CN103897423A

CN103897423A - Black vat dye and preparation method thereof

Info

Publication number: CN103897423A
Application number: CN201410123179.XA
Authority: CN
Inventors: 朱文朴; 唐波; 陈亿; 吴飞
Original assignee: CHONGQING HUACAI CHEMICAL Co Ltd
Current assignee: CHONGQING HUACAI CHEMICAL Co Ltd
Priority date: 2014-03-27
Filing date: 2014-03-27
Publication date: 2014-07-02

Abstract

The invention relates to a black vat dye and a preparation method thereof, and aims to provide a black vat dye with the advantages of simple process, short production period and good dyeing performance and a preparation method thereof. The black vat dye is prepared by the following method: reacting hydroxylamine sulfate and violanthrone in a solvent in the presence of a catalyst to obtain the black vat dye. By using the property that the violanthrone is dissolved in a sulfuric acid medium, the violanthrone and hydroxylamine sulfate are subjected to chemical reaction under the catalysis of vanadium pentoxide, thus obtaining a violanthrone compound of which the molecular structure contains both amino and hydroxyl. The prepared black vat dye has high black degree in dyed cotton and blended fabrics thereof after post treatment and commercialization, has good dyeing performance, and does not contain carcinogenic aromatic amine, polychlorinated biphenyl or forbidden textile chemicals.

Description

A kind of black vat dye and preparation method thereof

Technical field

The present invention relates to a kind of dye well its preparation method, be specifically related to a kind of black vat dye and preparation method thereof.

Background technology

In prior art, most black, gray vat dye are all derived by violanthrone, and therefore, in the process of research black, gray vat dye, it is necessary strengthening research amino, hydroxyl violanthrone.The black vat dyes such as the B150reactive Black B 150 BB, Vatdirectblack DB, vat direct black 3B or the 3G that used are in the market all the vat dyes as skeleton by violanthrone.Vatdirectblack DB is violanthrone nitrated making in sulfuric acid medium; B150reactive Black B 150 BB is violanthrone two nitrated making in the media such as sulfuric acid, oil of mirbane, Mono Chloro Acetic Acid or Glacial acetic acid; Vat direct black 3B or 3G be violanthrone in vitriol oil medium, nitrated with nitric acid reaction two under the catalysis of Vanadium Pentoxide in FLAKES after through reduction make containing diamino violanthrone.Need further exploitation for violanthrone derivative black dyes.

Summary of the invention

The object of the present invention is to provide black vat dye that a kind of technique dyeing performance simple, with short production cycle, that make is good and preparation method thereof.

For achieving the above object, the technical solution used in the present invention is: a kind of black vat dye is prepared as follows:

Oxammonium sulfate is reacted and makes black vat dye in solvent with violanthrone under catalyst action.

Further, described solvent is that massfraction is the vitriol oil of 85-105%, and described catalyzer is Vanadium Pentoxide in FLAKES.Further preferred, described vitriol oil massfraction is 90-95%.

Further preferred, described vitriol oil consumption is 4-10 times of violanthrone quality.

Further, the add-on of described Vanadium Pentoxide in FLAKES be violanthrone quality 0.001-0.01 doubly.Further preferred, the add-on of described Vanadium Pentoxide in FLAKES is 0.005-0.007 times of violanthrone quality.

Further, described reaction raw materials adds sequencing to be: first add the vitriol oil, add violanthrone again, finally add oxammonium sulfate and Vanadium Pentoxide in FLAKES.

Further, the described vitriol oil and violanthrone add fashionable, system temperature is controlled at not higher than 80 DEG C, added violanthrone after temperature be increased to 100-110 DEG C and constant temperature 0.5-2h, then system is not cooled to and adds oxammonium sulfate and Vanadium Pentoxide in FLAKES again after 70 DEG C.

Further, described oxammonium sulfate and Vanadium Pentoxide in FLAKES are incorporated as repeatedly and alternately add, and system temperature is controlled at not higher than 80 DEG C while adding oxammonium sulfate and Vanadium Pentoxide in FLAKES.

Further, described temperature of reaction is 100-140 DEG C, and the reaction times is 1.5-3h.

Further, the add-on of described oxammonium sulfate be violanthrone quality 0.2-1.0 doubly.Further preferred, the add-on of described oxammonium sulfate is 0.3-0.4 times of violanthrone quality.

Further, described temperature of reaction is 120-130 DEG C, and the reaction times is 2h.

In technique scheme, the consumption of each component is the optimum feed stock ratio that participates in reaction, but the variation that those skilled in the art can instruction according to the present invention be equal to.For example: be equal to because the parameter that the error of industrial production itself causes changes with technical scheme of the present invention.

The characteristic that the present invention utilizes violanthrone to dissolve in sulfuric acid medium with oxammonium sulfate chemical reaction, makes and in molecular structure, contains the amino violanthrone compound that contains again hydroxyl under the catalysis of Vanadium Pentoxide in FLAKES.It is high that the black dyes making is dying pitch black degree in cotton and BLENDED FABRIC thereof after aftertreatment commercialization, has good dyeing behavior, and not containing carcinogenic aromatic amine, polychlorobiphenyl and the TEXTILE CHEMICALS that bans use of.

Embodiment

For those skilled in the art are known and technical scheme clearly of the present invention more, spy provides preferred embodiment below, but technological thought of the present invention is not limited to following examples.

Embodiment mono-

To the 15ml that adds water in four-hole boiling flask, sulfuric acid (content is 98%) 170ml, stirs 15 minutes; Be cooled to below 80 DEG C, slowly drop into violanthrone dry powder 50g, control temperature in 80 DEG C, be warming up to 100 DEG C after finishing violanthrone dry powder, and in 100-110 DEG C, keep 1 hour; Be cooled to 70 DEG C, alternately add 30g oxammonium sulfate and 0.3g Vanadium Pentoxide in FLAKES for 6 times with being not less than, temperature is controlled in 80 DEG C; Add rear stirring 15 minutes, be slowly warming up to 120-125 DEG C, at this temperature, keep 2h; Keep being cooled to after finishing 60 DEG C and add water and emanate, filter, hot water wash, to neutral, obtains the former dyestuff of black, makes commercial dye through aftertreatment commercialization.

Embodiment bis-

To the 10ml that adds water in four-hole boiling flask, sulfuric acid (content is 98%) 170ml, stirs 15 minutes; Be cooled to below 80 DEG C, slowly drop into violanthrone dry powder 50g, control temperature in 80 DEG C, be warming up to 100 DEG C after finishing violanthrone dry powder, and in 100-110 DEG C, keep 0.5 hour; Be cooled to 70 DEG C, alternately add 50g oxammonium sulfate and 0.15g Vanadium Pentoxide in FLAKES for 6 times with being not less than, temperature is controlled in 80 DEG C; Add rear stirring 15 minutes, be slowly warming up to 130-135 DEG C, at this temperature, keep 1h; Keep being cooled to after finishing 60 DEG C and add water and emanate, filter, hot water wash, to neutral, obtains the former dyestuff of black, makes commercial dye through aftertreatment commercialization.

Embodiment tri-

To the 10ml that adds water in four-hole boiling flask, sulfuric acid (content is 98%) 200ml, stirs 15 minutes; Be cooled to below 80 DEG C, slowly drop into violanthrone dry powder 50g, control temperature in 80 DEG C, be warming up to 100 DEG C after finishing violanthrone dry powder, and in 100-110 DEG C, keep 2 hours; Be cooled to 70 DEG C, alternately add 15g oxammonium sulfate and 0.45g Vanadium Pentoxide in FLAKES for 6 times with being not less than, temperature is controlled in 80 DEG C; Add rear stirring 15 minutes, be slowly warming up to 105-110 DEG C, at this temperature, keep 2.5h; Keep being cooled to after finishing 60 DEG C and add water and emanate, filter, hot water wash, to neutral, obtains the former dyestuff of black, makes commercial dye through aftertreatment commercialization.

Claims

1. a black vat dye, is characterized in that: described dyestuff is prepared as follows:

2. the preparation method of black vat dye according to claim 1, is characterized in that: described solvent is that massfraction is the vitriol oil of 85-105%, and described catalyzer is Vanadium Pentoxide in FLAKES.

3. the preparation method of black vat dye according to claim 2, is characterized in that: described vitriol oil consumption is 4-10 times of violanthrone quality.

4. the preparation method of black vat dye according to claim 2, is characterized in that: the add-on of described Vanadium Pentoxide in FLAKES is 0.001-0.01 times of violanthrone quality.

5. the preparation method of black vat dye according to claim 2, is characterized in that: described reaction raw materials adds sequencing to be: first add the vitriol oil, add violanthrone again, finally add oxammonium sulfate and Vanadium Pentoxide in FLAKES.

6. the preparation method of black vat dye according to claim 5, it is characterized in that: the described vitriol oil and violanthrone add fashionable, system temperature is controlled at not higher than 80 DEG C, after having added violanthrone, temperature is increased to 100-110 DEG C and constant temperature 0.5-2h, and then system is not cooled to and adds oxammonium sulfate and Vanadium Pentoxide in FLAKES again after 70 DEG C.

7. the preparation method of black vat dye according to claim 6, is characterized in that: described oxammonium sulfate and Vanadium Pentoxide in FLAKES are incorporated as repeatedly and alternately add, and system temperature is controlled at not higher than 80 DEG C while adding oxammonium sulfate and Vanadium Pentoxide in FLAKES.

8. according to the preparation method of the black vat dye described in any one in claim 1 to 5, it is characterized in that: described temperature of reaction is 100-140 DEG C, the reaction times is 1.5-3h.

9. according to the preparation method of the black vat dye described in any one in claim 1 to 5, it is characterized in that: the add-on of described oxammonium sulfate is 0.2-1.0 times of violanthrone quality.

10. according to the preparation method of the black vat dye described in any one in claim 1 to 5, it is characterized in that: described temperature of reaction is 120-130 DEG C, the reaction times is 2h.