Mar . 20, 2024 09:28 Back to list

A kind of preparation method of bromindigo dyestuff

Bromindigo is a kind of high-grade vat dyes.The stamp and the dyeing that are mainly used in cotton, fiber crops, hair, silk, close fibre and composition thereof, colorant match power is good.In prior art, multiplex 98% sulfuric acid of bromindigo manufacturer, oleum are made reaction medium, after having reacted, with a large amount of spent acid of frozen water dilution generation, cannot recovery, bring very large pressure to environmental protection, and the bromindigo dye product coloured light of producing by this kind of method is green dark, can make the dyestuff after later stage colorant match also be faint in color.For another example US Patent No. 5380871 adopts sulfur oxychloride to make reaction medium, after having reacted, produces a large amount of spent acid equally pollute with frozen water dilution.

Summary of the invention

The object of the present invention is to provide the preparation method of a kind of technique bromindigo dyestuff simple, with short production cycle, more environmental protection.

For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of bromindigo dyestuff, is characterized in that: by the indigo oil of mirbane that is dissolved in, add bromizating agent, after reacting by heating 4-15h, with after organic solvent washing, filter to obtain filter cake, filter cake is with being drying to obtain product after hot wash.Reacting by heating the best is 8-10h.

Further preferred, described bromizating agent is bromine.The bromination effect of bromine is best, can certainly be other bromizating agent, as cupric bromide, N-bromo-succinimide, bromination dimethyl bromo sulphur, Sodium Bromide, Potassium Bromide, brometo de amonio, bromine chloride etc.

Further, the 8-18 that described oil of mirbane consumption is indigo quality doubly.

Further, the 11-14 that described oil of mirbane consumption is indigo quality doubly.

Further, the organic solvent of described washing use is methyl alcohol.

Further, described bromine is added dropwise in indigo oil of mirbane mixing solutions in 3-4h, and the mixed solution system described in dropping process is in 50 ± 2 DEG C of constant temperature.Namely bromine slowly evenly splashes in mixing solutions in 3-4h, instead of disposable adding, and this is in order to make reaction more steady and thorough.

Further, described bromine and indigo mol ratio are 4-6:1.

indigo blue vat blue

Further, described bromine and indigo mol ratio are 5.2-5.6:1.

Further, described heating steps temperature is 80-150 DEG C.

Further, described reacting by heating step temperature is 120-130 DEG C.

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.

Technique of the present invention be taking oil of mirbane as solvent, bromine is halogenating agent, under heating condition, prepares bromindigo.Compared with prior art, can not use the acids such as the vitriol oil, oleum or sulfur oxychloride in whole reaction process, can not cause the pollution of spent acid, oil of mirbane can repeat to apply mechanically and can Distillation recovery.The bromindigo dye product of preparing by the inventive method and existing standard ratio, intensity improves 10%, and coloured light is red gorgeous, and its printing fastness excellence can say that the inventive method is the method for a kind of more low-carbon environment-friendly of bromindigo dyestuffs industriesization production.

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-

1, in enamel reaction still, add the dry indigo pure powder of 20kg and 240kg oil of mirbane, stir well.

2,66kg bromine is slowly added drop-wise in indigo nitrobenzene solution with 3h under 50 ± 2 DEG C of temperature condition.

3, drip and be slowly warmed up to 120 DEG C afterwards, insulated and stirred 10h, then be cooled to below 60 DEG C.

4, add methyl alcohol diluted material, filter, wash several times with methyl alcohol, drain filter cake.Filtrate is reclaimed, and reclaims respectively methyl alcohol and oil of mirbane through distillation, repeats to be back to next batch.

indigo blue vat blue

5, to obtain former dyestuff with 80 DEG C of left and right hot water washing filter cakes to neutral, dry again, 110 points of intensity, coloured light is red gorgeous.

Embodiment bis-

1, in enamel reaction still, add the dry indigo pure powder of 20kg and 300kg oil of mirbane, stir well.

2,50kg bromine is slowly added drop-wise in indigo nitrobenzene solution with 3.5h under 50 ± 2 DEG C of temperature condition.

3, drip and be slowly warmed up to 90 DEG C afterwards, insulated and stirred 12h, then be cooled to below 60 DEG C.

5, to obtain former dyestuff with 80 DEG C of left and right hot water washing filter cakes to neutral, dry again, 110 points of intensity, coloured light is red gorgeous.

Embodiment tri-

1, in enamel reaction still, add the dry indigo pure powder of 20kg and 200kg oil of mirbane, stir well.

2,72kg bromine is slowly added drop-wise in indigo nitrobenzene solution with 4h under 50 ± 2 DEG C of temperature condition.

3, drip and be slowly warmed up to 140 DEG C afterwards, insulated and stirred 6h, then be cooled to below 60 DEG C.

5, to obtain former dyestuff with 80 DEG C of left and right hot water washing filter cakes to neutral, dry again, 110 points of intensity, coloured light is red gorgeous.

Claims (10)

Hide Dependent

1. a preparation method for bromindigo dyestuff, is characterized in that: by the indigo oil of mirbane that is dissolved in, add bromizating agent, after reacting by heating 4-15h, with after organic solvent washing, filter to obtain filter cake, filter cake is with being drying to obtain product after hot wash.

2. the preparation method of bromindigo dyestuff according to claim 1, is characterized in that: described bromizating agent is bromine.

3. the preparation method of bromindigo dyestuff according to claim 1 and 2, is characterized in that: the 8-18 that described oil of mirbane consumption is indigo quality doubly.

4. the preparation method of bromindigo dyestuff according to claim 1 and 2, is characterized in that: the 11-14 that described oil of mirbane consumption is indigo quality doubly.

5. the preparation method of bromindigo dyestuff according to claim 1 and 2, is characterized in that: the organic solvent of described washing use is methyl alcohol.

6. the preparation method of bromindigo dyestuff according to claim 2, is characterized in that: described bromine is added dropwise in indigo oil of mirbane mixing solutions in 3-4h, and the mixed solution system described in dropping process is in 50 ± 2 DEG C of constant temperature.

7. the preparation method of bromindigo dyestuff according to claim 2, is characterized in that: described bromine and indigo mol ratio are 4-6:1.

8. the preparation method of bromindigo dyestuff according to claim 2, is characterized in that: described bromine and indigo mol ratio are 5.2-5.6:1.

9. the preparation method of bromindigo dyestuff according to claim 5, is characterized in that: described heating steps temperature is 80-150 DEG C.

10. the preparation method of bromindigo dyestuff according to claim 6, is characterized in that: described reacting by heating step temperature is 120-130 DEG C.

a preparation method for bromindigo dyestuff

6,6'-Dibromoindigo