WO2015101290A1 - 一种分散染料组合物、分散染料及其的制备方法和用途 - Google Patents

一种分散染料组合物、分散染料及其的制备方法和用途 Download PDF

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Publication number
WO2015101290A1
WO2015101290A1 PCT/CN2014/095585 CN2014095585W WO2015101290A1 WO 2015101290 A1 WO2015101290 A1 WO 2015101290A1 CN 2014095585 W CN2014095585 W CN 2014095585W WO 2015101290 A1 WO2015101290 A1 WO 2015101290A1
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Prior art keywords
component
formula
disperse dye
weight percentage
dye
Prior art date
Application number
PCT/CN2014/095585
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English (en)
French (fr)
Inventor
赵国生
阮海兴
顾伟娣
陈百龙
叶华明
景雪苹
Original Assignee
浙江闰土股份有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Priority claimed from CN201310751841.1A external-priority patent/CN104371369B/zh
Priority claimed from CN201310752449.9A external-priority patent/CN104371362B/zh
Priority claimed from CN201310751747.6A external-priority patent/CN104371360B/zh
Priority claimed from CN201310751286.2A external-priority patent/CN104371358B/zh
Priority claimed from CN201310751296.6A external-priority patent/CN104371359B/zh
Priority claimed from CN201310753630.1A external-priority patent/CN104371365B/zh
Priority claimed from CN201310753414.7A external-priority patent/CN104371364B/zh
Priority claimed from CN201310753365.7A external-priority patent/CN104371370B/zh
Priority to BR112016012058A priority Critical patent/BR112016012058B8/pt
Priority to KR1020167020366A priority patent/KR101702513B1/ko
Priority to ES14876649.6T priority patent/ES2653737T3/es
Application filed by 浙江闰土股份有限公司 filed Critical 浙江闰土股份有限公司
Priority to EP14876649.6A priority patent/EP3147333B1/en
Priority to US15/102,669 priority patent/US10151062B2/en
Publication of WO2015101290A1 publication Critical patent/WO2015101290A1/zh

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Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/16General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
    • D06P1/19Nitro dyes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0033Blends of pigments; Mixtured crystals; Solid solutions
    • C09B67/0046Mixtures of two or more azo dyes
    • C09B67/0051Mixtures of two or more azo dyes mixture of two or more monoazo dyes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/16General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
    • D06P1/18Azo dyes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/34Material containing ester groups
    • D06P3/52Polyesters
    • D06P3/54Polyesters using dispersed dyestuffs

Definitions

  • the present invention relates to a disperse dye composition, a disperse dye, and a process for the preparation thereof and use thereof.
  • the disperse dyes are suitable for dyeing and printing fabrics, especially polyester and blended fabrics thereof.
  • the invention provides an economical and environment-friendly disperse dye with wide pH range, good light fastness, excellent compatibility, high strength and good washing fastness.
  • the present invention provides a disperse dye composition comprising or consisting of the following components:
  • X 1 is bromine or chlorine; and R 1 and R 2 are each independently a C 1 -C 4 alkyl group;
  • X 3 and X 4 are each independently hydrogen, chlorine or bromine, and R 5 and R 6 are each independently a C 2 -C 4 alkyl group, or one of the C 1 -C 4 alkyl groups is a cyano, phenyl, acetoxy or benzoyloxy substituted group; wherein component D is not CI dispersed orange 76;
  • each of X 5 and X 6 is independently hydrogen, chlorine or a nitro group, and R 7 is an alkyl group of C 1 to C 4 ;
  • X 7 and X 8 are each independently a bromine, a chlorine, a cyano group or a nitro group, and R 8 is a C 1 -C 4 alkanoylamino group or a C 1 -C 4 alkyl group, R 9 and R 10 each independently is a C 1 -C 4 alkyl group, and R 11 is hydrogen or a C 1 -C 4 alkoxy group;
  • X 7 is a cyano group or a nitro group
  • X 8 is a cyano group
  • R 11 is hydrogen
  • X 2 in the formula (3) is chlorine
  • X 7 in the formula (6) is a cyano group or a nitro group
  • X 8 is a cyano group
  • R 11 is hydrogen
  • component C is a compound represented by formula (3-1) and (3-2):
  • component B is a compound represented by formula (2-1):
  • Component C is a compound represented by formula (3-2):
  • each of X 3 and X 4 is independently hydrogen or bromine
  • each of X 7 and X 8 is independently a bromine, a cyano group or a nitro group.
  • the component B is one or both of the following compounds:
  • the component C is one or more of the following compounds:
  • the component C is one or more of the following compounds:
  • the component D is one or more of the following compounds:
  • the component E is one or more of the following compounds:
  • the component F is one or more of the following compounds:
  • the component F is one or more of the following compounds:
  • the component F is one or more of the following compounds:
  • component B is one or both of the compounds represented by formula (2-1) and formula (2-2):
  • Component C is one or more of the compounds represented by the following formulas (3-1) to (3-4):
  • component B is one or both of the compounds represented by formula (2-1) and formula (2-2):
  • Component C is one or both of the compounds represented by the following formulas (3-1) and (3-4):
  • the disperse dye composition according to the invention preferably, based on the total weight of the composition, comprises:
  • Component A with a weight percentage of 2 to 73%
  • Component B with a weight percentage of 7 to 40%
  • Component C with a weight percentage of 20 to 58%
  • component G is from 0 to 47% by weight.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 3 to 50%.
  • Component B has a weight percentage of 12 to 39%.
  • Component C has a weight percentage of 38 to 58%.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 60%.
  • Component B has a weight percentage of 7 to 37%
  • Component C has a weight percentage of 30 to 55%.
  • Component D has a weight percentage of from 3 to 6%.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 3 to 6%.
  • Component B has a weight percentage of 12 to 37%.
  • Component C has a weight percentage of 35 to 55%.
  • Component D has a weight percentage of 2 to 50%.
  • the disperse dye composition according to the present invention is preferably characterized in that, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 51%.
  • Component B has a weight percentage of 12 to 37%.
  • Component C has a weight percentage of 35 to 55%.
  • the weight percentage of component E is from 2 to 6%.
  • the disperse dye composition according to the present invention is preferably characterized in that, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 72%.
  • Component B has a weight percentage of 7 to 40%
  • Component C has a weight percentage of 20 to 48%.
  • the weight percentage of component F is from 1 to 10%.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 72%.
  • Component B has a weight percentage of 7 to 40%
  • Component C has a weight percentage of 20 to 48%.
  • the weight percentage of component G is from 1 to 10%.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 71%.
  • Component B has a weight percentage of 7 to 40%
  • Component C has a weight percentage of 20 to 48%.
  • Component E has a weight percentage of 1 to 5%.
  • Component G has a weight percentage of from 1 to 5%.
  • the disperse dye composition according to the present invention preferably, based on the total weight of the composition,
  • Component A has a weight percentage of 2 to 71%.
  • Component B has a weight percentage of 7 to 40%
  • Component C has a weight percentage of 20 to 48%.
  • Component E has a weight percentage of 1 to 5%.
  • Component F has a weight percentage of from 1 to 5%.
  • the various dye components of the present invention may generally carry some by-products and other impurities, provided that they do not interfere with the practice of the present invention.
  • the present invention provides a disperse dye comprising the disperse dye composition and excipient of the present invention.
  • the disperse dye of the present invention comprises an auxiliary agent and water.
  • the disperse dye according to the present invention which comprises one or a combination of two or more of the following: a naphthalene sulfonic acid formaldehyde condensate, a lignosulfonate, sodium sulfate, a surfactant, a bactericide, or the like.
  • Dye dispersant which comprises one or a combination of two or more of the following: a naphthalene sulfonic acid formaldehyde condensate, a lignosulfonate, sodium sulfate, a surfactant, a bactericide, or the like.
  • Dye dispersant which comprises one or a combination of two or more of the following: a naphthalene sulfonic acid formaldehyde condensate, a lignosulfonate, sodium sulfate, a surfactant, a bactericide, or the like.
  • the disperse dye of the present invention has a weight ratio of the auxiliary agent to the disperse dye composition of from 0.3 to 4:1.
  • the disperse dye is liquid after being ground by a sand mill or a grinder, and has a solid content of 20 to 50%, or the disperse dye is powdery or granular after spray drying, and the solid content is 87 to 96%.
  • the invention also provides a method of preparing a disperse dye according to the invention comprising the steps of:
  • the particles After mixing the dye components, the particles are treated by a sand mill or a grinder in the presence of an auxiliary material; or the dye components are separately particleized by a sand mill or a grinder in the presence of an auxiliary material. Process and mix again.
  • the invention also provides the use of a disperse dye according to the invention for dyeing and printing fabrics.
  • the present invention also provides a fabric which is prepared by dyeing and printing using a disperse dye according to the present invention.
  • the disperse dye of the invention has excellent light fastness, wide application range of pH value, good compatibility between components, high strength, low printing and dyeing cost, good washing fastness, and formula (2), (3) (4), (6) When chlorine is not contained, only Ouko-Tex Standard 100 (2013) Class I is required.
  • the disperse dye composition according to the present invention based on the total weight of the composition, comprises:
  • Component A having a weight percentage of 2 to 73%, preferably 2 to 72%, more preferably 2 to 71%, still more preferably 2 to 60%, still more preferably 2 to 51%, still more preferably 3 to 50% More preferably, it is 3 to 6%;
  • Component B having a weight percentage of 7 to 40%, preferably 7 to 37% or 12 to 39%, more preferably 12 to 37%;
  • Component C having a weight percentage of 20 to 58%, preferably 30 to 55% or 20 to 48%, more preferably 38 to 58% or 35 to 55%;
  • the weight percentage is from 0 to 70% of component D, preferably from 2 to 50%, more preferably from 3 to 6%;
  • the weight percentage is from 0 to 10% of component E, preferably from 2 to 6%, more preferably from 1 to 5%;
  • the weight percentage is from 0 to 47% of component F, preferably from 1 to 10%, more preferably from 1 to 5%;
  • the optional weight percentage is from 0 to 47% of component G, preferably from 1 to 10%, more preferably from 1 to 5%.
  • the weight percentage of the compound represented by the formula (3-1) is 1 to 99%, preferably 70 to 90%, and the compound represented by the formula (3-2) is from 1 to 99% by weight, preferably from 10 to 30% by weight.
  • the components A, B, C and the optional components D, E, F, G of the present invention are mixed with the auxiliary agent and water according to a certain ratio, and then ground and dispersed by a sand mill. The slurry is formed or further spray-dried to prepare a dye.
  • the components A, B, C, D, E, F, G are all known dye compounds and are commercially available or can be prepared by existing methods.
  • Example 1 was repeated except that the dye component of the formula (1) of Example 1 was replaced with the dye component of the following formula (8).
  • Example 1 The dye preparations of Example 1 and Comparative Example 1 were subjected to performance tests.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Example 1 and Comparative Example 1 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • High strength means that textiles of the same depth can reduce the amount of dye and reduce the printing cost when printing.
  • Example 2 was repeated except that the dye component of the formula (1) of Example 2 was replaced with the dye component of the following formula (9).
  • Example 2 The dye preparations of Example 2 and Comparative Example 2 were subjected to performance tests.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Example 2 and Comparative Example 2 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the polyester fiber was subjected to high temperature and high pressure dyeing, and the temperature was raised to 130 ° C in 35 minutes, held for 45 minutes, and cooled to 80 ° C for sampling.
  • Example 3 was repeated except that the dye component of the formula (1) of Example 3 was replaced with the dye component of the formula (4-1).
  • Example 3 The dye preparations of Example 3 and Comparative Example 3 were subjected to performance tests.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Example 3 and Comparative Example 3 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the method for determining compatibility is as follows: dyeing according to GB/T2394-2003, dyeing from 60 ° C, taking a sample immediately when the temperature is raised to 80 ° C, and then taking a sample every 10 ° C until 130 ° C, and Samples were taken at 130 ° C for 10 minutes, 20 minutes, 30 minutes, and 50 minutes, and a total of 10 swatches were taken. The sample was kept at 130 ° C for 50 minutes, and the sample of each temperature was taken as a sample to observe whether the hue change was synchronized. It is divided into five grades I, II, III, IV, V (instrument: computer colorimeter datacolor 600, color difference formula CMC 2:1). For the black color, the number of cloth samples in which DC (dampness difference) and DH (hue difference) are less than 0.6 are calculated.
  • Level I five and more than five
  • Class V one piece.
  • Example 4 was repeated except that the dye component of the formula (1) of Example 4 was replaced with the dye component of the following formula (10).
  • Example 4 The dye preparations of Example 4 and Comparative Example 4 were subjected to performance tests.
  • 0.5 g of the dyes of Example 4 and Comparative Example 4 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 5 was repeated except that 44 g of the dye component of formula (1) in Example 5 was replaced with 41.4 g of the dye component of formula (10) and 2.6 g of the dye component of formula (11).
  • Example 5 The dye preparations of Example 5 and Comparative Example 5 were subjected to performance tests.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Example 5 and Comparative Example 5 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Pipette 10ml of disperse dye suspension with Mix 90ml of water adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep for 45 minutes, cool to 80 °C sampling.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 6 was repeated except that the dye component of the formula (1) in Example 6 was replaced with the dye component of the formula (8).
  • Example 6 The dye preparations of Example 6 and Comparative Example 6 were subjected to performance tests.
  • 0.5 g of the dyes of Example 6 and Comparative Example 6 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 7 and Example 8 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the dye product was obtained in the same manner as in Example 6 in accordance with the composition formula in Table 9.
  • the finished dye product of Example 9 was subjected to performance testing.
  • 0.5 g of the dye of Example 9 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • the swatch color was observed and its light fastness was measured by the method of AATCC 16-2004. The results are shown in Table 10.
  • the dye product was obtained in the same manner as in Example 6 in accordance with the composition formula in Table 11.
  • 0.5 g of the dye of Examples 10-15 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 16 and 17 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • composition formula in Table 15 an appropriate amount of auxiliary agent was added to prepare a dye product.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 18 to 38 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • composition formula in Table 17 an appropriate amount of auxiliary agent was added to prepare a dye product.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 39 to 43 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • Example 44 was repeated except that the dye component of the formula (1) of Example 44 was replaced with the dye component of the following formula (8).
  • Example 44 The dye preparations of Example 44 and Comparative Example 44 were subjected to performance tests.
  • Example 44 0.5 g of the dyes of Example 44 and Comparative Example 44 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • High strength means that textiles of the same depth can reduce the amount of dye and reduce the printing cost when printing.
  • Example 45 was repeated except that the dye component of the formula (1) of Example 45 was replaced with the dye component of the following formula (9).
  • Example 45 The dye preparations of Example 45 and Comparative Example 45 were subjected to performance tests.
  • Example 45 0.5 g of the dyes of Example 45 and Comparative Example 45 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 46 was repeated except that the dye component of the formula (1) of Example 46 was replaced with the dye component of the formula (4-1).
  • Example 46 The dye preparations of Example 46 and Comparative Example 46 were subjected to performance tests.
  • Example 46 and Comparative Example 46 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the method for determining compatibility is as follows: dyeing according to GB/T2394-2003, dyeing from 60 ° C, taking a sample immediately when the temperature is raised to 80 ° C, and then taking a sample every 10 ° C until 130 ° C, and Samples were taken at 130 ° C for 10 minutes, 20 minutes, 30 minutes, and 50 minutes, and a total of 10 swatches were taken. The sample was kept at 130 ° C for 50 minutes, and the sample of each temperature was taken as a sample to observe whether the hue change was synchronized. It is divided into five grades I, II, III, IV, V (instrument: computer colorimeter datacolor 600, color difference formula CMC 2:1). For the black color, the number of cloth samples in which DC (dampness difference) and DH (hue difference) are less than 0.6 are calculated.
  • Level I five and more than five
  • Class V one piece.
  • Example 47 was repeated except that the dye component of the formula (1) of Example 47 was replaced with the dye component of the following formula (10).
  • Example 47 The dye preparations of Example 47 and Comparative Example 47 were subjected to performance tests.
  • Example 47 0.5 g of the dyes of Example 47 and Comparative Example 47 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 48 was repeated except that 44 g of the dye component of formula (1) in Example 48 was replaced with 41.4 g of the dye component of formula (10) and 2.6 g of the dye component of formula (11).
  • Example 48 The dye preparations of Example 48 and Comparative Example 48 were subjected to performance tests.
  • Example 48 0.5 g of the dyes of Example 48 and Comparative Example 48 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Pipette 10ml disperse dye suspension Mix with 90ml of water, adjust the pH of the dye bath to 5 with acetic acid, then raise the temperature to 60 ° C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 ° C in 35 minutes, keep for 45 minutes, cool to 80 Sampled at °C.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 49 was repeated except that the dye component of the formula (1) in Example 49 was replaced with the dye component of the formula (8).
  • Example 49 The dye products of Example 49 and Comparative Example 49 were subjected to performance tests.
  • Example 49 0.5 g of the dyes of Example 49 and Comparative Example 49 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • 2 g of polyester fiber was subjected to high temperature and high pressure dyeing, and the temperature was raised to 130 ° C in 35 minutes, kept for 45 minutes, and cooled to 80 ° C for sampling.
  • Example 50 was repeated except that the dye component of the formula (3-1) in Example 50 was replaced with the dye component of the following formula (12).
  • Example 50 The dye preparations of Example 50 and Comparative Example 50 were subjected to performance tests.
  • 0.5 g of the dyes of Example 50 and Comparative Example 50 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 51 was repeated except that 54 g of the dye component of formula (3-1) in Example 51 was replaced with a mixture of 27 g of the dye component of formula (12) and 27 g of the dye component of formula (3-1). Others remain unchanged.
  • Example 51 The dye preparations of Example 51 and Comparative Example 51 were subjected to performance tests.
  • Example 51 0.5 g of the dyes of Example 51 and Comparative Example 51 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the finished dye was prepared in accordance with the method of Example 51.
  • Example 52 and Example 53 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the finished dye product was prepared in accordance with the method of Example 51.
  • the finished dye product of Example 54 was subjected to performance testing.
  • 0.5 g of the dye of Example 54 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • the swatch color was observed and its light fastness was measured by the method of AATCC 16-2004. The results are shown in Table 30.
  • the finished dye was prepared in accordance with the method of Example 51.
  • 0.5 g of the dyes of Examples 55 and 56 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • 0.5 g of the dyes of Examples 57-64 were weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • 0.5 g of the dyes of Examples 65 and 66 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • 0.5 g of the dye of Examples 67-92 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • Example 93 was repeated except that the dye component of the formula (1) of Example 93 was replaced with the dye component of the following formula (8).
  • Example 93 The dye products of Example 93 and Comparative Example 93 were subjected to performance tests.
  • Example 93 and Comparative Example 93 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • High strength means that textiles of the same depth can reduce the amount of dye and reduce the printing cost when printing.
  • Example 94 was repeated except that the dye component of the formula (1) of Example 94 was replaced with the dye component of the following formula (9).
  • Example 94 The finished dyes of Example 94 and Comparative Example 94 were subjected to performance testing.
  • Example 94 and Comparative Example 94 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 95 was repeated except that the dye component of the formula (1) of Example 95 was replaced with the dye component of the formula (4-1).
  • Example 95 The dye preparations of Example 95 and Comparative Example 95 were subjected to performance tests.
  • Example 95 0.5 g of the dyes of Example 95 and Comparative Example 95 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the method for determining compatibility is as follows: dyeing according to GB/T2394-2003, dyeing from 60 ° C, taking a sample immediately when the temperature is raised to 80 ° C, and then taking a sample every 10 ° C until 130 ° C, and Samples were taken at 130 ° C for 10 minutes, 20 minutes, 30 minutes, and 50 minutes, and a total of 10 swatches were taken. The sample was kept at 130 ° C for 50 minutes, and the sample of each temperature was taken as a sample to observe whether the hue change was synchronized. It is divided into five grades I, II, III, IV, V (instrument: computer colorimeter datacolor 600, color difference formula CMC 2:1). For the black color, the number of cloth samples in which DC (dampness difference) and DH (hue difference) are less than 0.6 are calculated.
  • Level I five and more than five
  • Class V one piece.
  • Example 96 was repeated except that the dye component of the formula (1) of Example 96 was replaced with the dye component of the following formula (10).
  • Example 96 The finished dyes of Example 96 and Comparative Example 96 were subjected to performance testing.
  • Example 96 and Comparative Example 96 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 97 was repeated except that 44 g of the dye component of formula (1) in Example 97 was replaced with 41.4 g of the dye component of formula (10) and 2.6 g of the dye component of formula (11).
  • Example 97 The dye preparations of Example 97 and Comparative Example 97 were subjected to performance tests.
  • Example 97 and Comparative Example 97 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 98 was repeated except that the dye component of the formula (1) in Example 98 was replaced with the dye component of the formula (8).
  • Example 98 The dye preparations of Example 98 and Comparative Example 98 were subjected to performance tests.
  • Example 98 and Comparative Example 98 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 99 was repeated except that 9.5 g of the dye component of formula (1) in Example 99 was replaced with 5 g of the dye component of formula (1), and 36.5 g of the dye component of formula (2-2) was replaced with 41 g. (2-2) a dye component in which a mixture of 27 g of the dye component of the formula (3-1) and 27 g of the dye component of the formula (3-2) is replaced with 54 g of the dye component of the formula (3-1) Others remain unchanged.
  • Example 99 The dye preparations of Example 99 and Comparative Example 99 were subjected to performance tests.
  • Example 99 0.5 g of the dyes of Example 99 and Comparative Example 99 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 100 was repeated except that 10.8 g of the dye component of formula (3-1) and 43.2 g of the dye component of formula (3-2) in Example 100 were replaced with 54 g of the dye component of formula (3-2). Other than the other.
  • Example 100 The dye preparations of Example 100 and Comparative Example 100 were subjected to performance tests.
  • Example 100 0.5 g of the dyes of Example 100 and Comparative Example 100 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the finished dye product was prepared in accordance with the method of Example 100.
  • the dye product of Example 101 was subjected to performance testing.
  • 0.5 g of the dye of Example 101 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • the finished dye product was prepared in accordance with the method of Example 100.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 102 to 109 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • the swatch color light was observed and their light fastness and compatibility were measured by the method of Example 95 using AATCC 16-2004, and the results are shown in Table 50.
  • 0.5 g of the dyes of Examples 110 and 111 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • 0.5 g of the dye of Example 20-35 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 10ml of disperse dye suspension and mix with 90ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then heat up to 60 °C, and put 2g polyester fiber into high temperature and high pressure dyeing separately, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • Example 128 was repeated except that the dye component of the formula (1) of Example 128 was replaced with the dye component of the following formula (8).
  • Example 128 The dye preparations of Example 128 and Comparative Example 128 were subjected to performance tests.
  • Example 128 and Comparative Example 128 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • High strength means that textiles of the same depth can reduce the amount of dye and reduce the printing cost when printing.
  • Example 129 was repeated except that the dye component of the formula (1) of Example 129 was replaced with the dye component of the following formula (9).
  • Example 129 The dye preparations of Example 129 and Comparative Example 129 were subjected to performance tests.
  • Example 129 and Comparative Example 129 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 130 was repeated except that the dye component of the formula (1) of Example 130 was replaced with the dye component of the formula (4-1).
  • Example 130 The dye finished products of Example 130 and Comparative Example 130 were subjected to performance tests.
  • Example 130 0.5 g of the dyes of Example 130 and Comparative Example 130 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the method for determining compatibility is as follows: dyeing according to GB/T2394-2003, dyeing from 60 ° C, taking a sample immediately when the temperature is raised to 80 ° C, and then taking a sample every 10 ° C until 130 ° C, and Samples were taken at 130 ° C for 10 minutes, 20 minutes, 30 minutes, and 50 minutes, and a total of 10 swatches were taken. The sample was kept at 130 ° C for 50 minutes, and the sample of each temperature was taken as a sample to observe whether the hue change was synchronized. It is divided into five grades I, II, III, IV, V (instrument: computer colorimeter datacolor 600, color difference formula CMC 2:1). For the black color, the number of cloth samples in which DC (dampness difference) and DH (hue difference) are less than 0.6 are calculated.
  • Level I five and more than five
  • Class V one piece.
  • Example 131 was repeated except that the dye component of the formula (1) of Example 131 was replaced with the dye component of the following formula (10).
  • Example 131 The dye preparations of Example 131 and Comparative Example 131 were subjected to performance tests.
  • Example 131 and Comparative Example 131 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 132 was repeated except that 44 g of the dye component of formula (1) in Example 132 was replaced with 41.4 g of the dye component of formula (10) and 2.6 g of the dye component of formula (11).
  • Example 132 The dye finished products of Example 132 and Comparative Example 132 were subjected to performance testing.
  • Example 132 and Comparative Example 132 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • pH stability range pH range with intensity ⁇ 95% is the pH stability range.
  • Example 133 was repeated except that the dye component of the formula (1) in Example 133 was replaced with the dye component of the formula (8).
  • Example 133 The dye preparations of Example 133 and Comparative Example 133 were subjected to performance tests.
  • Example 133 and Comparative Example 133 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 134 was repeated except that the dye component of formula (3-2) in Example 134 was replaced with the following formula (13) In addition to the dye component, the others are unchanged.
  • Example 134 The dye preparations of Example 134 and Comparative Example 134 were subjected to performance tests.
  • Example 134 and Comparative Example 134 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example 135 was repeated except that 54 g of the dye of formula (3-2) in Example 135 was replaced with a mixture of 27 g of the dye component of formula (13) and 27 g of the dye component of formula (3-2). Others remain unchanged.
  • Example 135 The dye preparations of Example 135 and Comparative Example 135 were subjected to performance tests.
  • Example 135 and Comparative Example 135 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the finished dye was prepared in accordance with the method of Example 135.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 136 and 137 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the swatch color light was observed and their washing fastness, compatibility, and chlorophenol content were determined by using GB/T3921-2008, the method of Example 130, and GB/T18414.1-2006. The results are shown in Table 64.
  • the finished dye was prepared in accordance with the method of Example 135.
  • Example 138 The finished dye product of Example 138 was subjected to performance testing.
  • 0.5 g of the dye of Example 138 was weighed into 250 ml of water to prepare a disperse dye suspension. Pipette 30ml of disperse dye suspension and mix with 70ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then raise the temperature to 60 °C, and then put 2g polyester fiber into high temperature and high pressure dyeing, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • the swatch color light was observed and their light fastness, washing fastness and chlorophenol content were measured by AATCC 16-2004, GB/T3921-2008, GB/T18414.1-2006, and the results are shown in Table 66.
  • the finished dye was prepared in accordance with the procedure of Example 135.
  • 0.5 g of the dye product of Examples 139-141 was weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • 0.5 g of the dyes of Examples 142 to 152 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • Example Washing fastness Compatibility Chlorophenol content 142 5 II ⁇ 0.05 143 5 I ⁇ 0.05 144 5 I ⁇ 0.05 145 5 I ⁇ 0.05 146 5 I ⁇ 0.05 147 5 I ⁇ 0.05 148 5 I ⁇ 0.05 149 5 II ⁇ 0.05 150 5 II ⁇ 0.05 151 5 II ⁇ 0.05 152 5 II ⁇ 0.05
  • 0.5 g of the dyes of Examples 153 and 154 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension.
  • the swatch color light was observed and their light fastness, washing fastness and chlorophenol content were measured by AATCC16-2004, GB/T3921-2008, GB/T18414.1-2006, and the results are shown in Table 72.
  • a method similar to GB/T 2394-2003 0.5 g of the dyes of Examples 155 to 163 were weighed into 250 ml of water, respectively, to prepare a disperse dye suspension. Pipette 30ml of disperse dye suspension and mix with 70ml of water, adjust the pH of the dyeing bath to 5 with acetic acid, then raise the temperature to 60 °C, and then put 2g polyester fiber into high temperature and high pressure dyeing, heat up to 130 °C in 35 minutes, keep warm After 45 minutes, cool to 80 ° C for sampling.
  • Example Light fastness Washing fastness Compatibility Chlorophenol content 155 2 to 3 5 II ⁇ 0.05 156 2 to 3 5 I ⁇ 0.05 157 3 5 I ⁇ 0.05 158 3 5 I ⁇ 0.05 159 2 to 3 5 II ⁇ 0.05 160 2 to 3 5 II ⁇ 0.05 161 2 to 3 5 I ⁇ 0.05 162 3 5 II ⁇ 0.05 163 2 to 3 5 II ⁇ 0.05

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Abstract

一种分散染料组合物、分散染料及其的制备方法和用途。所述分散染料适用于织物,特别是涤纶及其混纺织物的染色和印花。

Description

一种分散染料组合物、分散染料及其的制备方法和用途 技术领域
本发明涉及一种分散染料组合物、分散染料及其的制备方法和用途。所述分散染料适用于织物,特别是涤纶及其混纺织物的染色和印花。
背景技术
随着人们对环保的日益重视,特别是一些欧洲国家相继出台了一些法规、政策等。同样的,近年来,中国对环保也提出了更高的要求,对一些重污染企业进行管制,染料企业如何求得生存和发展,是摆在染料制造商面前最大的,而且是最需迫切解决的难题。染料行业已经认识到这种机遇和挑战,因此逐渐开发出新颖、环保的染料。
发明内容
发明要解决的问题
本发明提供一种pH值范围广、日晒牢度好、配伍性优、强度高、水洗牢度好的经济环保型分散染料。
用于解决问题的方案
本发明提供一种分散染料组合物,其包括以下组分或由以下组分组成:
如式(1)所示的组分A:
Figure PCTCN2014095585-appb-000001
一种或两种以上如式(2)所示的组分B:
Figure PCTCN2014095585-appb-000002
式(2)中,X1为溴或氯;R1、R2各自独立为C1~C4的烷基;
一种或两种以上如式(3)所示的组分C:
Figure PCTCN2014095585-appb-000003
式(3)中,X2为溴或氯,R3、R4各自独立为C1~C4的烷基或CH2CH=CH2,Y为C1~C4的烷基;
任选的一种或两种以上如式(4)所示的组分D:
Figure PCTCN2014095585-appb-000004
式(4)中,X3、X4各自独立为氢、氯或溴,R5、R6各自独立为C2~C4的烷基,或C1~C4烷基中的一个氢被氰基、苯基、乙酰氧基或苯甲酰氧基取代的基团;其中组分D不为C.I.分散橙76;
任选的一种或两种以上如式(5)所示的组分E:
Figure PCTCN2014095585-appb-000005
式(5)中,X5、X6各自独立为氢、氯或硝基,R7为C1~C4的烷基;
任选的一种或两种以上如式(6)所示的组分F:
Figure PCTCN2014095585-appb-000006
式(6)中,X7、X8各自独立为溴、氯、氰基或硝基,R8为C1~C4的烷酰氨基或C1~C4的烷基,R9、R10各自独立为C1~C4的烷基,R11为氢或C1~C4的烷氧基;和
任选的如式(7)所示的组分G:
Figure PCTCN2014095585-appb-000007
根据本发明所述的分散染料组合物,优选地,式(6)中X7为氰基或硝基,X8为氰基,R11为氢。
根据本发明所述的分散染料组合物,优选地,式(3)中X2为氯,式(6)中X7为氰基或硝基,X8为氰基,R11为氢。
根据本发明所述的分散染料组合物,优选地,组分C为如式(3-1)和(3-2)所示的化合物:
Figure PCTCN2014095585-appb-000008
根据本发明所述的分散染料组合物,优选地,组分B为式(2-1)所示的化合物:
Figure PCTCN2014095585-appb-000009
组分C为式(3-2)所示的化合物:
Figure PCTCN2014095585-appb-000010
并且,式(4)中,X3、X4各自独立为氢或溴,式(6)中,X7、X8各自独立为溴、氰基或硝基。
根据本发明所述的分散染料组合物,优选地,所述组分B为以下化合物中的一种或两种:
Figure PCTCN2014095585-appb-000011
根据本发明所述的分散染料组合物,优选地,所述组分C为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000012
Figure PCTCN2014095585-appb-000013
根据本发明所述的分散染料组合物,优选地,所述组分C为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000014
根据本发明所述的分散染料组合物,优选地,其特征在于,所述组分D为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000015
Figure PCTCN2014095585-appb-000016
根据本发明所述的分散染料组合物,优选地,所述组分D为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000017
Figure PCTCN2014095585-appb-000018
根据本发明所述的分散染料组合物,优选地,所述组分E为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000019
根据本发明所述的分散染料组合物,优选地,所述组分F为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000020
根据本发明所述的分散染料组合物,优选地,所述组分F为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000021
Figure PCTCN2014095585-appb-000022
根据本发明所述的分散染料组合物,优选地,所述组分F为以下化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000023
根据本发明所述的分散染料组合物,优选地,组分B为如式(2-1)和式(2-2)所示化合物中的一种或两种:
Figure PCTCN2014095585-appb-000024
组分C为如下式(3-1)至(3-4)所示化合物中的一种或两种以上:
Figure PCTCN2014095585-appb-000025
根据本发明所述的分散染料组合物,优选地,组分B为如式(2-1)和式(2-2)所示化合物中的一种或两种:
Figure PCTCN2014095585-appb-000026
组分C为如下式(3-1)和(3-4)所示化合物中的一种或两种:
Figure PCTCN2014095585-appb-000027
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,包括:
重量百分比为2~73%的组分A,
重量百分比为7~40%的组分B,
重量百分比为20~58%的组分C,
任选的重量百分比为0~70%的组分D,
任选的重量百分比为0~10%的组分E,
任选的重量百分比为0~47%的组分F,和
任选的重量百分比为0~47%的组分G。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为3~50%,
组分B的重量百分比为12~39%,
组分C的重量百分比为38~58%。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为2~60%,
组分B的重量百分比为7~37%,
组分C的重量百分比为30~55%,
组分D的重量百分比为3~6%。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为3~6%,
组分B的重量百分比为12~37%,
组分C的重量百分比为35~55%,
组分D的重量百分比为2~50%。
根据本发明所述的分散染料组合物,优选地,其特征在于,基于所述组合物的总重量,
组分A的重量百分比为2~51%,
组分B的重量百分比为12~37%,
组分C的重量百分比为35~55%,
组分E的重量百分比为2~6%。
根据本发明所述的分散染料组合物,优选地,其特征在于,基于所述组合物的总重量,
组分A的重量百分比为2~72%,
组分B的重量百分比为7~40%,
组分C的重量百分比为20~48%,
组分F的重量百分比为1~10%。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为2~72%,
组分B的重量百分比为7~40%,
组分C的重量百分比为20~48%,
组分G的重量百分比为1~10%。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为2~71%,
组分B的重量百分比为7~40%,
组分C的重量百分比为20~48%,
组分E的重量百分比为1~5%,
组分G的重量百分比为1~5%。
根据本发明所述的分散染料组合物,优选地,基于所述组合物的总重量,
组分A的重量百分比为2~71%,
组分B的重量百分比为7~40%,
组分C的重量百分比为20~48%,
组分E的重量百分比为1~5%,
组分F的重量百分比为1~5%。
在实际生产过程中,本发明的各染料组分通常可能会带有一些副产物和其它杂质,但只要不影响本发明的实施即可。
本发明提供一种分散染料,包含本发明所述的分散染料组合物和辅料。
本发明所述的分散染料,所述辅料包括助剂和水。
本发明所述的分散染料,所述助剂包括以下的一种或两种以上的组合:萘系磺酸甲醛缩合物、木质素磺酸盐、硫酸钠、表面活性剂、杀菌剂,或其他染料分散剂。
本发明所述的分散染料,所述助剂与分散染料组合物的重量之比为0.3~4:1。
本发明所述的分散染料,所述分散染料用砂磨机或研磨机研磨后为液状,固含量为20~50%,或者所述分散染料喷雾干燥后为粉状或颗粒状,固含量为87~96%。
本发明还提供一种制备根据本发明所述的分散染料的方法,包括以下步骤:
将所述各染料组分混合后,在辅料的存在下用砂磨机或研磨机进行粒子化处理;或者将所述各染料组分分别在辅料存在下用砂磨机或研磨机进行粒子化处理,再进行混合。
本发明还提供一种根据本发明所述的分散染料用于织物的染色和印花的用途。
本发明还提供一种织物,通过使用根据本发明所述的分散染料进行染色和印花制备得到。
发明的效果
本发明所述的分散染料的日晒牢度优异、pH值适用范围广、各组份间的配伍性好,强度高,印染成本低,水洗牢度好,当式(2)、(3)、(4)、(6)不含有氯只含有溴时,符合Oeko-Tex Standard 100(2013)I级要求。
具体实施方式
根据本发明所述的分散染料组合物,基于所述组合物的总重量,包括:
重量百分比为2~73%的组分A,优选为2~72%,更优选为2~71%,更优选为2~60%,更优选为2~51%,更优选为3~50%,更优选为3~6%;
重量百分比为7~40%的组分B,优选为7~37%或12~39%,更优选为12~37%;
重量百分比为20~58%的组分C,优选为30~55%或20~48%,更优选为38~58%或35~55%;
任选的重量百分比为0~70%的组分D,优选为2~50%,更优选为3~6%;
任选的重量百分比为0~10%的组分E,优选为2~6%,更优选为1~5%;
任选的重量百分比为0~47%的组分F,优选为1~10%,更优选为1~5%;
任选的重量百分比为0~47%的组分G,优选为1~10%,更优选为1~5%。
根据本发明所述的分散染料组合物,在组分C为式(3-1)和式(3-2)所示的化合物情况下,式(3-1)所示的化合物的重量百分比为1~99%,优选为70~90%,式(3-2)所示的化合物的重量百分比为1~99%,优选为10~30%。
实施例
下面结合实施例对本发明作进一步说明,但本发明的保护范围并不限于此。
在实施例中,本发明的组分A、B、C和任选的组分D、E、F、G,按一定的配比与助剂和水拼混后,用砂磨机进行研磨分散制成浆料,或进一步进行喷雾干燥,从而制成染料。
所述组分A、B、C、D、E、F、G均为已知的染料化合物并且可以在市场上购得,或者可由现有的方法制备。
实施例1:
将15.6克式(1)染料组分、6.1克式(2-2)染料组分、16.3克式(3-1)染料组分、31克分散剂MF和31克木质素85A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例1:
重复实施例1,除了将实施例1的式(1)染料组分替换成下式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000028
将实施例1和对比例1的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例1和对比例1的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,测定结果见表1。
表1
名称 强度
实施例1 102%
对比例1 100%
强度高意味着,同样深度的纺织品,印染时可以减少染料用量,减少印染成本。
实施例2:
将15.6克式(1)染料组分、6.1克式(2-1)染料组分、16.3克式(3-2)染料组分、31克分散剂MF和31克木质素83A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例2:
重复实施例2,除了将实施例2的式(1)染料组分替换成下式(9)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000029
将实施例2和对比例2的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例2和对比例2的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g 聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004测定它们的日晒牢度,结果见表2。
表2
名称 日晒牢度(40h)
实施例2 2~3
对比例2 2
实施例3:
将15.6克式(1)染料组分、6.1克式(2-2)染料组分、11.4克式(3-1)染料组分、4.9克式(3-2)染料组分和11.4克分散剂MF,加水100克充分搅拌均匀,研磨分散,制成液状染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例3:
重复实施例3,除了将实施例3的式(1)染料组分替换成式(4-1)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000030
将实施例3和对比例3的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例3和对比例3的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,并且参照GB/T2400-2006测定它们的强度、日晒牢度和配伍性,结果见表3。
表3
名称 强度 日晒牢度 配伍性
实施例3 105% 3
对比例3 100% 2
测定配伍性的方法为:参照GB/T2394-2003进行染色,从60℃入染,当温度升到80℃时马上取一个样,以后每隔10℃取一个样,直到130℃,并且,在130℃保温10分钟、20分钟、30分钟、50分钟时分别取样,共取10块布样。以130℃保温50分钟为标样,各档温度所取布样为试样,观察其色相变化是否同步。共分五级制Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ(仪器:电脑测色仪datacolor 600,色差公式CMC 2:1)。对于黑色色泽,计算DC(艳度差)、DH(色调差)均小于0.6的布样块数。
Ⅰ级:五块及五块以上
Ⅱ级:四块
Ⅲ级:三块
Ⅳ级:二块
Ⅴ级:一块。
实施例4:
将15.6克式(1)染料组分、6.1克式(2-1)染料组分、16.4克式(3-4)染料组分、31克分散剂MF和31克扩散剂NNO,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例4:
重复实施例4,除了将实施例4的式(1)染料组分替换成下式(10)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000031
将实施例4和对比例4的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例4和对比例4的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参照GB/T2403-2006测定它们的强度、pH值范围,结果见表4。
表4
名称 强度 pH值稳定范围
实施例4 107% 3~9
对比例4 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例5:
将44克式(1)染料组分、22克式(2-2)染料组分、34克式(3-1)染料组分、31克分散剂MF和31克扩散剂NNO,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例5:
重复实施例5,除了将实施例5中的44克式(1)染料组分替换成41.4克式(10)染料组分和2.6克式(11)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000032
将实施例5和对比例5的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例5和对比例5的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与 90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参考GB/T2403-2006测定它们的强度、pH值范围,结果见表5。
表5
名称 强度 pH值稳定范围
实施例5 107% 3~9
对比例5 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例6:
将7.8克式(1)染料组分、7.8克式(4-1)染料组分、6.1克式(2-1)染料组分、16.4克式(3-4)染料组分、31克扩散剂MF和31克木质素85A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例6:
重复实施例6,除了将实施例6中的式(1)染料组分替换成式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000033
将实施例6和对比例6的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例6和对比例6的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却 到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,结果见表6。
表6
名称 强度
实施例6 102%
对比例6 100%
实施例7和8:
按照表7中的组成配方,与实施例6同样地制得染料成品。
表7单位:克
Figure PCTCN2014095585-appb-000034
将实施例7和实施例8的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例7和实施例8的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用实施例3的方法测定它们的配伍性,结果见表8。
表8
实施例 配伍性
7
8
实施例9:
按照表9中的组成配方,与实施例6同样地制得染料成品。
表9                                       单位:克
Figure PCTCN2014095585-appb-000035
将实施例9的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,称取0.5克实施例9的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004方法测定其日晒牢度,结果见表10。
表10
实施例 日晒牢度
9 3
实施例10-15
按照表11中的组成配方,与实施例6同样地制得染料成品。
表11                                       单位:克
Figure PCTCN2014095585-appb-000036
将实施例10-15的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例10-15的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例3的方法测定它们的日晒牢度、配伍性,结果见表12。
表12
实施例 日晒牢度 配伍性
10 2~3
11 2~3
12 2~3
13 2~3
14 2~3
15 3
实施例16-17
按照表13中的组成配方,加入适量助剂,制成染料成品。
表13                                       单位:克
Figure PCTCN2014095585-appb-000037
将实施例16-17的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例16和17的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用实施例3的方法测定它们的配伍性,结果见表14。
表14
实施例 配伍性
16
17
实施例18-38
按照表15中的组成配方,加入适量助剂,制成染料成品。
表15                                       单位:克
Figure PCTCN2014095585-appb-000038
将实施例18-38的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例18-38的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例3的方法测定它们的日晒牢度、配伍性,结果见表16。
表16
实施例 日晒牢度 配伍性
18 2~3
19 2~3
20 3
21 3
22 3
23 3
24 2~3
25 3
26 2~3
27 2~3
28 3
29 3
30 2~3
31 3
32 3
33 2~3
34 2~3
35 2~3
36 3
37 3
38 3
实施例39-43
按照表17中的组成配方,加入适量助剂,制成染料成品。
表17                                       单位:克
Figure PCTCN2014095585-appb-000039
将实施例39-43的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例39-43的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例3的方法测定它们的日晒牢度、配伍性,结果见表18。
表18
实施例 日晒牢度 配伍性
39 2~3
40 3
41 2~3
42 3
43 3
实施例44:
将41克式(1)染料组分、16克式(2-2)染料组分、43克式(3-1)染料组分、80克分散剂MF和80克木质素85A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例44:
重复实施例44,除了将实施例44的式(1)染料组分替换成下式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000040
将实施例44和对比例44的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例44和对比例44的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,测定结果见表19。
表19
名称 强度
实施例44 102%
对比例44 100%
强度高意味着,同样深度的纺织品,印染时可以减少染料用量,减少印染成本。
实施例45:
将41克式(1)染料组分、16克式(2-2)染料组分、43克式(3-1)染料组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例45:
重复实施例45,除了将实施例45的式(1)染料组分替换成下式(9)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000041
将实施例45和对比例45的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例45和对比例45的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004测定它们的日晒牢度,结果见表20。
表20
名称 日晒牢度(40h)
实施例45 3
对比例45 2~3
实施例46:
将41克式(1)染料组分、16克式(2-2)染料组分、43克式(3-1)染料组分和30克分散剂MF,加水200克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例46:
重复实施例46,除了将实施例46的式(1)染料组分替换成式(4-1)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000042
将实施例46和对比例46的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例46和对比例46的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,并且参照GB/T2400-2006测定它们的强度、日晒牢度和配伍性,结果见表21。
表21
名称 强度 日晒牢度 配伍性
实施例46 105% 3
对比例46 100% 2
测定配伍性的方法为:参照GB/T2394-2003进行染色,从60℃入染,当温度升到80℃时马上取一个样,以后每隔10℃取一个样,直到130℃,并且,在130℃保温10分钟、20分钟、30分钟、50分钟时分别取样,共取10块布样。以130℃保温50分钟为标样,各档温度所取布样为试样,观察其色相变化是否同步。共分五级制Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ(仪器:电脑测色仪datacolor 600,色差公式CMC 2:1)。对于黑色色泽,计算DC(艳度差)、DH(色调差)均小于0.6的布样块数。
Ⅰ级:五块及五块以上
Ⅱ级:四块
Ⅲ级:三块
Ⅳ级:二块
Ⅴ级:一块。
实施例47:
将41克式(1)染料组分、16克式(2-2)染料组分、43克式(3-1)染料组分、30克分散剂MF和30克扩散剂NNO,加水250克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例47:
重复实施例47,除了将实施例47的式(1)染料组分替换成下式(10)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000043
将实施例47和对比例47的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例47和对比例47的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参照GB/T2403-2006测定它们的强度、pH值范围,结果见表22。
表22
名称 强度 pH值稳定范围
实施例47 107% 3~8
对比例47 100% 3~6
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例48:
将44克式(1)染料组分、22克式(2-2)染料组分、34克式(3-1)染料组分、31克分散剂MF和31克扩散剂NNO,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例48:
重复实施例48,除了将实施例48中的44克式(1)染料组分替换成41.4克式(10)染料组分和2.6克式(11)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000044
将实施例48和对比例48的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例48和对比例48的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液 与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参考GB/T2403-1006测定它们的强度、pH值范围,结果见表23。
表23
名称 强度 pH值稳定范围
实施例48 107% 3~9
对比例48 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例49:
将7.8克式(1)染料组分、7.8克式(4-1)染料组分、6.1克式(2-1)染料组分、16.4克式(3-1)染料组分、31克扩散剂MF和31克木质素85A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例49:
重复实施例49,除了将实施例49中的式(1)染料组分替换成式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000045
将实施例49和对比例49的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例49和对比例49的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入 2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,结果见表24。
表24
名称 强度
实施例49 102%
对比例49 100%
实施例50:
将9.5克式(1)染料组分、36.5克式(2-2)染料组分、54克式(3-1)染料组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例50:
重复实施例50,除了将实施例50中的式(3-1)染料组分替换成下式(12)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000046
将实施例50和对比例50的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例50和对比例50的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,测定它们的强度、 日晒牢度,结果见表25。
表25
名称 强度 日晒牢度(40h)
实施例50 105% 3
对比例50 100% 2~3
实施例51:
将12克式(1)染料组分、34克式(2-2)染料组分、54克式(3-1)染料组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例51:
重复实施例51,除了将实施例51中的54克式(3-1)染料组分替换成27克式(12)染料组分和27克式(3-1)染料组分的混合物之外,其它不变。
将实施例51和对比例51的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例51和对比例51的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,测定它们的强度、日晒牢度,结果见表26。
表26
名称 强度 日晒牢度(40h)
实施例51 103% 3
对比例51 100% 2~3
实施例52和53
根据表27的组成配方,按照实施例51的方法制成染料成品。
表27                                       单位:克
Figure PCTCN2014095585-appb-000047
将实施例52和实施例53的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例52和实施例53的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用实施例46的方法测定它们的配伍性,结果见表28。
表28
实施例 配伍性
52
53
实施例54:
根据表29的配方,按照实施例51的方法制成染料成品。
表29                                       单位:克
Figure PCTCN2014095585-appb-000048
将实施例54的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,称取0.5克实施例54的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004方法测定其日晒牢度,结果见表30。
表30
实施例 日晒牢度
54 3
实施例55和56
根据表31的配方,按照实施例51的方法制成染料成品。
表31                                       单位:克
Figure PCTCN2014095585-appb-000049
将实施例55和56的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例55和56的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例46的方法测定它们的日晒牢度、配伍性,结果见表32。
表32
实施例 日晒牢度 配伍性
55 3
56 3
实施例57-64
按照表33中的配方,加入适量助剂,制成染料成品。
表33
Figure PCTCN2014095585-appb-000050
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例57-64的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用实施例46的方法测定它们的配伍性,结果见表34。
表34
实施例 配伍性
57
58
59
60
61
62
63
64
实施例65和66
按照表35中的配方,加入适量助剂,制成染料成品。
表35                                       单位:克
Figure PCTCN2014095585-appb-000051
将实施例65和66的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例65和66的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004测定它们的日晒牢度,结果见表36。
表36
实施例 日晒牢度
65 3
66 3
实施例67-92
按照表37中的配方,加入适量助剂,制成染料成品。
表37                                       单位:克
Figure PCTCN2014095585-appb-000052
Figure PCTCN2014095585-appb-000053
将实施例67-92的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例67-92的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例46的方法测定它们的日晒牢度、配伍性,结果见表38。
表38
实施例 日晒牢度 配伍性
67 3 I
68 3 I
69 3 I
70 3 I
71 3 II
72 3 I
73 3 I
74 3 I
75 3 I
76 3 II
77 3 II
78 3 II
79 3 II
80 3 II
81 3 II
82 3 II
83 3 II
84 3 II
85 3 II
86 3 II
87 3 II
88 3 I
89 3 I
90 3 II
91 3 I
92 3 II
实施例93:
将41克式(1)染料组分、16克式(2-2)染料组分、30克式(3-1)染料组分和13克式(3-2)染料组分的混合物、80克分散剂MF和80克木质素85A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例93:
重复实施例93,除了将实施例93的式(1)染料组分替换成下式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000054
将实施例93和对比例93的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例93和对比例93的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,测定结果见表39。
表39
名称 强度
实施例93 102%
对比例93 100%
强度高意味着,同样深度的纺织品,印染时可以减少染料用量,减少印染成本。
实施例94:
将41克式(1)染料组分、16克式(2-1)染料组分、30克式(3-1)染料 组分和13克式(3-2)染料组分的混合物、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例94:
重复实施例94,除了将实施例94的式(1)染料组分替换成下式(9)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000055
将实施例94和对比例94的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例94和对比例94的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004测定它们的日晒牢度,结果见表40。
表40
名称 日晒牢度(40h)
实施例94 3
对比例94 2
实施例95:
将41克式(1)染料组分、16克式(2-1)染料组分、30克式(3-1)染料组分和13克式(3-2)染料组分的混合物,以及30克分散剂MF,加水200克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例95:
重复实施例95,除了将实施例95的式(1)染料组分替换成式(4-1)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000056
将实施例95和对比例95的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例95和对比例95的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,并且参照GB/T2400-2006测定它们的强度、日晒牢度和配伍性,结果见表41。
表41
名称 强度 日晒牢度 配伍性
实施例95 105% 2~3
对比例95 100% 2 III
测定配伍性的方法为:参照GB/T2394-2003进行染色,从60℃入染,当温度升到80℃时马上取一个样,以后每隔10℃取一个样,直到130℃,并且,在130℃保温10分钟、20分钟、30分钟、50分钟时分别取样,共取10块布样。以130℃保温50分钟为标样,各档温度所取布样为试样,观察其色相变化是否同步。共分五级制Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ(仪器:电脑测色仪datacolor 600,色差公式CMC 2:1)。对于黑色色泽,计算DC(艳度差)、DH(色调差)均小于0.6的布样块数。
Ⅰ级:五块及五块以上
Ⅱ级:四块
Ⅲ级:三块
Ⅳ级:二块
Ⅴ级:一块。
实施例96:
将41克式(1)染料组分、16克式(2-2)染料组分、30克式(3-1)染料组分和13克式(3-2)染料组分的混合物、30克分散剂MF和30克扩散剂NNO,加水250克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例96:
重复实施例96,除了将实施例96的式(1)染料组分替换成下式(10)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000057
将实施例96和对比例96的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例96和对比例96的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参照GB/T2403-2006测定它们的强度、pH值范围,结果见表42。
表42
名称 强度 pH值稳定范围
实施例96 107% 3~9
对比例96 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例97:
将44克式(1)染料组分、22克式(2-2)染料组分、30.6克式(3-1)染料组分和3.4克式(3-2)染料组分的混合物、31克分散剂MF和31克扩散剂NNO,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例97:
重复实施例97,除了将实施例97中的44克式(1)染料组分替换成41.4克式(10)染料组分和2.6克式(11)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000058
将实施例97和对比例97的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例97和对比例97的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参考GB/T2403-2006测定它们的强度、pH值范围,结果见表43。
表43
名称 强度 pH值稳定范围
实施例97 107% 3~9
对比例97 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例98:
将7.8克式(1)染料组分、7.8克式(4-1)染料组分、6.0克式(2-1)染料组分、13.1克式(3-1)染料组分和3.3克式(3-2)染料组分的混合物、31克扩散剂MF和31克木质素85A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例98:
重复实施例98,除了将实施例98中的式(1)染料组分替换成式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000059
将实施例98和对比例98的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例98和对比例98的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008测定它们的强度,结果见表44。
表44
名称 强度
实施例98 102%
对比例98 100%
实施例99:
将9.5克式(1)染料组分、36.5克式(2-2)染料组分、27克式(3-1)染料组分和27克式(3-2)染料组分的混合物、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例99:
重复实施例99,除了将实施例99中的9.5克式(1)染料组分替换为5克式(1)染料组分、将36.5克式(2-2)染料组分替换为41克式(2-2)染料组分,将27克式(3-1)染料组分和27克式(3-2)染料组分的混合物替换成54克式(3-1)染料组分之外,其它不变。
将实施例99和对比例99的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例99和对比例99的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T3921-2008,测定它们的水洗牢度,结果见表45。
表45
名称 水洗牢度
实施例99 4~5
对比例99 4
实施例100:
将12克式(1)染料组分、34克式(2-2)染料组分、10.8克式(3-1)染料组分和43.2克式(3-2)染料组分的混合物、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例100:
重复实施例100,除了将实施例100中的10.8克式(3-1)染料组分和43.2克式(3-2)染料组分的混合物替换成54克式(3-2)染料组分之外,其它不变。
将实施例100和对比例100的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例100和对比例100的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,测定它们的强度、日晒牢度,结果见表46。
表46
名称 强度 日晒牢度(40h)
实施例100 103.5% 2~3
对比例100 100% 2
实施例101:
根据表47中的配方,按照实施例100的方法制成染料成品。
表47                                       单位:克
Figure PCTCN2014095585-appb-000060
将实施例101的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,称取0.5克实施例101的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004的方法,测定它们的日晒牢度,结果见表48。
表48
实施例 日晒牢度
101 3
实施例102-109
根据表49中的配方,按照实施例100的方法制成染料成品。
表49                                       单位:克
Figure PCTCN2014095585-appb-000061
将实施例102-109的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例102-109的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例95的方法测定它们的日晒牢度、配伍性,结果见表50。
表50
实施例 日晒牢度 配伍性
102 3
103 2~3
104 3
105 2~3
106 3
107 2~3
108 2~3
109 3
实施例110和111
按照表51中的配方,加入适量助剂,制成染料成品。
表51                                       单位:克
Figure PCTCN2014095585-appb-000062
将实施例110和111的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例110和111的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004的方法,测定它们的日晒牢度,结果见表52。
表52
实施例 日晒牢度
110 3
111 3
实施例112-127
按照表53中的配方,加入适量助剂,制成染料成品。
表53                                       单位:克
Figure PCTCN2014095585-appb-000063
将实施例112-127的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例20-35的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004,和采用实施例3的方法测定它们的日晒牢度、配伍性,结果见表54。
表54
实施例 日晒牢度 配伍性
112 2~3
113 2~3
114 2~3
115 3
116 3
117 3
118 2~3
119 3
120 2~3
121 2~3
122 2~3
123 2~3
124 3
125 2~3
126 3
127 3
实施例128:
将41克式(1)染料组分、16克式(2-1)染料组分、43克式(3-2)染料组分、80克分散剂MF和80克木质素85A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例128:
重复实施例128,除了将实施例128的式(1)染料组分替换成下式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000064
将实施例128和对比例128的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例128和对比例128的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、GB/T3921-2008测定它们的强度、水洗牢度,测定结果见表55。
表55
名称 强度 水洗牢度
实施例128 102% 5
对比例128 100% 4~5
强度高意味着,同样深度的纺织品,印染时可以减少染料用量,减少印染成本。
实施例129:
将41克式(1)染料组分、16克式(2-1)染料组分、43克式(3-2)染料 组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例129:
重复实施例129,除了将实施例129的式(1)染料组分替换成下式(9)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000065
将实施例129和对比例129的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例129和对比例129的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004测定它们的日晒牢度,结果见表56。
表56
名称 日晒牢度(40h)
实施例129 2~3
对比例129 2
实施例130:
将41克式(1)染料组分、16克式(2-1)染料组分、43克式(3-2)染料组分和30克分散剂MF,加水200克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例130:
重复实施例130,除了将实施例130的式(1)染料组分替换成式(4-1)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000066
将实施例130和对比例130的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例130和对比例130的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、AATCC16-2004,并且参照GB/T2400-2006测定它们的强度、日晒牢度和配伍性,结果见表57。
表57
名称 强度 日晒牢度 配伍性
实施例130 105% 2~3
对比例130 100% 2
测定配伍性的方法为:参照GB/T2394-2003进行染色,从60℃入染,当温度升到80℃时马上取一个样,以后每隔10℃取一个样,直到130℃,并且,在130℃保温10分钟、20分钟、30分钟、50分钟时分别取样,共取10块布样。以130℃保温50分钟为标样,各档温度所取布样为试样,观察其色相变化是否同步。共分五级制Ⅰ、Ⅱ、Ⅲ、Ⅳ、Ⅴ(仪器:电脑测色仪datacolor 600,色差公式CMC 2:1)。对于黑色色泽,计算DC(艳度差)、DH(色调差)均小于0.6的布样块数。
Ⅰ级:五块及五块以上
Ⅱ级:四块
Ⅲ级:三块
Ⅳ级:二块
Ⅴ级:一块。
实施例131:
将41克式(1)染料组分、16克式(2-1)染料组分、43克式(3-2)染料组分、30克分散剂MF和30克扩散剂NNO,加水250克充分搅拌均匀,研磨分散制成浆染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例131:
重复实施例131,除了将实施例131的式(1)染料组分替换成下式(10)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000067
将实施例131和对比例131的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例131和对比例131的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参照GB/T2403-2006测定它们的强度、pH值范围,结果见表59。
表58
名称 强度 pH值稳定范围
实施例131 107% 3~9
对比例131 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例132:
将44克式(1)染料组分、22克式(2-1)染料组分、34克式(3-2)染料组分、31克分散剂MF和31克扩散剂NNO,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的黑色聚酯。
对比例132:
重复实施例132,除了将实施例132中的44克式(1)染料组分替换成41.4克式(10)染料组分和2.6克式(11)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000068
将实施例132和对比例132的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例132和对比例132的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008,和参考GB/T2403-2006测定它们的强度、pH值范围,结果见表59。
表59
名称 强度 pH值稳定范围
实施例132 107% 3~9
对比例132 100% 3~7
注:pH值稳定范围:以强度≥95%的pH值范围为pH值稳定范围。
实施例133:
将7.8克式(1)染料组分、7.8克式(4-1)染料组分、6.0克式(2-1)染料组分、16.4克式(3-2)染料组分、31克扩散剂MF和31克木质素85A,加水200克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度 性能优良的黑色聚酯。
对比例133:
重复实施例133,除了将实施例133中的式(1)染料组分替换成式(8)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000069
将实施例133和对比例133的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例133和对比例133的染料成品至250ml的水中,制成分散染料悬浮液。吸取10ml分散染料悬浮液与90ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T6688-2008、GB/T3921-2008测定它们的强度、水洗牢度,结果见表60。
表60
名称 强度 水洗牢度
实施例133 102% 5
对比例133 100% 4~5
实施例134:
将9.5克式(1)染料组分、36.5克式(2-1)染料组分、54克式(3-2)染料组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例134:
重复实施例134,除了将实施例134中的式(3-2)染料组分替换成下式 (13)染料组分之外,其它不变。
Figure PCTCN2014095585-appb-000070
将实施例134和对比例134的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例134和对比例134的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T3921-2008、GB/T18414.1-2006测定它们的水洗牢度、氯苯酚含量,结果见表61。
表61
名称 水洗牢度 氯苯酚含量
实施例134 5 <0.05
对比例134 4~5 >0.05
实施例135:
将12克式(1)染料组分、34克式(2-1)染料组分、54克式(3-2)染料组分、80克分散剂MF和80克木质素83A,加水390克充分搅拌均匀,研磨分散并干燥,即得染料成品,染色得到各项牢度性能优良的蓝色聚酯。
对比例135:
重复实施例135,除了将实施例135中的54克式(3-2)染料组分替换成27克式(13)染料组分和27克式(3-2)染料组分的混合物之外,其它不变。
将实施例135和对比例135的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例135和对比例135的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T3921-2008、GB/T18414.1-2006,测定它们的水洗牢度、氯苯酚含量,结果见表62。
表62
名称 水洗牢度 氯苯酚含量
实施例135 5 <0.05
对比例135 4-5 >0.05
实施例136-137
根据表63中的配方,按照实施例135的方法制成染料成品。
表63                                       单位:克
Figure PCTCN2014095585-appb-000071
将实施例136和137的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例136和137的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃ 取样。
观察布样色光并采用GB/T3921-2008、实施例130的方法和GB/T18414.1-2006,测定它们的水洗牢度、配伍性、氯苯酚含量,结果见表64。
表64
实施例 水洗牢度 配伍性 氯苯酚含量
136 5 <0.05
137 5 <0.05
实施例138:
根据表65中的配方,按照实施例135的方法制成染料成品。
表65                                       单位:克
Figure PCTCN2014095585-appb-000072
将实施例138的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,称取0.5克实施例138的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004、GB/T3921-2008、GB/T18414.1-2006,测定它们的日晒牢度、水洗牢度、氯苯酚含量,结果见表66。
表66
实施例 日晒牢度 水洗牢度 氯苯酚含量
138 3 5 <0.05
实施例139-141
根据表67中的配方,按照实施例135的方法制成染料成品。
表67                                       单位:克
Figure PCTCN2014095585-appb-000073
将实施例139-141的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例139-141的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004、GB/T3921-2008、实施例130的方法、GB/T18414.1-2006,测定它们的日晒牢度、水洗牢度、配伍性、氯苯酚含量,结果见表68。
表68
实施例 日晒牢度 水洗牢度 配伍性 氯苯酚含量
139 2~3 5 <0.05
140 2~3 5 <0.05
141 2~3 5 <0.05
实施例142-152
按照表69中的配方,加入适量助剂,制成染料成品。
表69                                       单位:克
Figure PCTCN2014095585-appb-000074
将实施例142-152的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例142-152的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用GB/T3921-2008、实施例130的方法、GB/T18414.1-2006,测定它们的水洗牢度、配伍性、氯苯酚含量,结果见表70。
表70
实施例 水洗牢度 配伍性 氯苯酚含量
142 5 <0.05
143 5 <0.05
144 5 <0.05
145 5 <0.05
146 5 <0.05
147 5 <0.05
148 5 <0.05
149 5 <0.05
150 5 <0.05
151 5 <0.05
152 5 <0.05
实施例153-154
按照表71中的配方,加入适量助剂,制成染料成品。
表71                                       单位:克
Figure PCTCN2014095585-appb-000075
将实施例153和154的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例153和154的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004、GB/T3921-2008、GB/T18414.1-2006,测定它们的日晒牢度、水洗牢度、氯苯酚含量,结果见表72。
表72
实施例 日晒牢度 水洗牢度 氯苯酚含量
153 3 5 <0.05
154 3 5 <0.05
实施例155-163
按照表73中的配方,加入适量助剂,制成染料成品。
表73                                       单位:克
Figure PCTCN2014095585-appb-000076
将实施例155-163的染料成品进行性能测试。
具体测试方法如下:
按照GB/T2394-2003相似的方法,分别称取0.5克实施例155-163的染料成品至250ml的水中,制成分散染料悬浮液。吸取30ml分散染料悬浮液与70ml的水混合,用醋酸调节染浴pH到5,然后升温到60℃,同时分别放入2g聚酯纤维进行高温高压染色,在35分钟内升温到130℃,保温45分钟,冷却到80℃取样。
观察布样色光并采用AATCC16-2004、GB/T3921-2008、实施例130的方法、GB/T18414.1-2006,测定它们的日晒牢度、水洗牢度、配伍性、氯苯酚含量,结果见表74。
表74
实施例 日晒牢度 水洗牢度 配伍性 氯苯酚含量
155 2~3 5 <0.05
156 2~3 5 <0.05
157 3 5 <0.05
158 3 5 <0.05
159 2~3 5 <0.05
160 2~3 5 <0.05
161 2~3 5 <0.05
162 3 5 <0.05
163 2~3 5 <0.05

Claims (33)

  1. 一种分散染料组合物,其特征在于包括以下组分或由以下组分组成:
    如式(1)所示的组分A:
    Figure PCTCN2014095585-appb-100001
    一种或两种以上如式(2)所示的组分B:
    Figure PCTCN2014095585-appb-100002
    式(2)中,X1为溴或氯;R1、R2各自独立为C1~C4的烷基;
    一种或两种以上如式(3)所示的组分C:
    Figure PCTCN2014095585-appb-100003
    式(3)中,X2为溴或氯,R3、R4各自独立为C1~C4的烷基或CH2CH=CH2,Y为C1~C4的烷基;
    任选的一种或两种以上如式(4)所示的组分D:
    Figure PCTCN2014095585-appb-100004
    式(4)中,X3、X4各自独立为氢、氯或溴,R5、R6各自独立为C2~C4的烷基,或C1~C4烷基中的一个氢被氰基、苯基、乙酰氧基或苯甲酰氧基取代的基团;其中组分D不为C.I.分散橙76;
    任选的一种或两种以上如式(5)所示的组分E:
    Figure PCTCN2014095585-appb-100005
    式(5)中,X5、X6各自独立为氢、氯或硝基,R7为C1~C4的烷基;
    任选的一种或两种以上如式(6)所示的组分F:
    Figure PCTCN2014095585-appb-100006
    式(6)中,X7、X8各自独立为溴、氯、氰基或硝基,R8为C1~C4的烷酰氨基或C1~C4的烷基,R9、R10各自独立为C1~C4的烷基,R11为氢或C1~C4的烷氧基;和
    任选的如式(7)所示的组分G:
    Figure PCTCN2014095585-appb-100007
  2. 根据权利要求1所述的分散染料组合物,其特征在于,式(6)中X7为氰基或硝基,X8为氰基,R11为氢。
  3. 根据权利要求1所述的分散染料组合物,其特征在于,式(3)中X2为氯,式(6)中X7为氰基或硝基,X8为氰基,R11为氢。
  4. 根据权利要求1所述的分散染料组合物,其特征在于,组分C为如式(3-1)和(3-2)所示的化合物:
    Figure PCTCN2014095585-appb-100008
    Figure PCTCN2014095585-appb-100009
  5. 根据权利要求1所述的分散染料组合物,其特征在于,组分B为式(2-1)所示的化合物:
    Figure PCTCN2014095585-appb-100010
    组分C为式(3-2)所示的化合物:
    Figure PCTCN2014095585-appb-100011
    并且,式(4)中,X3、X4各自独立为氢或溴,式(6)中,X7、X8各自独立为溴、氰基或硝基。
  6. 根据权利要求1~4任一项所述的分散染料组合物,其特征在于,所述组分B为以下化合物中的一种或两种:
    Figure PCTCN2014095585-appb-100012
  7. 根据权利要求1、2或6所述的分散染料组合物,其特征在于,所述组分C为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100013
  8. 根据权利要求3所述的分散染料组合物,其特征在于,所述组分C为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100014
    Figure PCTCN2014095585-appb-100015
  9. 根据权利要求1~4、6~8中任一项所述的分散染料组合物,其特征在于,所述组分D为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100016
    Figure PCTCN2014095585-appb-100017
  10. 根据权利要求5所述的分散染料组合物,其特征在于,所述组分D为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100018
  11. 根据权利要求1~10中任一项所述的分散染料组合物,其特征在于,所述组分E为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100019
  12. 根据权利要求1、4、6、9或11中所述的分散染料组合物,其特征在于,所述组分F为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100020
    Figure PCTCN2014095585-appb-100021
  13. 根据权利要求5或10~11中任一项所述的分散染料组合物,其特征在于,所述组分F为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100022
  14. 根据权利要求1~3、6~9或11中所述的分散染料组合物,其特征在于,所述组分F为以下化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100023
  15. 根据权利要求1、2、6、7、9、11或14中所述的分散染料组合物,其特征在于,组分B为如式(2-1)和式(2-2)所示化合物中的一种或两种:
    Figure PCTCN2014095585-appb-100024
    组分C为如下式(3-1)至(3-4)所示化合物中的一种或两种以上:
    Figure PCTCN2014095585-appb-100025
    Figure PCTCN2014095585-appb-100026
  16. 根据权利要求1、3、6、8、9、11或14中所述的分散染料组合物,其特征在于,组分B为如式(2-1)和式(2-2)所示化合物中的一种或两种:
    Figure PCTCN2014095585-appb-100027
    组分C为如下式(3-1)和(3-4)所示化合物中的一种或两种:
    Figure PCTCN2014095585-appb-100028
    Figure PCTCN2014095585-appb-100029
  17. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,包括:
    重量百分比为2~73%的组分A,
    重量百分比为7~40%的组分B,
    重量百分比为20~58%的组分C,
    任选的重量百分比为0~70%的组分D,
    任选的重量百分比为0~10%的组分E,
    任选的重量百分比为0~47%的组分F,和
    任选的重量百分比为0~47%的组分G。
  18. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为3~50%,
    组分B的重量百分比为12~39%,
    组分C的重量百分比为38~58%。
  19. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~60%,
    组分B的重量百分比为7~37%,
    组分C的重量百分比为30~55%,
    组分D的重量百分比为3~6%。
  20. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为3~6%,
    组分B的重量百分比为12~37%,
    组分C的重量百分比为35~55%,
    组分D的重量百分比为2~50%。
  21. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~51%,
    组分B的重量百分比为12~37%,
    组分C的重量百分比为35~55%,
    组分E的重量百分比为2~6%。
  22. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~72%,
    组分B的重量百分比为7~40%,
    组分C的重量百分比为20~48%,
    组分F的重量百分比为1~10%。
  23. 根据权利要求1~16中任一项所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~72%,
    组分B的重量百分比为7~40%,
    组分C的重量百分比为20~48%,
    组分G的重量百分比为1~10%。
  24. 根据权利要求1、3、6、8、9、11、12或15中所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~71%,
    组分B的重量百分比为7~40%,
    组分C的重量百分比为20~48%,
    组分E的重量百分比为1~5%,
    组分G的重量百分比为1~5%。
  25. 根据权利要求1、3、6、8、9、11、12或15中所述的分散染料组合物,其特征在于,基于所述组合物的总重量,
    组分A的重量百分比为2~71%,
    组分B的重量百分比为7~40%,
    组分C的重量百分比为20~48%,
    组分E的重量百分比为1~5%,
    组分F的重量百分比为1~5%。
  26. 一种分散染料,其特征在于,包含根据权利要求1~25中任一项所述的分散染料组合物和辅料。
  27. 根据权利要求26所述的分散染料,其特征在于,所述辅料包括助剂和水。
  28. 根据权利要求27所述的分散染料,其特征在于,所述助剂包括以下的一种或两种以上的组合:萘系磺酸甲醛缩合物、木质素磺酸盐、硫酸钠、表面活性剂、杀菌剂,或其他染料分散剂。
  29. 根据权利要求27或28所述的分散染料,其特征在于,所述助剂与分散染料组合物的重量之比为0.3~4:1。
  30. 根据权利要求26~29中任一项所述的分散染料,其特征在于,所述分散染料用砂磨机或研磨机研磨后为液状,固含量为20~50%,或者所述分散染料喷雾干燥后为粉状或颗粒状,固含量为87~96%。
  31. 一种制备根据权利要求26~30中任一项所述的分散染料的方法,其特征在于,包括以下步骤:
    将所述各染料组分混合后,在辅料的存在下用砂磨机或研磨机进行粒子化处理;或者将所述各染料组分分别在辅料存在下用砂磨机或研磨机进行粒子化处理,再进行混合。
  32. 一种根据权利要求26~30中任一项所述的分散染料用于织物的染色和印花的用途。
  33. 一种织物,其特征在于,通过使用根据权利要求26~30中任一项所述的分散染料进行染色和印花制备得到。
PCT/CN2014/095585 2013-12-30 2014-12-30 一种分散染料组合物、分散染料及其的制备方法和用途 WO2015101290A1 (zh)

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