CN101724298B - Aftertreatment method for liquid disperse dye - Google Patents
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- CN101724298B CN101724298B CN 200910155193 CN200910155193A CN101724298B CN 101724298 B CN101724298 B CN 101724298B CN 200910155193 CN200910155193 CN 200910155193 CN 200910155193 A CN200910155193 A CN 200910155193A CN 101724298 B CN101724298 B CN 101724298B
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- 238000003756 stirring Methods 0.000 claims abstract description 15
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- 239000000203 mixture Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 8
- ROPYWXVRNREIQD-UHFFFAOYSA-N 2-[n-(2-cyanoethyl)-4-[(2,6-dichloro-4-nitrophenyl)diazenyl]anilino]ethyl acetate Chemical compound C1=CC(N(CCC#N)CCOC(=O)C)=CC=C1N=NC1=C(Cl)C=C([N+]([O-])=O)C=C1Cl ROPYWXVRNREIQD-UHFFFAOYSA-N 0.000 claims description 6
- ARIWANIATODDMH-UHFFFAOYSA-N Lauric acid monoglyceride Natural products CCCCCCCCCCCC(=O)OCC(O)CO ARIWANIATODDMH-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 6
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- 238000009413 insulation Methods 0.000 claims description 5
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- KTHUKEZOIFYPEH-UHFFFAOYSA-N 1-benzylnaphthalene Chemical compound C=1C=CC2=CC=CC=C2C=1CC1=CC=CC=C1 KTHUKEZOIFYPEH-UHFFFAOYSA-N 0.000 claims description 4
- 229920002907 Guar gum Polymers 0.000 claims description 4
- OJGMBLNIHDZDGS-UHFFFAOYSA-N N-Ethylaniline Chemical compound CCNC1=CC=CC=C1 OJGMBLNIHDZDGS-UHFFFAOYSA-N 0.000 claims description 4
- 239000013543 active substance Substances 0.000 claims description 4
- 150000001448 anilines Chemical class 0.000 claims description 4
- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical class CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- 239000000665 guar gum Substances 0.000 claims description 4
- 235000010417 guar gum Nutrition 0.000 claims description 4
- 229960002154 guar gum Drugs 0.000 claims description 4
- 229920000223 polyglycerol Polymers 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 4
- VQIRFOAILLIZOY-UHFFFAOYSA-N 2-[5-acetamido-n-(2-acetyloxyethyl)-4-[(2-bromo-4,6-dinitrophenyl)diazenyl]-2-ethoxyanilino]ethyl acetate Chemical compound C1=C(N(CCOC(C)=O)CCOC(C)=O)C(OCC)=CC(N=NC=2C(=CC(=CC=2Br)[N+]([O-])=O)[N+]([O-])=O)=C1NC(C)=O VQIRFOAILLIZOY-UHFFFAOYSA-N 0.000 claims description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N acrylic acid methyl ester Natural products COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 3
- 238000005829 trimerization reaction Methods 0.000 claims description 3
- 239000000230 xanthan gum Substances 0.000 claims description 3
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- 235000010493 xanthan gum Nutrition 0.000 claims description 3
- 229940082509 xanthan gum Drugs 0.000 claims description 3
- JSRUDOBCTLPTFO-UHFFFAOYSA-N 2-[5-acetamido-n-(2-acetyloxyethyl)-4-[(2-bromo-4,6-dinitrophenyl)diazenyl]-2-methoxyanilino]ethyl acetate Chemical compound C1=C(N(CCOC(C)=O)CCOC(C)=O)C(OC)=CC(N=NC=2C(=CC(=CC=2Br)[N+]([O-])=O)[N+]([O-])=O)=C1NC(C)=O JSRUDOBCTLPTFO-UHFFFAOYSA-N 0.000 claims 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 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 2
- 229920001732 Lignosulfonate Polymers 0.000 claims description 2
- 235000019357 lignosulphonate Nutrition 0.000 claims description 2
- CIPVVROJHKLHJI-UHFFFAOYSA-N n,n-diethyl-3-methylaniline Chemical compound CCN(CC)C1=CC=CC(C)=C1 CIPVVROJHKLHJI-UHFFFAOYSA-N 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims 1
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- CULIYQPRUGMRRT-UHFFFAOYSA-N 2-chloro-n-[2-[(2-cyano-4-nitrophenyl)diazenyl]-5-(diethylamino)phenyl]acetamide Chemical compound ClCC(=O)NC1=CC(N(CC)CC)=CC=C1N=NC1=CC=C([N+]([O-])=O)C=C1C#N CULIYQPRUGMRRT-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides an aftertreatment method for a liquid disperse dye. The aftertreatment method for the liquid disperse dye comprises the following steps: adding water to dissolve a filter cake containing the liquid disperse dye, which is obtained by diazotization, coupling and filtering, to obtain slurry with a solid content of 30 to 50 percent; adding polyglyceryl fatty acid ester surfactants of which the mass is 0.1 to 10 percent of that of the slurry and phenyl amines compounds of which the mass is 0.2 to 2 percent of that of the slurry; stirring and pulping for 1 to 5 hours; raising the temperature to between 80 and 110 DEG C and keeping the temperature for 1 to 7 hours; cooling to the normal temperature; adding a dispersing agent or dispersing agent of which the mass is 0.3 to 1 time of that of the dry weight of the filter cake; performing particle processing for 1 to 10 hours by a breaking device, and obtaining slurry; adding a thickening agent of which the mass is 0.1 to 0.3 percent of that of the slurry to the slurry with stirring; continuing to stir for 1 to 2 hours after finishing material addition; and filtering to obtain the liquid disperse dye. The method for preparing the liquid disperse dye has the advantages of low cost, simple operation, active role in environmental protection, and greater economic and social benefits.
Description
(1) technical field
The present invention relates to a kind of post-treating method of liquid dispersion dyestuff.
(2) background technology
The liquid dispersion dyestuff refers to the dispersed dye that liquid form exists, the liquid dispersion dyestuff has many good qualities than pulvis, slurry agent and granula, use the dispersion agent than the pulvis much less can reach good dispersion effect such as (1) liquid dispersion dyestuff, and because too much dispersion agent can limit the migration of dye particles when dyeing, therefore the high characteristics of dye utilization rate when liquid dyes has dyeing; (2) save spray-drying process, thereby saved the energy; (3) be convenient to automated operation, such as the use of various fluid conveying machines; Do not need specific installation when (4) dissolving, get final product diluting soln with cold water, avoided the disadvantages such as color dot that cause because of the dyestuff solubilizing poorly in dyeing or the stamp process; Do not have dust when (5) using, can improve working conditions, realize cleaner production etc.
But traditional liquid dispersion dyestuff quality guaranteed period is short, especially summer, is easy to occur sedimentation, has brought a lot of troubles for transportation and storage.
(3) summary of the invention
The object of the present invention is to provide a kind of particularly aftertreatment of the liquid dispersion dyestuff of trevira dyeing and stamp of hydrophobic fiber that is applicable to, more stable according to the liquid dispersion dyestuff that the method is prepared, even sedimentation can not occur at hot weather yet, thereby prolonged the quality guaranteed period, made things convenient for transportation and the storage of dyestuff.
The technical solution used in the present invention is:
A kind of post-treating method of liquid dispersion dyestuff, described method comprises:
The dispersed dye filter cake that (1) will obtain through diazotization, coupling, filtration according to a conventional method is dissolved in water, obtaining solid content is the slurries of 30%～50% (preferred 35%～45%), the adding quality is that polyglycerol fatty acid ester class tensio-active agent and the quality of slurries quality 0.1%～10% (preferred 0.2%～5%) is the amino benzenes compounds of slurries quality 0.2%～2%, stirring to pulp 1～5 hour is warming up to 80～110 ℃ of insulations 1～7 hour;
Described polyglycerol fatty acid ester class tensio-active agent is one of following or two or more mixture wherein: trimerization glycerol laurate, four Polyglycerine laurates, six Polyglycerine laurates, Tripolyglycerol monostearates, three Unigly GO 102Ss;
Described amino benzenes compounds is one of following or two or more mixture wherein: aniline, N, N-Diethyl Aniline, N, N-diethyl-m-toluidine, N-ethylaniline;
(2) step (1) gained slurries are cooled to normal temperature, adding quality is dispersion agent or the diffusant of 0.3～1 times of filter cake dry weight, carries out corpusculed with shredding unit and processes 1～10 hour, obtains slurry; Need 4 grades of diffustivitys of test or more than, control slurry coloured light, intensity, and spot qualified;
Different dispersed dye, the abrasive particles treatment time is also different, as long as diffustivity reaches 4 grades or above just passable, is generally 1～10 hour.Described diffusion adopts filter paper to ooze the circle method and measures, and the mensuration of dye shade and intensity can be carried out according to GB/T2394.Described spot test can be passed judgment on by the mensuration of dyestuff tar residual quantity, method is as follows: be poured on the filter paper after the drying through the slurry liquid of heating with not heating above-mentioned, if be tiny irregular black splotch on the filter paper, namely can be considered the impurity such as tar, on the contrary, if present the color and luster of uniformity on the filter paper, do not produce the spot color dot, namely spot is qualified.
(3) stir down, adding quality in step (2) slurry is the thickening material of stock quality 0.1%～0.3%, reinforced complete after, continue to stir 1～2 hour, filtration gets the liquid dispersion dyestuff.
In the post-treating method of described liquid dispersion dyestuff, the dispersed dye that adopt are the common kind in this area, can be single dispersed dye, also can be the disperse dye compositions after mixed the assembly, for the mixed dispersed dye of piecing together, the dispersed dye filter cake of different varieties can be used water dissolution together; Also can be that each dispersed dye are finished the again row mixing of disposed slurry liquid according to step (1); Can also be each dispersed dye remix after the processing of abrasive particles.In the aftertreatment technology of liquid dispersion dyestuff of the present invention, the dispersed dye that adopt are preferably one of following or two or more mixture wherein: the C.I. Disperse Blue-79, C.I. Disperse Blue-79: 1, C.I. EX-SF DISPERSE BLUE EX-SF 300 291, C.I. EX-SF DISPERSE BLUE EX-SF 300 291:1, C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93, C.I. EX-SF DISPERSE BLUE EX-SF 300 93:1, C.I. DISPERSE ORANGE 30 200 30, C.I. Red 167, C.I. DISPERSE ORANGE 30 200 288 or C.I. DISPERSE ORANGE 30 200 61.
Described dispersion agent or diffusant are conventional dispersion agent or the diffusant that is used for dispersed dye in this area, are preferably one of following or two or more mixture wherein: naphthalene sulfonic acidformaldehyde condensation product, sulfonated lignin, alkyl naphthalene sulfonic acid formaldehyde condensation products, benzyl naphthalene sulfonic formaldehyde condensation compound.
Preferably, described dispersion agent or diffusant are one of following or two or more mixture wherein: condensation compound of methyl naphthalene sulfonic acid and formaldehyde (Dispersant MF), naphthalene sulfonic acidformaldehyde condensation product (dispersing agent NNO), benzyl naphthalene sulfonic formaldehyde condensation compound (dispersing agent CNF), sodium lignosulfonate (xylogen 85A, 83A).
Thickening material described in the step (3) is the conventional thickening material that is used for dispersed dye in this area, it can be methyl acrylate compound, it also can be natural biological, be preferably one of following or two or more mixture wherein: methyl acrylate compound, xanthan gum or guar gum, feeding mode is for slowly adding gradually.
Preferably, be filtered into described in the step (3) through 300 order Double-layer screens and filter.
Preferably, shredding unit is shredder or sand mill described in the step (2).
Resulting liquid disperse dye in the described step (3), its viscosity can reach (10 ℃) 50～200mpa.s.The testing method of viscosity can be carried out according to GB/T21882.
The liquid dispersion dyestuff that adopts the method for the invention to prepare has the not characteristics such as free settling, good stability, even in hot environment, also can guarantee the quality more than 6 months; When the liquid dispersion dyestuff finished product that obtains is applied to print and dye, directly use behind the thin up, do not have dust, work light, be convenient to automatization, that colour fastness is high, form and aspect are stable, while is save energy widely, shortens the production cycle, raises labour productivity, improve work situation, reduce the three wastes, reduce the cost, suitable applying.
Beneficial effect of the present invention is mainly reflected in: adopt the inventive method to prepare the liquid dispersion dyestuff, cost is low, simple to operate, and protection of the environment is played a positive role, and has larger economic benefit and social benefit.
(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:
Embodiment 1:
1, in the four-hole boiling flask with condenser, thermometer, agitator and charging opening, add C.I. EX-SF DISPERSE BLUE EX-SF 300 B291 filter cake 70g (dry weight), C.I. DISPERSE ORANGE 30 200 61 filter cake 20g (dry weight), C.I. 63 DISPERSE Violet 63 93:1 filter cake 10g (dry weight) and 150g water, add again 5g Tripolyglycerol monostearates and 1g aniline, stirring to pulp 2 hours is warmed up to 95 ℃～100 ℃, and insulation was slowly stirred 3 hours;
2, with resulting slurry liquid cool to room temperature in the step 1, add 60g sodium lignosulfonate and 20g dispersing agent NNO, add water management slurry liquid solid content 45%, ground 5 hours with sand mill, obtain slurry, detect its diffustivity reach 4 grades or more than, the coloured light, intensity of control slurry, and spot qualified;
3, slurry qualified in the step 2 is transferred in the flask with agitator and charging opening, is slowly added while stirring the 0.8g guar gum, feed intake finish after restir 1～2 hour;
4, the slurry with step 3 gained filters through 300 order Double-layer screens, obtains the liquid dispersion dyestuff, and its viscosity is (10 ℃) 125mpa.s.
Embodiment 2:
1, in the four-hole boiling flask with condenser, thermometer, agitator and charging opening, add C.I. Red 167 filter cake 100g (dry weight) and 150g water, add again 3g Tripolyglycerol monostearates and 1g aniline, stirring to pulp 2 hours, be warmed up to 95 ℃～100 ℃, insulation was slowly stirred 3 hours;
2, the slurries cool to room temperature of gained in the step 1 adds 30g Dispersant MF and 30g xylogen 85A, adds water management slurry liquid solid content 39%, grinds 4 hours with sand mill, obtains slurry, detect its diffustivity reach 4 grades or more than; The coloured light, intensity of control slurry, and spot qualified;
3, slurry qualified in the step 2 is moved on in the flask with agitator and charging opening, slowly adds while stirring the xanthan gum after the 0.9g modification, feed intake finish after restir 1～2 hour;
4, the slurry with step 3 gained filters through 300 order Double-layer screens, filters through 300 order Double-layer screens, obtains the liquid dispersion dyestuff, and its viscosity is (10 ℃) 135mpa.s.
Embodiment 3:
1, in the four-hole boiling flask with condenser, thermometer, agitator and charging opening, add C.I. Disperse Blue-79 filter cake 41.5g (dry weight), C.I. DISPERSE ORANGE 30 200 44 filter cake 49.1g (dry weight), C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93 filter cake 9.4g (dry weight) and 150g water, add again 5g trimerization glycerol laurate and 1gN, N-Diethyl Aniline, stirring to pulp 2 hours, be warmed up to 95 ℃～100 ℃, insulation was slowly stirred 3 hours;
2, with resulting slurry liquid cool to room temperature in the step 1, add the 80g sodium lignosulfonate, add water management slurry liquid solid content 42%, ground 5 hours with sand mill, obtain slurry, detect its diffustivity reach 4 grades or more than, the coloured light, intensity of control slurry, and spot qualified;
3, slurry qualified in the step 2 is transferred in the flask with agitator and charging opening, is slowly added while stirring the 1g guar gum, feed intake finish after restir 1～2 hour;
4, the slurry with step 3 gained filters through 300 order Double-layer screens, obtains the liquid dispersion dyestuff, and its viscosity is (10 ℃) 120mpa.s.
Stability test: the liquid dye that embodiment 1, embodiment 2 make were stored 6 months at 0～50 ℃, and whether have layering, flocculation, crystal separate out, the results are shown in following table 1 if observing these liquid dye:
Table 1
| Embodiment | Solid content % | January | February | March |
| Example 1 | 41 | Nothing | Nothing | Nothing |
| Example 2 | 39 | Nothing | Nothing | Nothing |
| Example 3 | 42 | Nothing | Nothing | Nothing |
From the above results as can be known, according to the method for the invention preparation, the liquid dispersion dye stability that obtains is good, is difficult for sedimentation occurs, and can guarantee the quality more than 6 months 0 ℃～50 ℃ of temperature.
Claims (6)
1. the post-treating method of a liquid dispersion dyestuff, described method comprises:
(1) will obtain the dispersed dye filter cake through diazotization, coupling, filtration is dissolved in water, obtain solid content and be 30% ~ 50% slurries, the adding quality is that polyglycerol fatty acid ester class tensio-active agent and the quality of slurries quality 0.1% ~ 10% is the amino benzenes compounds of slurries quality 0.2% ~ 2%, stirring to pulp 1 ~ 5 hour is warming up to 80 ~ 110 ℃ of insulations 1 ~ 7 hour;
Described polyglycerol fatty acid ester class tensio-active agent is one of following or two or more mixture wherein: trimerization glycerol laurate, four Polyglycerine laurates, six Polyglycerine laurates, Tripolyglycerol monostearates, three Unigly GO 102Ss;
Described amino benzenes compounds is one of following or two or more mixture wherein: aniline, N, N-Diethyl Aniline, N, N-diethyl-m-toluidine, N-ethylaniline;
Described liquid dispersion dyestuff is one of following or two or more mixture wherein: C.I. Disperse Blue-79, C.I. Disperse Blue-79: 1, C.I. EX-SF DISPERSE BLUE EX-SF 300 291, C.I. EX-SF DISPERSE BLUE EX-SF 300 291:1, C.I. 63 ,DIS,PER,SE ,Vio,let, 63 93, C.I. EX-SF DISPERSE BLUE EX-SF 300 93:1, C.I. Red 167, C.I. DISPERSE ORANGE 30 200 61;
(2) step (1) gained slurries are cooled to normal temperature, adding quality is dispersion agent or the diffusant of 0.3 ~ 1 times of filter cake dry weight, carries out corpusculed with shredding unit and processes 1 ~ 10 hour, obtains slurry;
(3) stir down, adding quality in step (2) slurry is the thickening material of stock quality 0.1% ~ 0.3%, reinforced complete after, continue to stir 1 ~ 2 hour, filtration gets the liquid dispersion dyestuff.
2. the method for claim 1 is characterized in that dispersion agent described in the step (2) or diffusant are one of following or two or more mixture wherein: naphthalene sulfonic acidformaldehyde condensation product, sulfonated lignin, alkyl naphthalene sulfonic acid formaldehyde condensation products, benzyl naphthalene sulfonic formaldehyde condensation compound.
3. method as claimed in claim 2 is characterized in that described dispersion agent or diffusant are one of following or two or more mixture wherein: condensation compound of methyl naphthalene sulfonic acid and formaldehyde, naphthalene sulfonic acidformaldehyde condensation product, benzyl naphthalene sulfonic formaldehyde condensation compound, sodium lignosulfonate.
4. the method for claim 1 is characterized in that thickening material described in the step (3) is one of following or two or more mixture wherein: methyl acrylate compound, xanthan gum or guar gum.
5. the method for claim 1 is characterized in that being filtered into described in the step (3) through 300 order Double-layer screens and filters.
6. the method for claim 1 is characterized in that shredding unit is shredder or sand mill described in the step (2).
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| CN 200910155193 CN101724298B (en) | 2009-12-08 | 2009-12-08 | Aftertreatment method for liquid disperse dye |
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| CN 200910155193 CN101724298B (en) | 2009-12-08 | 2009-12-08 | Aftertreatment method for liquid disperse dye |
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| CN101724298B true CN101724298B (en) | 2013-04-24 |
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| CN104497629B (en) * | 2014-12-31 | 2017-09-22 | 浙江闰土股份有限公司 | Yellow liquid disperse dyes and its preparation method and purposes |
| CN104497631B (en) * | 2014-12-31 | 2017-06-06 | 浙江闰土股份有限公司 | Blue liquid disperse dyes and its preparation method and purposes |
| CN104530763B (en) * | 2014-12-31 | 2017-10-27 | 浙江闰土染料有限公司 | Blue liquid disperse dyes and its preparation method and purposes |
| CN104530761B (en) * | 2014-12-31 | 2017-06-23 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
| CN104448933B (en) * | 2014-12-31 | 2017-07-07 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
| CN104530760B (en) * | 2014-12-31 | 2017-06-23 | 浙江闰土股份有限公司 | Red liquid disperse dyes and its preparation method and purposes |
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