CN103627209A

CN103627209A - Preparation method of polycarboxy water-soluble sulfur black

Info

Publication number: CN103627209A
Application number: CN201310496902.4A
Authority: CN
Inventors: 潘毅
Original assignee: DALIAN JX CHEM-INDUSTRIAL CORP
Current assignee: DALIAN JX CHEM-INDUSTRIAL CORP
Priority date: 2013-10-22
Filing date: 2013-10-22
Publication date: 2014-03-12

Abstract

The invention relates to a preparation method of polycarboxy water-soluble sulfur black. The preparation method comprises the steps of adding double sulfur black, water and sodium hydroxide into a reaction kettle, heating to 140 DEG C, hydrolyzing, keeping the reaction for 7-8h, keeping the pressure in the kettle at 0.3mpa, and then cooling to 40 DEG C; adding a sodium chloroacetate water solution and polycarboxylic aldehyde which are well prepared in advance, performing reflux at the temperature of 90-95 DEG C for 6-8h, and cooling materials to 40 DEG C; dropping hydrochloric acid while stirring to regulate the pH value to 1-2, reacting till an end point of totally precipitating the materials, and filtering to obtain a filter cake for later use; adding water into the filter cake, stirring, regulating the pH value to 7-8 by using sodium carbonate, and drying. As the internal structure of the product prepared by the preparation method provided by the invention has an additional polycarboxylic group, the product can be used for dyeing cotton, flax and fabric, as well as leather; the product has relatively good dye uptake and dyeing pitch black degree, and the resistance to dry and wet friction is in line with the national standard; compared with a special leather dye, the price is cheap.

Description

A kind of preparation method of many carboxyls solubilised sulphur black

technical fieldthe present invention relates to a kind of preparation method of fine chemical product.

background technologythe preparation method of solubilised sulphur black is as follows: nitro chlorobenzene adds reaction of Salmon-Saxl with sodium polysulphide carries out under certain pressure and temperature after hydrolysis, then blowing oxidation, after filtering, obtains after the sulfonation of drying with Sodium Pyrosulfite effect.Product is mainly used in the dyeing of cotton, fiber crops, fabric.Because the inorganic salt that product includes are more, little to the dye penetration power of leather, the scope of application limits to some extent.

summary of the inventionthe object of the present invention is to provide a kind of dyeing that not only can be used on the article such as cotton, fiber crops can also be for the preparation method of many carboxylics solubilised sulphur black of the dyeing of leather.

1, raw material used is as follows:

Double sulphur black intensity >=220%

Sodium hydrate content >=96%

Content of hydrochloric acid >=30%

Sodium chloroacetate content >=98%

Many carboxyls aldehyde >=97%

2, making method is as follows:

1) by double sulphur black, water, sodium hydroxide in mass ratio 1:3-4:0.9-1 add and in reactor, be warming up to 140 ℃ of hydrolysis, keep reaction 7-8 hour, then still internal pressure 0.3mpa cools to 40 ℃.Add again the sodium chloroacetate aqueous solution and the many carboxyls aldehyde that prepare in advance, wherein the mass ratio of sodium chloroacetate and sulphur black is 0.95-1.0, the mass ratio of many carboxyls aldehyde and sulphur black is 0.18-0.20, and it is in its quality 2.2-2.5 water doubly that sodium chloroacetate is dissolved in, in 90-95 ℃ of backflow 6-8 hour, material is cooled to 40 ℃.

2) stir the lower hydrochloric acid tune PH:1-2 that drips, material is all separated out as terminal, filters, and filter cake is continued to employ.

3) filter cake adds water stirring, with sodium carbonate, is adjusted to PH:7-8, dry.

The present invention compared with prior art tool has the following advantages:

1. because this interiors of products structure has increased many carboxyls, not only can be used for the dyeing of cotton, fiber crops, fabric, also can be used for the dyeing of leather.

2. product has the pitch black degree of good dye uptake and dyeing, and resistance to dry wet friction meets GB, compares low price with special-purpose leather dyestuff.

Embodiment

example 1

The double sulphur black 260g of intensity 223% and water 940g are added in reactor, under stirring, add sodium hydroxide 250g, close charging opening, be warming up to 140 ℃, insulation 8h, still internal pressure 0.3mpa, then cools to 40 ℃.Another water intaking 580g, adds sodium chloroacetate 252g, stirring and dissolving, and the Mono Chloro Acetic Acid aqueous solution that this is prepared is added in reactor, and adds many carboxyls aldehyde 50g, and by reflux valve opening, material is warming up to 95 ℃, refluxes 6 hours, lowers the temperature 40 ℃.Hydrochloric acid is dripped in reactor, adjust PH:1, material is all separated out as terminal, filters, and filter cake is continued to employ.Filter cake is added in reactor, add water 1000ml, stir, with sodium carbonate, adjust PH:7, material all scatters, and then carries out roller drying, obtains 430g product of the present invention.

example 2

The double sulphur black 260g of intensity 220% and water 1040g are added in reactor, under stirring, add sodium hydroxide 260g, close charging opening, be warming up to 140 ℃, insulation 7h, still internal pressure 0.3mpa, then cools to 40 ℃.Another water intaking 610g, adds sodium chloroacetate 247g, stirring and dissolving, and the Mono Chloro Acetic Acid aqueous solution that this is prepared is added in reactor, and adds many carboxyls aldehyde 52g, and by reflux valve opening, material is warming up to 90 ℃, refluxes 8 hours, lowers the temperature 40 ℃.Hydrochloric acid is dripped in reactor, adjust PH:2, material is all separated out as terminal, filters, and filter cake is continued to employ.Filter cake is added in reactor, add water 1000ml, stir, with sodium carbonate, adjust PH:8, material all scatters, and then carries out roller drying, obtains 427g product of the present invention.

Claims

1. a preparation method for the solubilised sulphur black of carboxyl more than, is characterized in that:

1) by double sulphur black, water, sodium hydroxide in mass ratio 1:3-4:0.9-1 add and in reactor, be warming up to 140 ℃ of hydrolysis, keep reaction 7-8 hour, still internal pressure 0.3mpa, then cool to 40 ℃, add again the sodium chloroacetate aqueous solution and the many carboxyls aldehyde that prepare in advance, wherein the mass ratio of sodium chloroacetate and sulphur black is 0.95-1.0, the mass ratio of many carboxyls aldehyde and sulphur black is 0.18-0.20, and it is in its quality 2.2-2.5 water doubly that sodium chloroacetate is dissolved in, in 90-95 ℃ of backflow 6-8 hour, material is cooled to 40 ℃;

2) stir the lower hydrochloric acid tune PH:1-2 that drips, material is all separated out as terminal, filters, and filter cake is continued to employ;