CN104987750A - Low-alkaline or alkali-free active golden yellow dye and preparation method thereof - Google Patents
Low-alkaline or alkali-free active golden yellow dye and preparation method thereof Download PDFInfo
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Abstract
The invention relates to low-alkaline or alkali-free active golden yellow dye and a preparation method thereof. The low-alkaline or alkali-free active golden yellow dye comprises any compound selected from the general formula (1) or a mixture formed by compounding any two or more compounds selected from the general formula (1) in any proportion, wherein in the formula (1), M represents hydrogen or alkali metal; B is a dual-amine connecting bridge group. The low-alkaline or alkali-free active golden yellow dye is quite good in color staining and capable of resisting the high temperature of 140 DEG C, can be used for one-bath one-step dyeing of interweaving and blending of brocade cotton or polyester cotton and helps a printing and dyeing mill to save energy and reduce emission.
Description
Technical field
The present invention relates to the reactive dyestuff field in new material technology, particularly a kind of low alkali or non-alkali reactive golden yellow dye well its preparation method.
Background technology
Traditional reactive dyeing all needs to be cross-linked set with alkaline agent and cotton fibre, the alkaline agent generally added is soda ash, consumption is at 20g/l, not only waste a large amount of alkaline agents, and make alkalinity in dyeing waste water higher, need outer acid adding agent to neutralize, not only serious waste resource, and add three-protection design difficulty.
Chlorine on active group " chlorotriazine " in traditional KE type or HE type reactive dyestuffs is open existence, though dyestuff can be high temperature resistant, but the staining fastness of dyestuff is bad, when blended union dyeing is done with such dyestuff by printing and dyeing mill, the technique often adopted is for washing/cotton two one-bath two-step process, brocade/cotton two one-bath two-step process etc., and these process energy consumptions are large, waste water is many, and manpower consumption is also large.
Summary of the invention
The above-mentioned Problems existing of technology, it is better that first goal of the invention of the present invention there are provided the level such as a kind of staining fastness, resistance to 140 DEG C of high temperature, and energy consumption is low, the low alkali of the one that waste discharge is few or non-alkali reactive golden yellow dyestuff; Second goal of the invention is the preparation method providing above-mentioned a kind of low alkali or non-alkali reactive golden yellow dyestuff; In addition, the low alkali provided based on first goal of the invention or non-alkali reactive golden yellow dyestuff; The low alkali that 3rd goal of the invention of the present invention is to provide another kind of auxiliary agent to improve or non-alkali reactive golden yellow dyestuff.
In order to realize above-mentioned three goals of the invention be technically associated, the technical solution used in the present invention is:
A kind of low alkali or non-alkali reactive golden yellow dyestuff, it comprises any one compound in the formula of being selected from (1) general formula, or in formula (1) general formula any two or more compound according to the composite mixture of arbitrary proportion;
In its Chinese style (1):
M is hydrogen or basic metal;
B is the connection abutment of band diamine, is selected from the one in following structure:
-NHCH
2cH
2nH-,-NHCH
2cH
2cH
2nH-, the M connected in abutment are hydrogen or basic metal.
As preferably, described B is the connection abutment of band diamine, is selected from the one in following structure:
-NHCH
2cH
2nH-,-NHCH
2cH
2cH
2nH-, the M connected in abutment represent-Na ,-K or-Li.
As preferably, the reactive golden yellow dyestuff shown in formula (1) is the mixture of following formula (1-1) to a kind of or any several concrete structure formula in formula (1-12):
A preparation method for above-mentioned low alkali or non-alkali reactive golden yellow dyestuff, adopts following raw material: formula I, formula II, formula III, formula (V) and B structure.
M wherein in formula I represents hydrogen or basic metal;
Described B structure is selected from the one in following structure:
nH
2cH
2cH
2nH
2, NH
2cH
2cH
2cH
2nH
2, in B structure, M represents hydrogen or basic metal;
The preparation process of process comprises as follows:
A. doazo reaction: formula I is carried out diazotization reaction under the effect of Sodium Nitrite and hydrochloric acid;
B. coupled reaction: the diazotization reaction product of above-mentioned formula I and formula II carry out coupled reaction;
C. a contracting reaction: the conjugates of b step reaction and formula III are carried out condensation reaction;
D. two contracting reactions: a contracting thing of c step reaction and B structure are carried out condensation reaction;
E. three contracting reactions: two contracting things of d step reaction and formula (V) are carried out condensation reaction, and reaction terminates the low alkali of rear acquisition or non-alkali reactive golden yellow dyestuff finished product;
Further, the doazo reaction described in step a carries out under needing the effect of Sodium Nitrite and hydrochloric acid, and temperature controls to carry out under control 1.0-2.0 at 0-20 DEG C, pH;
Coupled reaction described in step b is carried out under needing the effect of sodium bicarbonate or soda ash, and temperature controls to control at 4.0-6.0 at 5-25 DEG C, pH
Carry out under a contracting reaction needed sodium bicarbonate described in step c or the effect of soda ash, temperature of reaction controls to control to carry out under 5.0-7.0 at 10-30 DEG C, pH;
Carry out under two contracting reaction needed sodium bicarbonate described in steps d or the effect of soda ash, temperature of reaction controls to control to carry out under 5.0-7.0 at 30-50 DEG C, pH;
Carry out under three contracting reaction needed sodium bicarbonate described in step e or the effect of soda ash, temperature of reaction controls to control to carry out under 4.0-6.0 at 70-90 DEG C, pH;
In order to realize above-mentioned 3rd goal of the invention, technical scheme of the present invention is specific as follows:
A kind of low alkali or non-alkali reactive golden yellow dyestuff, mixed by above-mentioned low alkali or non-alkali reactive golden yellow dyestuff and auxiliary agent and form; Described auxiliary agent is selected from a kind of or two or more arbitrarily mixture in Sodium sulfate anhydrous.min(99), Sodium hexametaphosphate 99, condensation compound of methyl naphthalene sulfonic acid and formaldehyde, naphthalene sulfonic acidformaldehyde condensation product.Further, described auxiliary agent is Sodium sulfate anhydrous.min(99).
Compared with prior art, beneficial effect of the present invention is as follows:
One, the low alkali that the present invention relates to or non-alkali reactive golden yellow dyestuff, only need to add 1-3g/l alkaline agent during this reactive dyeing and just can be cross-linked set with cotton fibre, even do not add alkaline agent, under the condition of dye bath pH=7, this invention reactive golden yellow dyestuff and cotton fibre just can be made to be cross-linked set.This is a kind of and the diverse novel process of traditional technology, new technology, is specially adapted to various union dyeing.These group reactive dyestuffs become covalent bonds with cotton fibre, therefore stablize and have the dry levels such as fastness, light fastness, washing fastness that wet preferably.The pyridine carboxylic acid thrown off is a kind of VITAMIN, less on environmental protection impact.
Two, infect KE type or HE type reactive dyestuffs in active group " chlorotriazine " on chlorine be open existence, and the chlorine on active group " chlorotriazine " in reactive dyestuffs of the present invention by nicotinic acid or γ-picolinic acid replace, so the percent hydrolysis of dyestuff also can decrease during dyeing, dye structure is more stable, can the hot conditions of resistance to 140 DEG C.Neutral fixation, the characteristic condition such as high temperature resistant other dyeings just can be given play to, thus the dyeing technique of applicable blended union, the blend dyeing novel process of existing market maturation mainly can be used for washing/cotton one-bath one-step dyeing, brocade/cotton one-bath one-step dyeing, wash/cotton one-bath two-step process, brocade/cotton one-bath two-step process etc., and the dyeing of traditional blended union is for washing/cotton two one-bath two-step process, brocade/cotton two one-bath two-step process etc.The appearance energy efficient greatly of this patent product, reduces discharge of wastewater, decreases manpower consumption etc.
Three, through testing and verification, due to the relation of dye structure, the cotton of this invention reactive golden yellow dyestuff, nylon, terylene staining are very good.This advantage adopts the printing and dyeing novel process such as bath one step or bath two steps when being also more applicable for the dyeing of blended union.
Four, used in the method for the invention various starting material can commercially obtain, and raw material is easy to get, and synthesis cost is low.
Five, the preparation process of compound prepared of the present invention and use procedure are all safety, environmental protection, energy-conservation.
Embodiment
The explanation of the following examples just to technical scheme of the present invention, does not form any restriction to technical scheme of the present invention and protection domain.
Embodiment 1: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-1) structure:
(1-1) its synthetic method step of compound of structure is as follows:
1, doazo reaction: 30g2-naphthylamines-3,6,8-trisulfonic acid is added end water 50g, trash ice 100g, dispersion agent 1g pulls an oar 2 hours.Evenly add in sodium nitrite solution more afterwards, and keep congo-red test paper to show blue look.Sodium nitrite solution adds complete, is incubated 12-15 DEG C of reaction 1.5 hours, adds 0.5g thionamic acid and to disappear unnecessary Sodium Nitrite.Shown in following (a) formula of doazo reaction equation:
Wherein, sodium nitrite solution is formed by the molten clear configuration in advance of 4g Sodium Nitrite+15g water stirring.
2, coupled reaction: between 10g, urea groups aniline adds water 100g, pulls an oar after 30 minutes, adds sodium bicarbonate 5g slowly and adjusts pH to 6-7, and stablize 10 minutes.Add 50g trash ice and be cooled to less than 10 DEG C.Again by above-mentioned 2-naphthylamines-3,6,8-trisulfonic acid, diazo liquid between urea groups aniline
Slowly add below liquid level, add sodium bicarbonate 6g simultaneously slowly and keep pH=5-6, temperature T=5-15 DEG C.Complete to pot, react 2-3 hour to terminal.Shown in following (b) formula of coupled reaction equation:
3, a contracting reaction: 10g cyanuric chloride adds water 50g, trash ice 150g, dispersion agent 1g in about 0 DEG C making beating 1 hour.Above-mentioned coupling solution being added slowly cyanuric chloride suspends in material, control PH≤6.0 time reinforced, temperature 0-15 DEG C.Complete to pot, first stir after 10 minutes, evenly add sodium bicarbonate 5g slowly and adjust pH=5-6.Be incubated the reaction of 8-10 DEG C of insulation pH value to terminal (1-2 hour).Shown in following (c) formula of one contracting reaction equation:
4, two contracting reactions: a contracting terminal arrives, and is added slowly by 10.5g4.4-diaminobenzil-2.2-disulfonic acid dry powder, adds sodium bicarbonate 5g slowly and adjusts pH=5-6, stir 20 minutes, be warming up to 45-55 DEG C, then add sodium bicarbonate 2g adjustment pH=5-7 slowly, insulation reaction to terminal, 7-8 hour.Shown in following (d) formula of two contracting reaction equations:
5, three contracting reactions: 7g nicotinic acid dry powder directly adds in two contracting liquid, stirs after 10 minutes, is directly warming up to 80-85 DEG C, and keeps pH=4-6 with 10g sodium bicarbonate.Control reaction (reaction 8-10 hour) to terminal.Shown in following (e) formula of three contracting reaction equations:
6, steam drying: terminal directly obtains 86g formula (1-1) reactive golden yellow dyestuff with steam drying after arriving.
Embodiment 2: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-2) structure:
(1-2) its synthetic method step of compound of structure is as follows:
1, doazo reaction: 30g2-naphthylamines-3,6,8-trisulfonic acid is added end water 50g, trash ice 100g, dispersion agent 1g pulls an oar 2 hours.Evenly add sodium nitrite solution the same in above-described embodiment 1, and keep congo-red test paper to show blue look.Sodium nitrite solution adds complete, is incubated 12-15 DEG C of reaction 1.5 hours, adds 0.5g thionamic acid and to disappear unnecessary Sodium Nitrite.Shown in following (a) formula of doazo reaction equation:
2, coupled reaction: between 10g, urea groups aniline adds water 100g, pulls an oar after 30 minutes, adds soda ash 3.2g slowly and adjusts pH to 6-7, and stablize 10 minutes.Add 50g trash ice and be cooled to less than 10 DEG C.Again by above-mentioned 2-naphthylamines-3,6,8-trisulfonic acid, diazo liquid between add slowly below urea groups aniline liquid level, add soda ash 3.8g simultaneously slowly and keep pH=5-6, temperature T=5-15 DEG C.Complete to pot, reaction to terminal (2-3 hour).Shown in following (b) formula of coupled reaction equation:
3, a contracting reaction: 10g cyanuric chloride adds water 50g, trash ice 150g, dispersion agent 1g in about 0 DEG C making beating 1 hour.Above-mentioned coupling solution being added slowly cyanuric chloride suspends in material, control PH≤6.0 time reinforced, temperature 0-15 DEG C.Complete to pot, first stir after 10 minutes, evenly add soda ash 3.2g slowly and adjust pH=5-6.Be incubated the reaction of 8-10 DEG C of insulation pH value to terminal (1-2 hour).Shown in following (c) formula of one contracting reaction equation:
4, two contracting reactions: a contracting terminal arrives, 10.5g4.4-diaminobenzil-2.2-disulfonic acid dry powder is added slowly, slowly add soda ash 3.2g and adjust pH=5-6, stir 20 minutes, be warming up to 45-55 DEG C, slowly add soda ash 1.3g again and adjust pH=5-7, insulation reaction is (7-8 hour) to terminal.Shown in following (d) formula of two contracting reaction equations:
5, three contracting reactions: 7g γ-picolinic acid dry powder directly adds in two contracting liquid, stirs after 10 minutes, is directly warming up to 80-85 DEG C, and keeps pH=4-6 with 6.3g soda ash.Control reaction (reaction 8-10 hour) to terminal.Shown in following (e) formula of three contracting reaction equations:
6, steam drying: terminal directly obtains 86g formula (1-2) reactive golden yellow dyestuff with steam drying after arriving.
Embodiment 3: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-3) structure:
(1-3) its synthetic method step of compound of structure is as follows:
1, doazo reaction: 30g2-naphthylamines-3,6,8-trisulfonic acid is added end water 50g, trash ice 100g, dispersion agent 1g pulls an oar 2 hours.Evenly add sodium nitrite solution, and keep congo-red test paper to show blue look.Sodium nitrite solution adds complete, is incubated 12-15 DEG C of reaction 1.5 hours, adds 0.5g thionamic acid and to disappear unnecessary Sodium Nitrite.Shown in following (a) formula of doazo reaction equation:
2, coupled reaction: between 10g, urea groups aniline adds water 100g, pulls an oar after 30 minutes, adds sodium bicarbonate 5g slowly and adjusts pH to 6-7, and stablize 10 minutes.Add 50g trash ice and be cooled to less than 10 DEG C.Again by above-mentioned 2-naphthylamines-3,6,8-trisulfonic acid diazo liquid between add slowly below urea groups aniline liquid level, add sodium bicarbonate 6g simultaneously slowly and keep pH=5-6, temperature T=5-15 DEG C.Complete to pot, reaction to terminal (2-3 hour).Shown in following (b) formula of coupled reaction equation:
3, a contracting reaction: 10g cyanuric chloride adds water 50g, trash ice 150g, dispersion agent 1g in about 0 DEG C making beating 1 hour.Above-mentioned coupling solution being added slowly cyanuric chloride suspends in material, control PH≤6.0 time reinforced, temperature 0-15 DEG C.Complete to pot, first stir after 10 minutes, evenly add sodium bicarbonate 5g slowly and adjust pH=5-6.Be incubated the reaction of 8-10 DEG C of insulation pH value to terminal (1-2 hour).Shown in following (c) formula of one contracting reaction equation:
4, two contracting reactions: a contracting terminal arrives, and is added slowly by 9.5g2,2-disulfonic acid p-diaminodiphenyl dry powder, slowly add sodium bicarbonate 5g and adjust pH=5-6, stir 20 minutes, be warming up to 45-55 DEG C, slowly add sodium bicarbonate 2g again and adjust pH=5-7, insulation reaction is (7-8 hour) to terminal.Shown in following (d) formula of two contracting reaction equations:
5, three contracting reactions: 7g nicotinic acid dry powder directly adds in two contracting liquid, stirs after 10 minutes, is directly warming up to 80-85 DEG C, and keeps pH=4-6 with 10g sodium bicarbonate.Control reaction (reaction 8-10 hour) to terminal.Shown in following (e) formula of three contracting reaction equations:
6, steam drying: terminal directly obtains 85g formula (1-3) reactive golden yellow dyestuff with steam drying after arriving.
Embodiment 4: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-4) structure:
(1-4) its synthetic method step of compound of structure is as follows:
1, doazo reaction: 2-naphthylamines-3,6, the 8-trisulfonic acid of 30g is added end water 50g, trash ice 100g, dispersion agent 1g pulls an oar 2 hours.Evenly add sodium nitrite solution, and keep congo-red test paper to show blue look.Sodium nitrite solution adds complete, is incubated 12-15 DEG C of reaction 1.5 hours, adds 0.5g thionamic acid and to disappear unnecessary Sodium Nitrite.Shown in following (a) formula of doazo reaction equation:
2, coupled reaction: between 10g, urea groups aniline adds water 100g, pulls an oar after 30 minutes, adds soda ash 3.2g slowly and adjusts pH to 6-7, and stablize 10 minutes.Add 50g trash ice and be cooled to less than 10 DEG C.Again by above-mentioned 2-naphthylamines-3,6,8-trisulfonic acid diazo liquid between add slowly below urea groups aniline liquid level, add soda ash 3.8g simultaneously slowly and keep pH=5-6, temperature T=5-15 DEG C.Complete to pot, reaction to terminal (2-3 hour).Shown in following (b) formula of coupled reaction equation:
3, a contracting reaction: 10g cyanuric chloride adds water 50g, trash ice 150g, dispersion agent 1g in about 0 DEG C making beating 1 hour.Above-mentioned coupling solution being added slowly cyanuric chloride suspends in material, control PH≤6.0 time reinforced, temperature 0-15 DEG C.Complete to pot, first stir after 10 minutes, evenly add soda ash 3.2g slowly and adjust pH=5-6.Be incubated the reaction of 8-10 DEG C of insulation pH value to terminal (1-2 hour).Shown in following (c) formula of one contracting reaction equation:
4, two contracting reactions: a contracting terminal arrives, and is added slowly by 9.5g2,2-disulfonic acid p-diaminodiphenyl dry powder, slowly add sodium bicarbonate 5g and adjust pH=5-6, stir 20 minutes, be warming up to 45-55 DEG C, slowly add sodium bicarbonate 2g again and adjust pH=5-7, insulation reaction is (7-8 hour) to terminal.Shown in following (d) formula of two contracting reaction equations:
5, three contracting reactions: 7g γ-picolinic acid dry powder directly adds in two contracting liquid, stirs after 10 minutes, is directly warming up to 80-85 DEG C, and keeps pH=4-6 with 10g sodium bicarbonate.Control reaction (reaction 8-10 hour) to terminal.Shown in following (e) formula of three contracting reaction equations:
6, steam drying: terminal directly obtains 85g formula (1-4) reactive golden yellow dyestuff with steam drying after arriving.
Embodiment 5: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-5) structure:
Formula (1-5) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 6: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-6) structure:
Formula (1-6) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 7: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-7) structure:
Formula (1-7) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 8: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-8) structure:
Formula (1-8) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 9: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-9) structure:
Formula (1-9) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 10: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-10) structure:
Formula (1-10) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 11: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-11) structure:
Formula (1-11) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 12: a kind of low alkali or non-alkali reactive golden yellow dyestuff, be made up of the compound of simple formula (1-12) structure:
Formula (1-12) its preparation method adopts following raw material:
Its preparation process and embodiment 1,2,3,4 identical.
Embodiment 13: a kind of low alkali or non-alkali reactive golden yellow dyestuff, by formula (1-1) the structural compounds 80g in embodiment 1, formula (1-2) structural compounds 10g in embodiment 2, mix in embodiment 12 Chinese style (1-12) structural compounds 10g tempering tank, or spraying dry after common dissolving.
Embodiment 14: a kind of low alkali or non-alkali reactive golden yellow dyestuff, by embodiment 3 Chinese style (1-3) structural compounds 5g, embodiment 4 Chinese style (1-4) structural compounds 50g, embodiment 5 Chinese style (1-5) structural compounds 5g, the mixture of embodiment 6 Chinese style (1-6) structural compounds 40g mixes in tempering tank with 10g Sodium sulfate anhydrous.min(99), or spraying dry after common dissolving.
Embodiment 15: a kind of low alkali or non-alkali reactive golden yellow dyestuff, by embodiment 1 Chinese style (1-1) structural compounds 50g, embodiment 2 Chinese style (1-2) structural compounds 20g, embodiment 10 Chinese style (1-10) structural compounds 10g, the mixture of embodiment 7 Chinese style (1-7) structural compounds 20g mixes in tempering tank with 20g Sodium sulfate anhydrous.min(99), or spraying dry after common dissolving.
Embodiment 16: a kind of low alkali or non-alkali reactive golden yellow dyestuff, by embodiment 5 Chinese style (1-5) structural compounds 50g, embodiment 12 Chinese style (1-12) structural compounds 50g and Sodium hexametaphosphate 99 15g mixes in tempering tank, or spraying dry after common dissolving.
Embodiment 17: a kind of low alkali or non-alkali reactive golden yellow dyestuff, by embodiment 6 Chinese style (1-6) structural compounds 30g, mix in embodiment 11 Chinese style (1-11) structural compounds 70g and condensation compound of methyl naphthalene sulfonic acid and formaldehyde 20g tempering tank, or spraying dry after common dissolving.
Embodiment 18: a kind of low alkali or non-alkali reactive golden yellow dyestuff, is to change the reaction raw materials sodium bicarbonate in preparation process 2,3,4,5 or soda ash into saleratus with the difference of embodiment 1.
The part Dyeing Example of above-mentioned low alkali or non-alkali reactive golden yellow dyestuff:
Respectively taking the above-mentioned dyestuff of 1g (1-1)---the dye monomer compound that (1-12) is obtained or its two kinds or two or more mixture (embodiment 13-17) are placed in dye cup, dyestuff weighs 2% with fabric and dyes, be in the dye bath of 1:20 containing 60g/L Sodium sulfate anhydrous.min(99), bath raio, adsorb 30min at 60 DEG C, add soda ash (consumption 0-3g/L) fixation 45min.Dyeing and weaving thing through washing, soaping, dry.The red cotton obtained has the redness of homogeneity, satisfied Exposure to Sunlight and fastness to rubbing, and specific performance is in table 1.
Table 1
Detect according to great many of experiments and show that reactive golden yellow dyestuff of the present invention has excellent application performance than the reactive golden yellow dyestuff of traditional HE type or KE type, concrete correlation data is in table 2.
Table 2
Finally, it is also to be noted that enumerate above be only specific embodiments of the invention son.Obviously, the invention is not restricted to above examples of implementation, many distortion can also be had.All distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.
Claims (7)
1. a low alkali or non-alkali reactive golden yellow dyestuff, it is characterized in that: it comprises any one compound in the formula of being selected from (1) general formula, or in formula (1) general formula any two or more compound according to the composite mixture of arbitrary proportion;
In its Chinese style (1):
M is hydrogen or basic metal;
B is the connection abutment of band diamine, is selected from the one in following structure:
-NHCH
2cH
2nH-,-NHCH
2cH
2cH
2nH-, the M connected in abutment are hydrogen or basic metal.
2. the low alkali of one according to claim 1 or non-alkali reactive golden yellow dyestuff, is characterized in that:
Described B is the connection abutment of band diamine, is selected from the one in following structure:
-NHCH
2cH
2nH-,-NHCH
2cH
2cH
2nH-, the M connected in abutment represent-Na ,-K or-Li.
3. the low alkali of one according to claim 1 or non-alkali reactive golden yellow dyestuff, is characterized in that:
Golden yellow reactive dyestuffs shown in formula (1) are the mixture of following formula (1-1) to a kind of or any several concrete structure formula in formula (1-12):
。
4. a preparation method for a kind of low alkali or non-alkali reactive golden yellow dyestuff as claimed in claim 1, is characterized in that:
Adopt following raw material: formula I, formula II, formula III, formula (V) and B structure.
M wherein in formula I represents hydrogen or basic metal;
Described B structure is selected from the one in following structure:
nH
2cH
2cH
2nH
2, NH
2cH
2cH
2cH
2nH
2, in B structure, M represents hydrogen or basic metal;
The preparation process of process comprises as follows:
A. doazo reaction: formula I is carried out diazotization reaction under the effect of Sodium Nitrite and hydrochloric acid;
B. coupled reaction: the diazotization reaction product of above-mentioned formula I and formula II carry out coupled reaction;
C. a contracting reaction: the conjugates of b step reaction and formula III are carried out condensation reaction;
D. two contracting reactions: a contracting thing of c step reaction and B structure are carried out condensation reaction;
E. three contracting reactions: two contracting things of d step reaction and formula (V) are carried out condensation reaction, and reaction terminates the low alkali of rear acquisition or non-alkali reactive golden yellow dyestuff finished product;
。
5. the low alkali of one according to claim 5 or non-alkali reactive golden yellow preparation of dyestuff method, is characterized in that:
Doazo reaction described in step a carries out under needing the effect of Sodium Nitrite and hydrochloric acid, and temperature controls to carry out under control 1.0-2.0 at 0-20 DEG C, pH;
Coupled reaction described in step b is carried out under needing the effect of sodium bicarbonate or soda ash, and temperature controls to control at 4.0-6.0 at 5-25 DEG C, pH
Carry out under a contracting reaction needed sodium bicarbonate described in step c or the effect of soda ash, temperature of reaction controls to control to carry out under 5.0-7.0 at 10-30 DEG C, pH;
Carry out under two contracting reaction needed sodium bicarbonate described in steps d or the effect of soda ash, temperature of reaction controls to control to carry out under 5.0-7.0 at 30-50 DEG C, pH;
Carry out under three contracting reaction needed sodium bicarbonate described in step e or the effect of soda ash, temperature of reaction controls to control to carry out under 4.0-6.0 at 70-90 DEG C, pH.
6. low alkali or a non-alkali reactive golden yellow dyestuff, is characterized in that: mixed by golden yellow reactive dyestuffs according to claim 1 and auxiliary agent and form; Described auxiliary agent is selected from a kind of or two or more arbitrarily mixture in Sodium sulfate anhydrous.min(99), Sodium hexametaphosphate 99, condensation compound of methyl naphthalene sulfonic acid and formaldehyde, naphthalene sulfonic acidformaldehyde condensation product.
7. the golden yellow reactive dyestuffs of one according to claim 6, is characterized in that: described auxiliary agent is Sodium sulfate anhydrous.min(99).
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| CN106833012A (en) * | 2016-12-05 | 2017-06-13 | 泰兴锦云染料有限公司 | A kind of Yellow reactive dyes and its preparation and application |
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| CN104371355A (en) * | 2014-09-29 | 2015-02-25 | 浙江亿得化工有限公司 | Low-alkali or alkali-free active golden dye and preparation method thereof |
| CN105400230B (en) * | 2015-11-18 | 2018-04-24 | 浙江闰土研究院有限公司 | A kind of method that azo dyes is prepared by coupling reaction |
| CN106752061B (en) * | 2016-12-23 | 2019-07-16 | 浙江浩川科技有限公司 | A kind of method preparing benzidine yellow pigment and benzidine yellow pigment |
| CN111100478B (en) * | 2019-12-30 | 2021-03-05 | 浙江劲光实业股份有限公司 | Preparation method and application of blue dye with three active groups |
| CN112480707B (en) * | 2020-10-30 | 2022-05-31 | 苏州澳缘盛新材料科技有限公司 | Reactive dye yellow and preparation method and application thereof |
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| US20030150354A1 (en) * | 2001-05-14 | 2003-08-14 | Seiko Epson Corporation | Ink set and ink jet recording method |
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| CN106833012A (en) * | 2016-12-05 | 2017-06-13 | 泰兴锦云染料有限公司 | A kind of Yellow reactive dyes and its preparation and application |
| CN106833012B (en) * | 2016-12-05 | 2018-08-31 | 泰兴锦云染料有限公司 | A kind of Yellow reactive dyes and its preparation and application |
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