CN101173112A - Novel method for producing reduction eriochrome BC(C.I. Vat Blue 6) - Google Patents

Abstract

The invention relates to a novel method for producing and preparing vat blue BC (C. I. Vat Blue 6). The method comprises the steps as follows: vat blue RSN is prepared as raw materials to dissolve in oil of vitriol; chlorination is conducted by two steps, thereby making full use of the raw materials chlorine gas; wherein, the byproducts of the reaction are few; after crystallizing and filtering, the chloridized product is washed with vitriol in 70 percent, and is deacidized in acidic condition. The invention improves the quality, reduces the consumption of raw materials and increases the economic benefit.

Description

Blue BC (C.I. Vat Blue 6) novel preparation method is floated in reduction

Technical field:

The present invention relates to a preparation reduction and float the production novel preparation method of blue BC (C.I.Vat Blue 6).

Background technology:

Vat dyes is the high-grade dyestuff that a veriety is numerous, bright in colour, fastness is excellent, be widely used in the printing and dyeing of cotton, hair, silk, fiber crops, synthon and BLENDED FABRIC thereof, intertexture, because vat dyes has good sun-proof, weather, heat-resisting, anti-molten Ji, washing fastness.Wherein many kinds can be made into pigment dyestuff through special processing, and it is painted to be used for paint, plastics, rubber and coating aspect.

The general production technique of vat dyes is numerous and diverse, and three-waste pollution is serious, and under current environmental protection pressure, the production technique of vat dyes and intermediate thereof is improved in this class vat dyes development very important.

It is anthrone class vat dyes that blue BC dyestuff is floated in reduction, is one of kind very important in the vat dyes, dyes the cotton vivid sky blue that is, fastness is good, and fast light, anti-chlorine floats, alkaline resistance properties is good.

The production embodiment:

1, in dissolution kettle, add the vitriol oil, controlled temperature at 30 ℃ with 300 kilograms in interior slow input Vat Blue RSN dry powder.After stirring fully dissolving, adding water acid adjustment degree is 84-86%, and binder is to tail chlorine still.

2, tail chlorine still charging is warming up to 52-54 ℃, is incubated 10 minutes.Throw 3.5 kilograms of Manganse Dioxide, begin logical chlorine, the logical chlorine time is as the criterion to the chlorination terminal point with main chlorine still.

3, the logical chlorine of main chlorine still is thrown 6 kilograms of Manganse Dioxide earlier, and continuous logical after 4 hours, logical chlorine temperature is controlled at cl content and is controlled between the 13.5-14%.

4, be discharged to crystallization kettle, the crystallization kettle charging, temperature control is in 35 ℃, time is about 40 minutes, and acidity control is at 81-82.5%, and the back drips separating water 40-45 lattice, top temperature is no more than 45 ℃, acidity control is at 75-76%, stir be cooled to 30 ℃ static, static 16 hours, the filter charging, mother liquor is collected the appointment basin, and blowing is finished in charging, with 75% sulfuric acid scrubbing of preparation.

5, washing finishes back blowing, discharging.

6, add fuming acid 625L in reduction kettle, open and stir, slowly drop into the crystallization material in the 5th step in still, temperature is controlled in 35 degree, stirs 30 minutes, adds fuming acid 300L in still, and temperature is controlled in 35 degree, pulls an oar 16 hours.

7, in reduction kettle, add water 4500L, throw sodium sulphite anhydrous 99.3 250kg; Cover kettle cover, stirring and dissolving slowly dripped for the 6th step to break the material of oar still in still, and temperature is strict controlled in 50 degree, drip finish after, be incubated 5 hours, temperature is controlled between 45～50 degree during insulation, after insulation finishes, the survey terminal point of taking a sample.Add soft water 900L after qualified, controlling acidity is 25%～30%, be cooled to 35 degree blowings advance filter with 50 degree water washings to neutrality, blowing, discharging, dry must the reduction are floated blue BC (C.I.VatBlue 6) product.

Claims (2)

1. the formula compound that structure is following.

2. the preparation method of the compound of claim 1, it is characterized in that through following steps: with sulfuric acid is solvent, sulphonating agent, logical chlorine makes the Vat Blue RSN chlorination under the catalyzer condition, restores and must reduce and float blue BC (C.I.Vat Blue 6) product.

It is characterized in that:

The former dyestuff of exsiccant Vat Blue RSN is a sulphonating agent with the vitriol oil in concentrated sulfuric acid solution, and Manganse Dioxide is catalyzer, feeds chlorine, makes its chlorination generate thick reduction and floats blue BC.Temperature of reaction is carried out in this reaction chlorination reactor between 52-54 ℃.Material after the chlorination restores to such an extent that blue BC (C.I.Vat Blue 6) is floated in reduction under acidic conditions.This process temperature is strict controlled in 50 degree.