CN102964870A - Active black dye composition - Google Patents
Active black dye composition Download PDFInfo
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- CN102964870A CN102964870A CN2012104166064A CN201210416606A CN102964870A CN 102964870 A CN102964870 A CN 102964870A CN 2012104166064 A CN2012104166064 A CN 2012104166064A CN 201210416606 A CN201210416606 A CN 201210416606A CN 102964870 A CN102964870 A CN 102964870A
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- formula
- black dye
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- percentage composition
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- 239000000203 mixture Substances 0.000 title claims abstract description 88
- 229910052739 hydrogen Inorganic materials 0.000 claims description 11
- 229910052783 alkali metal Inorganic materials 0.000 claims description 9
- 150000001340 alkali metals Chemical group 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 6
- 238000004043 dyeing Methods 0.000 abstract description 24
- 238000005406 washing Methods 0.000 abstract description 6
- 238000007639 printing Methods 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 3
- 230000015784 hyperosmotic salinity response Effects 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 90
- 239000004744 fabric Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000835 fiber Substances 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 0 Cc(c(*)c1)cc(N=Nc(c(S(O)(=O)=O)cc(c2ccc3NC)c3N=N[C@@]3C=CC(*=C)=CC3S(O)(=O)=O)c2O)c1OC Chemical compound Cc(c(*)c1)cc(N=Nc(c(S(O)(=O)=O)cc(c2ccc3NC)c3N=N[C@@]3C=CC(*=C)=CC3S(O)(=O)=O)c2O)c1OC 0.000 description 7
- 229920000742 Cotton Polymers 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 239000003513 alkali Substances 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000009980 pad dyeing Methods 0.000 description 4
- 239000000344 soap Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229940056729 sodium sulfate anhydrous Drugs 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- -1 alkali metal salt Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000985 reactive dye Substances 0.000 description 2
- 238000010186 staining Methods 0.000 description 2
- 210000004243 sweat Anatomy 0.000 description 2
- WODGMMJHSAKKNF-UHFFFAOYSA-N 2-methylnaphthalene-1-sulfonic acid Chemical compound C1=CC=CC2=C(S(O)(=O)=O)C(C)=CC=C21 WODGMMJHSAKKNF-UHFFFAOYSA-N 0.000 description 1
- SRDOTWUOTQTGAK-UHFFFAOYSA-N C=O.C1(=CC=CC2=CC=CC=C12)S(=O)(=O)OCC1=CC=CC=C1 Chemical compound C=O.C1(=CC=CC2=CC=CC=C12)S(=O)(=O)OCC1=CC=CC=C1 SRDOTWUOTQTGAK-UHFFFAOYSA-N 0.000 description 1
- QLMGMYFMJRCJNA-UHFFFAOYSA-N CC1C2[IH]C2CC1 Chemical compound CC1C2[IH]C2CC1 QLMGMYFMJRCJNA-UHFFFAOYSA-N 0.000 description 1
- 229920002292 Nylon 6 Polymers 0.000 description 1
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- DPDMMXDBJGCCQC-UHFFFAOYSA-N [Na].[Cl] Chemical compound [Na].[Cl] DPDMMXDBJGCCQC-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052728 basic metal Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000007859 condensation product Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000010016 exhaust dyeing Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 239000012943 hotmelt Substances 0.000 description 1
- 238000010409 ironing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 235000015598 salt intake Nutrition 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000007447 staining method Methods 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Coloring (AREA)
Abstract
The invention provides an active black dye composition, which comprises 45-90 weight parts of at least a component shown as a formula (I), 1-30 weight parts of at least a component B shown as a formula (II), and 1-40 weight parts of at least as a component C shown as a formula (III) and / or 1-40 weight parts of at least a component D shown as a formula (IV). The reactive black dye composition provided by the invention can be used for textile printing and dyeing, has advantages of good promotion performance, strong salt tolerance, easiness for washing and excellent wet-processing fastness, and is a rare economical black dye.
Description
(1) technical field
The present invention relates to a kind of reactive dye compositions, particularly excellent, the easy washing of a kind of lifting force, the active black dye composition that dyeing behavior is stable.
(2) background technology
In cotton fiber dyeing, black almost accounts for 40 ~ 50%, and the more substantive dyestuff of usefulness and thioxine dyes are forbidden and limit use owing to environmental issue.Reactive black KN-B since cheap, fastness well, higher degree of fixation and easy detergency, and do not have the environmental issue that comprises AOX, so a large usage quantity.But also exist the defectives such as lifting force is poor, pitch black degree is inadequate simultaneously, thereby limited being widely used of it.
Existing reactive black dye colorant match product exists still in actual application that depth is strong, dye uptake and degree of fixation is not high, the DYED FABRICS problem such as easy cleaning not, such as patent CN102245712, CN1730566 etc.This is because the used dye strength of deep color dyeing is high, the loose colour amount of dye increases, and fiber has a saturation value to the absorption of dyestuff, dye strength generally should not surpass 10% of dyeing saturation value, excessive dyestuff can not on dye and set, can pile up at fabric face, if easy cleaning is bad, certainly will affect the wet colour fastness of dyeing and weaving thing, thereby cause dyeing behavior not good enough.
(3) summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of active black dye composition, it is good to have a depth, and lifting force is excellent, and dye uptake is high, and degree of fixation is high, and few, the easy washing of dyeing process dye dosage, raffinate are clear, and dyeing behavior is stable.
The technical solution used in the present invention is:
A kind of active black dye composition, at least a component A shown in formula I that mainly comprises 45 ~ 90 mass parts, at least a B component shown in formula II of 1 ~ 30 mass parts, and 1 ~ 40 mass parts at least a shown in formula III component C and/or at least a component D shown in formula IV of 1 ~ 40 mass parts;
In the formula I:
R
1, R
2Independent separately is H, C
1~ C
4Alkyl, C
1~ C
4Alkoxyl group or-SO
3M
1, be preferably-H ,-CH
3,-OCH
3Or-SO
3M
1M
1Be hydrogen or alkali metal atom, be preferably-H or-Na.
In the formula II:
R
3, R
4Independently be separately-H ,-C
1~ C
4Alkyl ,-C
1~ C
4Alkoxyl group or-SO
3M
2, be preferably-H ,-CH
3,-OCH
3Or-SO
3M
2R
5For-H or-SO
3M
2Y
1For-CH=CH
2Or-C
2H
4OSO
3M
2M
2Be hydrogen or alkali metal atom, be preferably-H or-Na.
In the formula III:
R
6For-COOR
7,-CN or-CONR
8R
9, R wherein
7Be M
3Or C
1~ C
4Alkyl, R
8And R
9Independently be-H or C separately
1~ C
4Alkyl; Y
2For-CH=CH
2Or-C
2H
4OSO
3M
3M
3Be hydrogen or alkali metal atom, be preferably-H or-Na.
In the formula IV:
R
10For-SO
3M
4R
11For-COOM
4,-SO
3M
4,-SO
2CH=CH
2Or-SO
2C
2H
4OSO
3M
4Y
3, Y
4Separately be-CH=CH
2,-C
2H
4OSO
3M
4M
4Be H or alkali metal atom, preferred H or Na.
Preferably, based on described component A ~ D quality sum, the quality percentage composition of component A is 50 ~ 85%, and the quality percentage composition of B component is 1 ~ 25%, the quality percentage composition of component C is 0 ~ 35%, and the quality percentage composition of component D is that 0 ~ 35%(component C and D quality percentage composition are not 0 simultaneously).
Preferably, described active black dye composition is comprised of component A, B component and component C, and wherein, the quality percentage composition of component A is 50 ~ 85%, and the quality percentage composition of B component is 5 ~ 20%, and the quality percentage composition of component C is 10～35%.
Preferably, described active black dye composition is comprised of component A, B component and component D, and wherein, the quality percentage composition of component A is 55 ~ 85%, and the quality percentage composition of B component is 1 ~ 20%, and the quality percentage composition of component D is 10～35%.
Preferably, described active black dye composition is comprised of component A, B component, component C and component D, wherein, the quality percentage composition of component A is 50 ~ 85%, the quality percentage composition of B component is 1 ~ 25%, and the quality percentage composition of component C is 5～35%, and the quality percentage composition of component D is 1 ~ 25%.
Described component A is preferably one of following or two or more mixture wherein:
Described B component is preferably one of following or two or more mixture wherein:
Described component C is preferably one of following or two or more mixture wherein:
Described component D is preferably one of following or two or more mixture wherein:
Preferably, active black dye composition of the present invention, by the component A shown at least a formula (I-1)～formula (I-7), B component shown at least a formula (II-1)～(II-7), component C shown at least a formula (III-1)～(III-9) forms, and wherein, the quality percentage composition of component A is 50 ~ 85%, the quality percentage composition of B component is 5 ~ 20%, and the quality percentage composition of component C is 10 ~ 35%.
Perhaps active black dye composition of the present invention, by the component A shown at least a formula (I-1)～formula (I-7), B component shown at least a formula (II-1)～(II-7), component D shown at least a formula (IV-1) ~ (IV ~ 12) forms, wherein, the quality percentage composition of component A is 55 ~ 85%, and the quality percentage composition of B component is 1 ~ 20%, and the quality percentage composition of component D is 10 ~ 35%.
Perhaps the present composition is comprised of the component C shown in the component A shown at least a formula (I-1)～formula (I-9), the B component shown at least a formula (II-1)～(II-7), at least a formula (III-1)～(III-9) and the component D shown at least a formula (IV-1) ~ (IV ~ 12), the quality percentage composition of component A is 50 ~ 85%, the quality percentage composition of B component is 1 ~ 25%, the quality percentage composition of component C is 5～35%, and the quality percentage composition of component D is 1 ~ 25%.
Active black dye composition of the present invention particularly preferably is comprised of component A as follows, B component and component C, wherein:
Component A: be selected from least a dyestuff shown in formula (I-1) ~ (I-3);
B component: be selected from least a dyestuff shown in formula (II-1) ~ (II-3);
Component C: be selected from least a dyestuff shown in formula (III-1), (III-2), (III-7) and (III-8);
Based on said components A, B and C quality sum, the quality percentage composition of component A is 50 ~ 85%, and the quality percentage composition of B component is 5 ~ 20%, and the quality percentage composition of component C is 10 ~ 35%;
Perhaps, active black dye composition of the present invention particularly preferably is comprised of component A as follows, B component and component D, wherein:
Component A: be selected from least a dyestuff shown in formula (I-1) ~ (I-3);
B component: be selected from least a dyestuff shown in formula (II-1) ~ (II-3);
Component D: be selected from least a dyestuff shown in formula (IV-1) ~ (IV-3), (IV-7), (IV-8);
Based on said components A, B and D quality sum, the quality percentage composition of component A is 55 ~ 85%, and the quality percentage composition of B component is 1 ~ 20%, and the quality percentage composition of component D is 10 ~ 35%;
Perhaps, active black dye composition of the present invention particularly preferably is comprised of component A as follows, B component, component C and component D, wherein:
Component A: be selected from least a dyestuff shown in formula (I-1) ~ (I-3);
B component: be selected from least a dyestuff shown in formula (II-1) ~ (II-3);
Component C: be selected from least a dyestuff shown in formula (III-1) ~ (III-2), (III-7) ~ (III-8);
Component D: be selected from least a dyestuff shown in formula (IV-1) ~ (IV-3), (IV-7) ~ (IV-8).
Based on said components A, B, C and D quality sum, the quality percentage composition of component A is 50 ~ 85%, and the quality percentage composition of B component is 1 ~ 25%, and the quality percentage composition of component C is 5～35%, and the quality percentage composition of component D is 1 ~ 25%.
The dye composition of formula I～formula IV of the present invention can free acid (M
1~ M
4For-H) or the form of salt exist, preferably the form with salt exists, described salt can be an alkali metal salt (M
1~ M
4Be basic metal), be particularly preferably sodium salt (M
1~ M
4For-Na).
Active black dye composition of the present invention, employed component A, B component, component C and component D can be synthetic by mode well known to those skilled in the art easily, and wherein the compound of (I) of the present invention, (II), (III) and (IV) can be respectively according to the method described in patent CN101580649, KR100686977, CN102245712, the CN1569969 or similarly method preparation.
Active black dye composition of the present invention, its preparation method comprises formula I～formula IV dyestuff is mixed according to aforementioned proportioning, mixing can adopt conventional mechanical system to carry out, as at shredder, carry out in kneader or the clarifixator, in the mixing process, single dyestuff (I), (II), (III) and (IV) can powdery, granular, the aqueous solution or resulting solution form exist, when single dyestuff (I), (II), (III) and (IV) is during with the form blending of resulting solution, separating composite active black dye of the present invention from resulting solution can carry out with general known method, for example using ionogen (such as sodium-chlor or Repone K) from reaction medium dyestuff to be saltoutd leaches, or mixing solutions evaporated, spraying drying, at this moment, can add the commercialization usual auxiliaries, described auxiliary agent is one of following or the mixture of its arbitrary proportion: solubility promoter, dispersion agent, the alkali resistance auxiliary agent, dust-proofing agent, tensio-active agent, buffer reagent and dyeing accelerant etc., preferred naphthalene sulfonic acidformaldehyde condensation product (NNO), condensation compound of methyl naphthalene sulfonic acid and formaldehyde (Dispersant MF), dispersing agent CNF (benzyl naphthalenesulfonate formaldehyde condensation compound), Sodium sulfate anhydrous.min(99) (industrial sulphuric acid sodium) etc.Above auxiliary agent is commercially available conventional variety, usually, depending on actual needs, the add-on 0 ~ 45% of auxiliary agent, preferred 0 ~ 40% be advisable (account for dyestuff always fill a prescription form weight).
Active black dye composition of the present invention is applicable to the printing and dyeing of cellulosic fibre, tynex and fabric thereof, wherein, the preferred cotton fibre of cellulosic fibre and regenerated fibre, certain vegetative fiber that also can comprise other is such as bast-fibre or fabric; Tynex preferably includes skin, hair or silk at interior animal fiber material, and the filamentary materials such as synthetic nylon 6, nylon 66.When adopting active black dye composition of the present invention to print and dye above-mentioned filamentary material, can abide by known reactive dyes dyeing method carries out, such as reactive dyestuffs in exhaustion staining and pad dyeing staining commonly used, described exhaust dyeing be with textile impregnation in dye liquor, make dyestuff go up gradually the method for dyeing and weaving thing, usually need dyed-fixation-washing-soap boiling-washing-dehydration-operations such as oven dry.
Described pad dyeing then be first textile impregnation in dye liquor, then make fabric pass through roll, dye liquor evenly is rolled into fabric, the dyeing process of processing through decatize or hot melt etc. again, usually need through pad dye liquor-oven dry-(padding fixation liquid)-decatize or bake-wash-soap-wash-operation such as dry.
Usually, because the difference that the dyeing pool requires on the fabric, the dyestuff usage quantity also can be different, when using dip method dyeing, dye level (owf) is generally 0.1%～10%(dyestuff and accounts for fabric weight per-cent), bath raio 1:2 ~ 1:60(fabric and dye liquor weight ratio, preferred 1:10 ~ 1:30, just dye 30 ~ 60 ℃ of temperature controls, dyeing time 10 ~ 30 minutes, 85 ~ 95 ℃ of soap boiling temperature, 10 ~ 15 minutes soap boiling time, 60 ~ 100 ℃ of color fixing temperatures, 10 ~ 50 minutes fixation time, fixation pH value 9 ~ 11.When using pad dyeing method dyeing, the pick-up of cellulosic fibre is generally 60 ~ 80%, 100 ~ 103 ℃ of steam temperatures, steaming time 1 ~ 3 minute.In the pad dyeing method, present more use be the cold-rolling heap staining method, dyestuff and alkaline matter are incorporated in the pad fix machine, and at room temperature clot banks up and carried out fixation in 2 ~ 30 hours, carry out afterwards thorough rinsing.
Beneficial effect of the present invention is mainly reflected in: active black dye composition of the present invention, and when being used for fabric printing, it is good to have enhancing, and degree of fixation is high, dye uptake is high, is easy to washing, and dyeing residual liquid is clear, the Salt And Alkali Tolerance stable performance, wet colour fastness is excellent, is rare economical dark black dye.
(4) embodiment
The present invention is described further below in conjunction with specific embodiment, but protection scope of the present invention is not limited in this:
Compound described in the embodiment can adopt known method, similarly is synthesized with the form of free acid or the form of its salt, and except as otherwise noted, following " part " is folding hundred weight parts.
Embodiment 1:
The dyestuff of 60 parts of formulas (I-1), the dyestuff of 13 parts of formulas (II-1), dyestuff and 4 parts of Sodium sulfate anhydrous.min(99) of 23 parts of formulas (III-8) are carried out mechanically mixing, and the composite dye that obtains dyes the cotton aterrimus that is.
Embodiment 2
The dyestuff of 57 parts of formulas (I-3), the dyestuff of 16 parts of formulas (II-2), dyestuff and 2.5 parts of Sodium sulfate anhydrous.min(99) of 27 parts of formulas (III-7) are carried out mechanically mixing, and the composite dye that obtains dyes the cotton aterrimus that is.
Embodiment 3
With the dyestuff of 56 parts of formulas (I-3), the dyestuff of 17 parts of formulas (II-2), the dyestuff of 12 parts of formulas (III-7), the dyestuff of 15 parts of formulas (IV-1), carry out mechanically mixing, the composite dye that obtains dyes the cotton aterrimus that is.
Embodiment 4～28:
The dyestuff of listed proportioning in the mechanically mixing table 1 dyes the cotton aterrimus that is.
Table 1
Application Example:
Get the reactive black dye that the embodiment of the invention 1 ~ 28 makes, be dissolved in respectively in the water, add Sodium sulfate anhydrous.min(99) 50g/L and be configured to dye liquor.Dyeing concentration 4%(dyestuff is heavy to cloth); the heavy grams of bath raio 1:10(cloth is to dye liquor volume milliliter number), insert 60 ℃ of lower absorption of cotton 30 minutes, add alkali (sodium hydroxide 15g/L, yellow soda ash 10g/L) fixation 45 minutes; DYED FABRICS obtains black dyeing and weaving thing through washing, soap boiling, drying.
(1) colour fastness
Test its washing fastness according to ISO 105-C03,60 ℃:
Former state Bian Se＞=4-5 level; Zhan Se＞=4 grade
Test its fastness to perspiration according to ISO 105-E04:
Acid sweat: Bian Se＞=4 grades; Zhan Se＞=3-4 level
Alkali sweat: Bian Se＞=4 grades; Zhan Se＞=3-4 level
Test its fastness to rubbing according to ISO 105-X12:
Metal to-metal contact:＞=4-5 level; Wet friction:＞=2-3 level
Test its water-fast Lao of soaking Du＞=4-5 level according to ISO 105-E01.
Test its fastness to ironing according to ISO 105-X11, Bian Se＞=4-5 level.
(2) salt tolerant alkalescence: during above-mentioned dyeing, along with the increase of salt consumption, pH value, power part increases respectively, and coloured light is not had impact substantially, and reactive black dye Salt And Alkali Tolerance of the present invention stable performance is described.
The counterstain experiment:
Comparative Examples 1 according to the embodiment 31 among the patent CN102245712, is prepared as follows the reactive black dye of three components:
Comparative Examples 2 according to the embodiment 6 among the patent CN1730566, is prepared as follows the reactive black dye of three components:
According to the described method of above-mentioned Application Example, choose among the present invention and carry out the dyeing behavior contrast with Comparative Examples 1,2 immediate embodiment 22, embodiment 5, embodiment 21, the result is as follows:
(1) lifting force contrast, the K/S value under the coloured differently degree of depth
| Dye level | 2.0% | 4.0% | 6.0% | 8.0% | 10.0% | 12.0% |
| Embodiment 5 | 18.59 | 27.06 | 34.12 | 37.10 | 39.78 | 40.61 |
| Embodiment 21 | 17.69 | 26.12 | 32.85 | 35.32 | 37.83 | 39.80 |
| Embodiment 22 | 17.03 | 24.97 | 30.17 | 35.19 | 37.26 | 39.63 |
| Comparative Examples 1 | 12.92 | 20.64 | 26.11 | 29.11 | 31.63 | 32.94 |
| Comparative Examples 2 | 15.24 | 23.00 | 27.91 | 33.73 | 34.13 | 34.24 |
As seen from the above table, along with the increase of dye level, depth of the present invention is significantly better than the comparative example.
(2) dye uptake contrast, %
| Dyeing time | 0 | 15min | 30min | 40min | 50min | 70min | 90min |
| Embodiment 5 | 0 | 45.98 | 49.32 | 70.23 | 77.15 | 79.38 | 80.75 |
| Embodiment 21 | 0 | 44.45 | 46.27 | 69.32 | 76.09 | 78.66 | 79.98 |
| Embodiment 22 | 0 | 43.37 | 45.61 | 69.56 | 75.81 | 78.47 | 79.76 |
| Comparative Examples 1 | 0 | 32.90 | 37.16 | 64.47 | 70.45 | 71.64 | 72.00 |
| Comparative Examples 2 | 0 | 30.46 | 36.09 | 65.52 | 71.26 | 73.06 | 73.32 |
(3) degree of fixation contrast, %
| The fixation time | 0 | 15min | 30min | 40min | 50min | 70min | 90min |
| Embodiment 5 | ? | ? | 0 | 63.89 | 72.02 | 74.59 | 76.19 |
| Embodiment 21 | ? | ? | 0 | 64.10 | 71.73 | 74.08 | 75.57 |
| Embodiment 22 | ? | ? | 0 | 64.58 | 71.33 | 74.64 | 75.66 |
| Comparative Examples 1 | ? | ? | 0 | 57.39 | 63.94 | 66.32 | 67.10 |
| Comparative Examples 2 | ? | ? | 0 | 57.97 | 65.68 | 69.02 | 69.42 |
As seen from the above table, dyestuff of the present invention obviously is better than the comparative example, and for the industry, it all is being significantly improved aspect lifting force, dye uptake and the degree of fixation.
Claims (8)
1. active black dye composition, at least a component A shown in formula I that mainly comprises 45 ~ 90 mass parts, at least a B component component shown in formula II of 1 ~ 30 mass parts, and 1 ~ 40 mass parts at least a shown in formula III component C and/or at least a component D shown in formula IV of 1 ~ 40 mass parts;
In the formula I:
R
1, R
2Independent separately is H, C
1~ C
4Alkyl, C
1~ C
4Alkoxyl group or-SO
3M
1M
1Be hydrogen or alkali metal atom;
In the formula II:
R
3, R
4Independently be separately-H ,-C
1~ C
4Alkyl ,-C
1~ C
4Alkoxyl group or-SO
3M
2R
5For-H or-SO
3M
2Y
1For-CH=CH
2Or-C
2H
4OSO
3M
2M
2Be hydrogen or alkali metal atom.
In the formula III:
R
6For-COOR
7,-CN or-CONR
8R
9, R wherein
7Be M
3Or C
1~ C
4Alkyl, R
8And R
9Independently be-H or C separately
1~ C
4Alkyl; Y
2For-CH=CH
2Or-C
2H
4OSO
3M
3M
3Be hydrogen or alkali metal atom;
In the formula IV:
R
10For-SO
3M
4R
11For-COOM
4,-SO
3M
4,-SO
2CH=CH
2Or-SO
2C
2H
4OSO
3M
4Y
3, Y
4Separately be-CH=CH
2,-C
2H
4OSO
3M
4M
4Be H or alkali metal atom.
2. active black dye composition as claimed in claim 1, it is characterized in that described active black dye composition is comprised of component A, B component and component C, the quality percentage composition of component A is 50 ~ 85%, and the quality percentage composition of component B is 5 ~ 20%, and the quality percentage composition of component C is 10～35%.
3. active black dye composition as claimed in claim 1, it is characterized in that described active black dye composition is comprised of component A, B component and component D, the quality percentage composition of component A is 55 ~ 85%, and the quality percentage composition of component B is 1 ~ 20%, and the quality percentage composition of component D is 10～35%.
4. active black dye composition as claimed in claim 1, it is characterized in that: described active black dye composition is comprised of component A, B component, component C and component D, the quality percentage composition of component A is 50 ~ 85%, the quality percentage composition of component B is 1 ~ 25%, the quality percentage composition of component C is 5～35%, and the quality percentage composition of component D is 1 ~ 25%.
5. such as the described active black dye composition of one of claim 1 ~ 4, it is characterized in that described component A is one of following or two or more mixture wherein:
6. such as the described active black dye composition of one of claim 1 ~ 4, it is characterized in that described B component is one of following or two or more mixture wherein:
7. such as claim 1,2, one of 4 described active black dye compositions, it is characterized in that described component C is one of following or two or more mixture wherein:
8. such as claim 1,3, one of 4 described active black dye compositions, it is characterized in that described component D is one of following or two or more mixture wherein:
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| CN104927394A (en) * | 2015-05-27 | 2015-09-23 | 江苏沃尔得化工有限公司 | Synthetic process for active dye black |
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