CN102199363B

CN102199363B - Method for producing disperse blue dye

Info

Publication number: CN102199363B
Application number: CN201110085967A
Authority: CN
Inventors: 王海民; 程燕明; 张毅
Original assignee: JIANGSU YUANZHENG CHEMICAL CO Ltd
Current assignee: JIANGSU YUANZHENG CHEMICAL CO Ltd
Priority date: 2011-04-07
Filing date: 2011-04-07
Publication date: 2012-08-29
Anticipated expiration: 2031-04-07
Also published as: CN102199363A

Abstract

The invention relates to a method for producing disperse blue dye, which is characterized in that: C.I. disperse blue 56 original dye is added into a reaction vessel, dissolved by a proper quantity of DMF, a proper amount of magnesium oxide is added to be used as an acid binding agent, a proper amount of benzoyl chloride is added drop by drop into the reaction vessel under the condition of stirring, heated, after adding is finished, then reacted by isothermally stirring to obtain a reaction product; the reaction product is diluted into a proper amount of icy water, the temperature is maintained less than 15 DEG C, filtered, water is added to filter cake for pulping, the temperature is raised until 55 DEG C to 65 DEG C, the temperature is kept for 2 to 4 hours, then processes of standing overnight, filtering and then washing, drying are performed to obtain disperse blue dye. According to the invention, disperse blue dye solves a technical problem of disperse dyes in transferring printing, the washing fastness, friction fastness and light fastness and the like of the transfer products are obviously improved, disperse blue dye has less sewage and a high utilization rate during the use. The invention provides a rare and novel disperse dye used for transferring printing.

Description

A kind of working method of dispersed blue dye

Technical field

The present invention relates to a kind of working method of dispersed blue dye, especially a kind of working method that is applicable to the improvement property blue disperse dye of cotton, polyester-cotton blend transfer printing.

Background technology

Transfer printing is up-to-date a kind of environmental protection dyeing and printing technology, is described as " green weaving, ecological dyeing and finishing ".It is widely used in the stamp to cut down the consumption of energy, to reduce waste water more and more.But though especially dispersed dye also have much, all there is same shortcoming in the dyestuff that matches, is exactly that dye utilization rate is very low, and the washing fastness, crockfastness, the light fastness that shift product are relatively poor.

Summary of the invention

The objective of the invention is to: provide each item fastness such as a kind of washing fastness, crockfastness, light fastness all be significantly improved, strong to the fabric avidity, production technique is simple, is mainly used in the working method of the blue disperse dye of transfer printing.

Technical problem to be solved by this invention is to realize through following technical scheme.The present invention is a kind of working method of dispersed blue dye, is characterized in:

(1) in reactor, adds the former dyestuff of C.I. Disperse Blue-56, after an amount of DMF dissolving, add an amount of Natural manganese dioxide and make acid binding agent; Under agitation dropwise add in the reactor an amount of Benzoyl chloride 99min.; Be warmed up to 50-80 ℃, added back constant temperature stirring reaction 2-5 hour, get reaction product;

(2) reaction product is diluted in an amount of frozen water, keeps temperature to be no more than 15 ℃, filter, collect filtrating and remove to reclaim DMF; Filter cake is warmed up to 55-65 ℃ after adding the water making beating, is incubated 2-4 hour, and static spending the night filtered after scouring, is drying to obtain dispersed blue dye.

In the working method technical scheme of above-described dispersed blue dye, the mass ratio of former dyestuff of described C.I. Disperse Blue-56 and Benzoyl chloride 99min. is preferably 1:2-4; Former dyestuff of described C.I. Disperse Blue-56 and DMF, magnesian mass ratio are preferably 1:2-5:0.08-0.15.

The present invention uses Benzoyl chloride 99min. that the former dyestuff of C.I. Disperse Blue-56 is carried out modification, and its reaction equation is:

Compared with prior art; The solution of the dispersed blue dye of the inventive method preparation the technical barriers of dispersed dye in transfer printing; Each item fastness such as washing fastness, crockfastness, light fastness that shift product all are significantly improved, and it is few to use sewage, and dye utilization rate is high.It is rare novel dispersed dye that are used for transfer printing.

Embodiment

Below further describe concrete technical scheme of the present invention,, and do not constitute restriction its right so that those skilled in the art understands the present invention further.

Embodiment 1.A kind of working method of dispersed blue dye the steps include:

(1) in reactor, adds the former dyestuff of C.I. Disperse Blue-56, after an amount of DMF dissolving, add an amount of Natural manganese dioxide and make acid binding agent; Under agitation dropwise add in the reactor an amount of Benzoyl chloride 99min.; Be warmed up to 50 ℃, added back constant temperature stirring reaction 2 hours, get reaction product;

(2) reaction product is diluted in an amount of frozen water, keeps temperature to be no more than 15 ℃, filter, collect filtrating and remove to reclaim DMF; Filter cake is warmed up to 55 ℃ after adding the water making beating, is incubated 2 hours, and static spending the night filtered after scouring, is drying to obtain dispersed blue dye.

In the present embodiment, former dyestuff of described C.I. Disperse Blue-56 and Benzoyl chloride 99min., DMF, magnesian mass ratio are 1:2:2:0.08.

Embodiment 2.A kind of working method of dispersed blue dye the steps include:

(1) in reactor, adds the former dyestuff of C.I. Disperse Blue-56, after an amount of DMF dissolving, add an amount of Natural manganese dioxide and make acid binding agent; Under agitation dropwise add in the reactor an amount of Benzoyl chloride 99min.; Be warmed up to 80 ℃, added back constant temperature stirring reaction 5 hours, get reaction product;

(2) reaction product is diluted in an amount of frozen water, keeps temperature to be no more than 15 ℃, filter, collect filtrating and remove to reclaim DMF; Filter cake is warmed up to 65 ℃ after adding the water making beating, is incubated 4 hours, and static spending the night filtered after scouring, is drying to obtain dispersed blue dye.

In the present embodiment, former dyestuff of described C.I. Disperse Blue-56 and Benzoyl chloride 99min., DMF, magnesian mass ratio are 1:4:5:0.15.

Embodiment 3.A kind of working method of dispersed blue dye the steps include:

(1) in reactor, adds the former dyestuff of C.I. Disperse Blue-56, after an amount of DMF dissolving, add an amount of Natural manganese dioxide and make acid binding agent; Under agitation dropwise add in the reactor an amount of Benzoyl chloride 99min.; Be warmed up to 65 ℃, added back constant temperature stirring reaction 3 hours, get reaction product;

(2) reaction product is diluted in an amount of frozen water, keeps temperature to be no more than 15 ℃, filter, collect filtrating and remove to reclaim DMF; Filter cake is warmed up to 60 ℃ after adding the water making beating, is incubated 3 hours, and static spending the night filtered after scouring, is drying to obtain dispersed blue dye.

In the present embodiment, former dyestuff of described C.I. Disperse Blue-56 and Benzoyl chloride 99min., DMF, magnesian mass ratio are 1:3:3:0.10.

Embodiment 4.The preparation experiment one of dispersed blue dye.

In the 1500ml four-hole bottle, add the former dyestuff of 10 gram C.I. Disperse Blue-56s,, and add 0.8 and restrain Natural manganese dioxide and make acid binding agent with 30 gram DMF dissolvings; 28 gram Benzoyl chloride 99min.s are under agitation dropwise added in the reactor, be warmed up to 55 ℃, added back constant temperature stirring reaction 3 hours; Product is stored, for use.

The thickener that reaction is good is diluted in the 45 gram frozen water, keeps temperature to be no more than 15 ℃, filters, and collects filtrating and removes to reclaim DMF; Filter cake adds water making beating 1 hour, is warmed up to 60 ℃, is incubated 3 hours, and after scouring is filtered in static filtration, bakes 2 hours, and the solid pure dyestuff that obtains is handled through commercialization, promptly gets modification dyestuff (1).

Embodiment 5.The preparation experiment two of dispersed blue dye.

In the 250ml four-hole bottle, add the former dyestuff of 1.5 gram C.I. Disperse Blue-56s,, and add 0.15 and restrain Natural manganese dioxide and make acid binding agent with 5 gram DMF dissolvings; 5 gram Benzoyl chloride 99min.s are under agitation dropwise added in the reactor, be warmed up to 70 ℃, added back constant temperature stirring reaction 3 hours; Product is stored, for use.

The thickener that reaction is good is diluted in the 7.5 gram frozen water, keeps temperature to be no more than 15 ℃, filters, and collects filtrating and removes to reclaim DMF.Filter cake adds water making beating 1 hour, is warmed up to 60 ℃, is incubated 3 hours, and after scouring is filtered in static filtration, bakes 2 hours, and the solid pure dyestuff that obtains is handled through commercialization, promptly gets modification dyestuff (2).

Embodiment 6.The preparation experiment three of dispersed blue dye.

In the 3000ml enamel still, add the former dyestuff of 20 gram C.I. Disperse Blue-56s,, and add 2 and restrain Natural manganese dioxide and make acid binding agent with 50 gram DMF dissolvings; 56 gram Benzoyl chloride 99min.s are under agitation dropwise added in the reactor, be warmed up to 70 ℃, added back constant temperature stirring reaction 3 hours; Product is stored, for use.

The thickener that reaction is good is diluted in the 90 gram frozen water, keeps temperature to be no more than 15 ℃, filters, and collects filtrating and removes to reclaim DMF.Filter cake adds water making beating 1 hour, is warmed up to 60 ℃, is incubated 3 hours, and after scouring is filtered in static filtration, oven dry, and the solid pure dyestuff that obtains is handled through commercialization, promptly gets modification dyestuff (3).

Embodiment 7.The preparation experiment four of dispersed blue dye.

In the 1000ml reaction kettle, add 8 gram C.I. Disperse Blue-56s,, and add 0.8 and restrain Natural manganese dioxide and make acid binding agent with 20 gram DMF dissolvings; 18 gram Benzoyl chloride 99min.s are under agitation dropwise added in the reactor, be warmed up to 75 ℃, added back constant temperature stirring reaction 3 hours; Product is stored, for use.

The thickener that reaction is good is diluted in the 30 gram frozen water, keeps temperature to be no more than 15 ℃, filters, and collects filtrating and removes to reclaim DMF.Filter cake adds water making beating 1 hour, is warmed up to 60 ℃, is incubated 3 hours, and after scouring is filtered in static filtration, bakes 2 hours, and the solid pure dyestuff that obtains is handled through commercialization, promptly gets modification dyestuff (4).

It is after former dyestuff, auxiliary agent and water are mixed according to a certain percentage that the commercialization of the described dyestuff of last embodiment is handled, through traditional sand milling technology, and resulting aqueous commodity, or the powdery commodity of spray-dried gained again.Dispersion agent, diffusant and the tensio-active agent thereof etc. used always when described auxiliary agent is the dispersed dye commercialization.Preferably include one of following or its mixture: naphthalene sulfonic acidformaldehyde condensation product, sulfonated lignin, alkyl naphthalene sulfonic acid formaldehyde condensation products.Like condensation compound of methyl naphthalene sulfonic acid and formaldehyde (Dispersant MF), naphthalene sulfonic acidformaldehyde condensation product (dispersing agent NNO), benzyl naphthalene sulfonic formaldehyde condensation compound (dispersing agent CNF), sodium lignosulfonate (xylogen 85A, 83A) etc.Usually, auxiliary agent is 1.5 ~ 6:1 with the ratio of former dyestuff weight.

Modification dyestuff (1), (2), (3) and (4) of the foregoing description 4-7 gained are respectively applied for the transfer printing experiment, and the technical process of described transfer printing experiment is following:

1, the pre-treatment of polyester-cotton blend stamp grey cloth: the stamp grey cloth immersed soak two through two in the bridging agent that bath raio is 1:50 and roll (pick-up is 10%), then in 90 ℃ of dry finishings.

2, hot transfer paper preparation: with acetone soln dyestuff is dissolved in the small beaker, adds tackiness agent and thinner successively, stir, make it into ink-like, evenly be applied to dyestuff on the paper with scraper again, dry.

3, printing technology: pretreated cotton, polyester-cotton fabric are pasted with the transfer paper front mutually, carry out hot transfer printing at 180 ℃～190 ℃, the time is 30 seconds.

PRINTED FABRIC A, B, C, D that the modification dyestuff (1) of the foregoing description 4-7 gained, (2), (3) and (4) are obtained through the technical process of transfer printing; Comparative Examples is for using unmodified C.I. Disperse Blue-56 commercialization dyestuff; The PRINTED FABRIC E that obtains through the technical process of transfer printing; Adopt international standards GB/T3921-1997, GB/T3920-1997, GB/T8427-1998 surveys its washing fastness, fastness to rubbing, light fastness respectively, sees the following form:

PRINTED FABRIC	Washing fastness	Fastness to rubbing	Light fastness
				A	5	5	7-8
B	5	5	7-8
				C	5	5	7-8
D	5	5	7-8
				E	3	3	5

Claims

1. the working method of a dispersed blue dye is characterized in that:

2. the working method of dispersed blue dye according to claim 1, it is characterized in that: the mass ratio of former dyestuff of C.I. Disperse Blue-56 and Benzoyl chloride 99min. is 1:2-4.

3. the working method of dispersed blue dye according to claim 1, it is characterized in that: former dyestuff of C.I. Disperse Blue-56 and DMF, magnesian mass ratio are 1:2-5:0.08-0.15.