CN104478770A - Black reactive dye semi-finished product and preparation method and application thereof - Google Patents

Black reactive dye semi-finished product and preparation method and application thereof Download PDF

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Publication number
CN104478770A
CN104478770A CN201410752312.8A CN201410752312A CN104478770A CN 104478770 A CN104478770 A CN 104478770A CN 201410752312 A CN201410752312 A CN 201410752312A CN 104478770 A CN104478770 A CN 104478770A
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China
Prior art keywords
mixing solutions
so3x
coox
black dye
sodium nitrite
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Inventor
陆海英
庄胜峰
陆再宏
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WUJIANG TAOYUAN DYE CO Ltd
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WUJIANG TAOYUAN DYE CO Ltd
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Abstract

The invention relates to a black reactive dye semi-finished product and a preparation method and application thereof. The chemical structural general formula of the semi-finished product is shown in a formula (I), and the structural formula is as shown in the specification, wherein R1 refers to -CH3(CH2)n, -CH3(CH2)n O, -COOX or -SO3X; R2 refers to -H, -CH3(CH2)n, -CH3(CH2)n O, -COOX or -SO3X; R3 refers to -H, -CH3(CH2)n, -CH3(CH2)n O, -COOX or -SO3X; R4 refers to -H, -CH3(CH2)n, -CH3(CH2)n O, -COOX or -SO3X; R5 refers to -(CH2)<n+1>-; and X can be Na, K or Li. On one hand, the black reactive dye semi-finished product has a bisazo structure, and the fixation rate and deep dyeing property of the product can be improved; on the other hand, the black reactive dye semi-finished product comprises multiple sulfonated groups, can achieve the effects similar to a surfactant, is conveniently compound and mixed with other organic matters and is dissolved in water to prepare a dye solution.

Description

A kind of active black dye work in-process, preparation method and application thereof
Technical field
The invention belongs to organic dye field, relate to a kind of dyestuff work in-process, be specifically related to a kind of active black dye work in-process, preparation method and application thereof.
Background technology
Reactive dyestuffs, also known as chemically-reactive dyes, for when dyeing and the dye of fiber react with.In this kind of dye molecule containing can with the group of fiber generation chemical reaction, during dyeing, dyestuff and fiber-reactive, form covalent linkage therebetween, becomes overall, and washable and fastness to rubbing is improved.
Application number be 201110294102.5 Chinese invention patent disclose a kind of reactive black dye mixture, comprise the reactive black dye of 65% ~ 50%, the active orange dye of 35% ~ 20% and 20 ~ 10% auxiliary agent.Although the dye mixture of this invention has very high dye yield on fiber, and the color part that do not obtain of fiber very easily cleans again; But it has three kinds of compositions, and need used additives is coordinated, not only add the cost of dyestuff, and auxiliary agent is common anion surfactant, easily in dyeing course, produces more foam, add the difficulty that cloth is clean.Therefore, synthesize a kind of active black dye work in-process, for the preparation of active black dye, and the component that as far as possible can reduce black dyes just seems particularly necessary.
Summary of the invention
The present invention seeks to provide a kind of environment-friendly type active black dye work in-process to overcome the deficiencies in the prior art.
For achieving the above object, the technical solution used in the present invention is: a kind of active black dye work in-process, and its chemical structure of general formula is such as formula shown in (Ι):
（Ι），
In formula, R 1for-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 2for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 3for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 4for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 5for-(CH2) n+1-;
X is from Na, K or Li;
Wherein n is integer and 0≤n≤3.
Optimally, R 1for-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 3for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX.
Optimally, R 2for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 4for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX.
Optimally, its chemical structural formula is such as formula shown in (Ι-1):
（Ι-1），
In formula, X is from Na, K or Li.
Another object of the present invention is to provide the half-finished preparation method of a kind of above-mentioned active black dye, and it comprises the following steps:
A () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and obtain the first mixing solutions in 1 ~ 3 hour after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1;
B temperature that () controls described first mixing solutions controls to be 5 ~ 8 DEG C, and adds wherein react 2 ~ 4 hours to obtain the second mixing solutions; Described with described mol ratio be 1:0.95 ~ 0.98;
C () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and within 1 ~ 3 hour, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1, described in with described mol ratio be 1:0.95 ~ 1.05;
D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph to 5.5 ~ 6, and reacts 1 ~ 3 hour to obtain the 4th mixing solutions at being placed in 10 ~ 15 DEG C;
E () regulates described 4th mixing solutions pH value to 5.5 ~ 6, add gac reaction wherein and filter after 20 ~ 60 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 2 ~ 5%.
Optimally, step (a) is with in step (c), and the feed postition of described hydrochloric acid, described Sodium Nitrite is for dripping, and rate of addition is 0.5 ~ 2.5kg/ hour.
Optimally, in described step (a) and step (c), control solution ph and make aobvious blue, the micro-blueness of starch potassium iodide paper of congo-red test paper, when starch potassium iodide paper colour developing is deepened, add a certain amount of described in or ; If when starch potassium iodide paper shows colourless, add a certain amount of described sodium nitrite solution.
Further, step (a), with in step (c), when described starch potassium iodide paper shows colourless, is added at a certain amount of described sodium nitrite solution is placed on 5 ~ 8 DEG C and is reacted 1 ~ 2 hour, eliminate excessive nitrous acid with a certain amount of thionamic acid.
Another object of the present invention is to provide the half-finished application of a kind of above-mentioned active black dye, for preparing active black dye.
Optimally, above-mentioned active black dye also comprises second half finished product A, and described active black dye work in-process and described half-finished mass ratio are 75 ~ 85:12 ~ 25, and the chemical structural formula of described work in-process A is
。
Because technique scheme is used, the present invention compared with prior art has following advantages: active black dye work in-process of the present invention, and its chemical structure of general formula is such as formula shown in (Ι):
（Ι），
In formula, R 1for-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X; R 2for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X; R 3for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X; R 4for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X; R 5for-(CH2) n+1-; X is from Na, K or Li; These black dyes work in-process have tetrazo structure on the one hand, can improve its degree of fixation and depth; It has multiple sulfonation group on the other hand, can play the effect being similar to tensio-active agent, conveniently carries out composite mixing with other organism, makes dye solution after water-soluble.
Embodiment
Active black dye work in-process of the present invention, its chemical structure of general formula is such as formula shown in (Ι):
（Ι），
In formula, R 1for-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 2for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 3for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 4for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 5for-(CH2) n+1-;
X is from Na, K or Li;
Wherein n is integer and 0≤n≤3; These active black dye work in-process have tetrazo structure on the one hand, can improve its degree of fixation and depth; It has multiple sulfonation group on the other hand, can play the effect being similar to tensio-active agent, conveniently carries out composite mixing with other organism, makes dye solution after water-soluble.
R in formula 1be preferably-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 3be preferably-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 2be preferably-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 4be preferably-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX.The half-finished chemical structural formula of black dyes is preferably such as formula shown in (Ι-1):
（Ι-1），
In formula, X is from Na, K or Li.
In order to prepare above-mentioned active black dye work in-process, it comprises the following steps:
A () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and obtain the first mixing solutions in 1 ~ 3 hour after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1; B temperature that () controls described first mixing solutions controls to be 5 ~ 8 DEG C, and adds wherein react 2 ~ 4 hours to obtain the second mixing solutions; Described with described mol ratio be 1:0.95 ~ 0.98; C () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and within 1 ~ 3 hour, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1, described in with described mol ratio be 1:0.95 ~ 1.05; D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph to 5.5 ~ 6, and reacts 1 ~ 3 hour to obtain the 4th mixing solutions at being placed in 10 ~ 15 DEG C; E () regulates described 4th mixing solutions pH value to 5.5 ~ 6, add gac reaction wherein and filter after 20 ~ 60 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 2 ~ 5%.; The method reaction conditions is simple, does not need the reaction conditionss such as protection of inert gas, high temperature, vacuum, high pressure, is conducive to its scale operation; And take filtrate after reaction, filter residue can directly be collected, and filtrate only needs drying, and side reaction degree is little, pollutes little, is conducive to protection of the environment.
Step (a) is with in step (c), and the feed postition of described hydrochloric acid, described Sodium Nitrite is for dripping, and rate of addition is preferably 0.5 ~ 2.5kg/ hour; And need to control solution ph and make that congo-red test paper is aobvious blue, the micro-blueness of starch potassium iodide paper, when starch potassium iodide paper colour developing is deepened, add a certain amount of described in or ; If when starch potassium iodide paper shows colourless, add a certain amount of described sodium nitrite solution, , or the additional amount of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined.When starch potassium iodide paper shows colourless, add at a certain amount of described sodium nitrite solution is placed on 5 ~ 8 DEG C and react 1 ~ 2 hour, eliminate excessive nitrous acid with a certain amount of thionamic acid.
Above-mentioned active black dye work in-process can be re-dubbed active black dye with work in-process A, and for the dyeing of various cloth, the mass ratio of active black dye work in-process and work in-process A is 75 ~ 85:12 ~ 25, and wherein the chemical structural formula of work in-process A is
。
Below will the present invention is described in detail by specific embodiment.
Embodiment 1
The present embodiment provides a kind of active black dye work in-process, and its chemical structural formula is shown below:
；
The half-finished preparation method of above-mentioned active black dye, comprises the following steps:
A () will be added to the water dissolving, adds ice cube wherein and keep temperature to be 0 DEG C, add sodium nitrite solution and react and obtain the first mixing solutions in 3 hours after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5:1; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is 0.5kg/ hour; And need to control solution ph and make aobvious blue, the micro-blueness of starch potassium iodide paper of congo-red test paper, when starch potassium iodide paper colour developing is deepened, add appropriate ; If when starch potassium iodide paper shows colourless, add appropriate sodium nitrite solution, or the additional amount of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined.When starch potassium iodide paper shows colourless, add at sodium nitrite solution is placed on 5 DEG C and react 2 hours, eliminate excessive nitrous acid with a certain amount of thionamic acid;
B temperature that () controls described first mixing solutions controls to be 5 DEG C, and adds wherein react 4 hours to obtain the second mixing solutions; with mol ratio be 1:0.95;
C () will be added to the water dissolving, adds ice cube wherein and keep temperature to be 0 DEG C, add sodium nitrite solution and react and within 3 hours, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5:1, described in with described mol ratio be 1:0.95; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is preferably 0.5kg/ hour; And need to control solution ph and make that congo-red test paper is aobvious blue, the micro-blueness of starch potassium iodide paper, when starch potassium iodide paper colour developing is deepened, add a certain amount of described in ; If when starch potassium iodide paper shows colourless, add a certain amount of sodium nitrite solution, or the not dosage of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined; When starch potassium iodide paper shows colourless, add at a certain amount of sodium nitrite solution is placed on 5 DEG C and react 2 hours, eliminate excessive nitrous acid with a certain amount of thionamic acid;
D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph uses sodium bicarbonate to regulate pH to 5.5(), and react 3 hours to obtain the 4th mixing solutions at being placed in 10 DEG C;
E () regulates described 4th mixing solutions pH value to 5.5, add gac wherein and react filtration after 20 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 2%.
Embodiment 2
The present embodiment provides a kind of active black dye, and it comprises active black dye work in-process in embodiment 1 and work in-process A, wherein, active black dye work in-process in embodiment 1 account for 75wt%(massfraction), work in-process A accounts for 25 wt%, and wherein, the chemical structural formula of work in-process A is
。
Embodiment 3
The present embodiment provides a kind of active black dye, and it is identical with the active black dye moiety in embodiment 2, different unlike its massfraction, wherein
account for 85wt%, account for 15wt%.
Embodiment 4
The present embodiment provides a kind of active black dye, and it is identical with the active black dye moiety in embodiment 2, different unlike its massfraction, wherein
account for 80wt%, account for 20wt%.
Embodiment 5
The present embodiment provides the half-finished preparation method of active black dye in a kind of embodiment 1, comprises the following steps:
A () will be added to the water dissolving, keeps temperature to be 5 DEG C, adds sodium nitrite solution and react and obtain the first mixing solutions in 1 hour after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.7:1.1; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is 2.5kg/ hour; And need to control solution ph and make aobvious blue, the micro-blueness of starch potassium iodide paper of congo-red test paper, when starch potassium iodide paper colour developing is deepened, add appropriate ; If when starch potassium iodide paper shows colourless, add appropriate sodium nitrite solution, or the additional amount of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined.When starch potassium iodide paper shows colourless, add at sodium nitrite solution is placed on 8 DEG C and react 1 hour, eliminate excessive nitrous acid with a certain amount of thionamic acid;
B temperature that () controls described first mixing solutions controls to be 8 DEG C, and adds wherein react 2 hours to obtain the second mixing solutions; with mol ratio be 1:0.98;
C () will be added to the water dissolving, keeps temperature to be 5 DEG C, adds sodium nitrite solution and react and within 1 hour, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.7:1.1, described in with described mol ratio be 1:1.05; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is preferably 2.5kg/ hour; And need to control solution ph and make that congo-red test paper is aobvious blue, the micro-blueness of starch potassium iodide paper, when starch potassium iodide paper colour developing is deepened, add a certain amount of described in ; If when starch potassium iodide paper shows colourless, add a certain amount of sodium nitrite solution, or the not dosage of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined; When starch potassium iodide paper shows colourless, add at a certain amount of sodium nitrite solution is placed on 8 DEG C and react 1 hour, eliminate excessive nitrous acid with a certain amount of thionamic acid;
D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph to 6, and reacts 1 hour to obtain the 4th mixing solutions at being placed in 15 DEG C;
E () regulates described 4th mixing solutions pH value to 6, add gac wherein and react filtration after 60 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 5%.
Embodiment 6
The present embodiment provides the half-finished preparation method of active black dye in a kind of embodiment 1, comprises the following steps:
A () will be added to the water dissolving, keeps temperature to be 3 DEG C, adds sodium nitrite solution and react and obtain the first mixing solutions in 2 hours after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.6:1.05; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is 2kg/ hour; And need to control solution ph and make aobvious blue, the micro-blueness of starch potassium iodide paper of congo-red test paper, when starch potassium iodide paper colour developing is deepened, add appropriate ; If when starch potassium iodide paper shows colourless, add appropriate sodium nitrite solution, or the additional amount of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined.When starch potassium iodide paper shows colourless, add at sodium nitrite solution is placed on 6 DEG C and react 1.5 hours, eliminate excessive nitrous acid with a certain amount of thionamic acid;
B temperature that () controls described first mixing solutions controls to be 6 DEG C, and adds wherein react 3 hours to obtain the second mixing solutions; with mol ratio be 1:0.96;
C () will be added to the water dissolving, keeps temperature to be 3 DEG C, adds sodium nitrite solution and react and within 2 hours, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.6:1.05, described in with described mol ratio be 1:1; The feed postition of hydrochloric acid, Sodium Nitrite is for dripping, and rate of addition is preferably 2kg/ hour; And need to control solution ph and make that congo-red test paper is aobvious blue, the micro-blueness of starch potassium iodide paper, when starch potassium iodide paper colour developing is deepened, add a certain amount of described in ; If when starch potassium iodide paper shows colourless, add a certain amount of sodium nitrite solution, or the not dosage of Sodium Nitrite all shows blueness by congo-red test paper, the colour-change of starch potassium iodide paper is determined; When starch potassium iodide paper shows colourless, add at a certain amount of sodium nitrite solution is placed on 6 DEG C and react 1.5 hours, eliminate excessive nitrous acid with a certain amount of thionamic acid;
D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph to 5.8, and reacts 2 hours to obtain the 4th mixing solutions at being placed in 12 DEG C;
E () regulates described 4th mixing solutions pH value to 5.8, add gac wherein and react filtration after 40 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 3%.
Embodiment 7
The present embodiment provides a kind of active black dye work in-process, and its chemical structural formula is shown below:
（Ι），
In formula, R 1for-CH3CH2, R 2for-CH3CH2, R 3for-CH3CH2, R 4for-CH3CH2, R 5for-(CH2) 2-; X is K.
Embodiment 8
The present embodiment provides a kind of active black dye work in-process, and its chemical structural formula is shown below:
（Ι），
In formula, R 1for-CH3 (CH2) 3, R 2for-CH3 (CH2) 3O, R 3for-COOLi, R 4for-SO3Li, R 5for-(CH2) 4-; X is Li.
Embodiment 9
The present embodiment provides a kind of active black dye work in-process, and its chemical structural formula is shown below:
（Ι），
In formula, R 1for-CH3, R 2for-CH3O, R 3for-SO3Na, R 4for-H, R 5for-(CH2) 2-; X is Na.
Above-described embodiment is only for illustrating technical conceive of the present invention and feature; its object is to person skilled in the art can be understood content of the present invention and implement according to this; can not limit the scope of the invention with this; all equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.

Claims (10)

1. active black dye work in-process, is characterized in that, its chemical structure of general formula is such as formula shown in (Ι):
（Ι），
In formula, R 1for-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 2for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 3for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 4for-H ,-CH3 (CH2) n ,-CH3 (CH2) n O ,-COOX or-SO3X;
R 5for-(CH2) n+1-;
X is Na, K or Li;
Wherein n is integer and 0≤n≤3.
2. active black dye work in-process according to claim 1, is characterized in that: R 1for-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 3for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX.
3. active black dye work in-process according to claim 1, is characterized in that: R 2for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX; R 4for-H ,-SO3X ,-CH3CH2 ,-CH3CH2O or-COOX.
4. active black dye work in-process according to claim 1, is characterized in that: its chemical structural formula is such as formula shown in (Ι-1):
（Ι-1），
In formula, X is from Na, K or Li.
5. the half-finished preparation method of arbitrary described active black dye in Claims 1-4, it is characterized in that, it comprises the following steps:
A () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and obtain the first mixing solutions in 1 ~ 3 hour after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1;
B temperature that () controls described first mixing solutions controls to be 5 ~ 8 DEG C, and adds wherein react 2 ~ 4 hours to obtain the second mixing solutions; Described with described mol ratio be 1:0.95 ~ 0.98;
C () will be added to the water dissolving, keeps temperature to be 0 ~ 5 DEG C, adds sodium nitrite solution reaction and within 1 ~ 3 hour, obtain the 3rd mixing solutions after adding hydrochloric acid soln, described in , described hydrochloric acid and described Sodium Nitrite mol ratio be 1:0.5 ~ 0.7:1 ~ 1.1, described in with described mol ratio be 1:0.95 ~ 1.05;
D described 3rd mixing solutions adds in described second mixing solutions by (), adjust ph to 5.5 ~ 6, and reacts 1 ~ 3 hour to obtain the 4th mixing solutions at being placed in 10 ~ 15 DEG C;
E () regulates described 4th mixing solutions pH value to 5.5 ~ 6, add gac reaction wherein and filter after 20 ~ 60 minutes, get filtrate drying, the volume ratio of described gac and described 4th mixing solutions is 2 ~ 5%.
6. the half-finished preparation method of active black dye according to claim 5, is characterized in that: in step (a) and step (c), the feed postition of described hydrochloric acid, described Sodium Nitrite is for dripping, and rate of addition is 0.5 ~ 2.5kg/ hour.
7. the half-finished preparation method of active black dye according to claim 5, it is characterized in that: described step (a) is with in step (c), control solution ph and make aobvious blue, the micro-blueness of starch potassium iodide paper of congo-red test paper, when starch potassium iodide paper colour developing deepen time, add a certain amount of described in or ; If when starch potassium iodide paper shows colourless, add a certain amount of described sodium nitrite solution.
8. the preparation method of the active red disazo dye of environment-friendly type according to claim 7, it is characterized in that: step (a) is with in step (c), when described starch potassium iodide paper shows colourless, add at a certain amount of described sodium nitrite solution is placed on 5 ~ 8 DEG C and react 1 ~ 2 hour, eliminate excessive nitrous acid with a certain amount of thionamic acid.
9. an active black dye, is characterized in that: it comprises arbitrary described active black dye work in-process in Claims 1-4.
10. active black dye according to claim 9, it is characterized in that: it also comprises second half finished product A, the mass ratio of described active black dye work in-process and described work in-process A is 75 ~ 85:12 ~ 25, and the chemical structural formula of described work in-process A is
。
CN201410752312.8A 2014-12-11 2014-12-11 Black reactive dye semi-finished product and preparation method and application thereof Pending CN104478770A (en)

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