually into a 2000L reactor, and put in 500kg of 1,4-dihydroxyanthraquinone, 200kg of 1,4-dihydroxyanthraquinone leuco, Put in 150kg of boric acid and 100kg of catalyst (glycolic acid), then raise the temperature to 128°C for condensation reaction under normal pressure for 18 hours; install a condensate receiving tank in the secondary freezing and condensing device for the tail gas of the reactor, and the receiving liquid is mainly water and mesitylene Aniline, after layered separation, the mesitidine in the upper layer is reused, and the wastewater in the lower layer enters the sewage treatment station;

[0023] (b) Cool the material in the reactor to 70°C, add 1000kg of methanol for isolation, and then cool down to 50°C; transport it to a closed suction ...

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PUM

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Abstract

The invention relates to an environment-friendly preparation method of solvent blue 104 dye. The preparation method comprises the following steps: (a) adding 2,4,6-trimethylaniline into a reaction vessel, adding 1,4-dihydroxy anthraquinone, a 1,4-dihydroxy anthraquinone leuco compound, boric acid and a catalyst while stirring, then heating to 125-130 DEG C, and reacting for 15-18 hours to the end point, wherein the mass ratio of the 2,4,6-trimethylaniline, the 1,4-dihydroxy anthraquinone, the 1,4-dihydroxy anthraquinone leuco compound, the boric acid and the catalyst is (12-18):(3-5):(1.5-2):(0.8-1.5):1; and the catalyst is a mixture of one or more of acetic acid, hydroxyacetic acid and salicylic acid; and (b) cooling the product of the step (a) to 50-70 DEG C, then adding methanol, segregating, stirring, then cooling to 30-50 DEG C, performing vacuum filtration, washing, and drying. Thus, the conversion rate and yield of the product can be improved, and the discharge of waste can be reduced, thereby being beneficial to relieving environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of a dye, in particular to an environment-friendly preparation method of solvent blue 104 dye. Background technique [0002] Solvent blue 104 is usually used in packaging, decoration, paint, ink and coloring of polyester, nylon, etc.; also known as 1,4-bis[(2,4,6-trimethylphenyl)amino]-9,10- Anthracenedione, chemical formula C 32 h 30 N 2 o 2 , CAS No. 116-75-6. The existing solvent blue 104 production process has a long reaction time, low reaction purity, and a large amount of washing wastewater for production, which easily causes pollution to the environment. Contents of the invention [0003] The object of the invention is to provide an environmentally friendly preparation method of solvent blue 104 dye in order to overcome the deficiencies in the prior art. [0004] In order to achieve the above object, the technical solution adopted in the present invention is: a kind of environment-friendly pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09B1/32
CPCC09B1/325
Inventor 杨庆水周利霞陶一敏
Owner 中关村科技租赁股份有限公司
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