[go: up one dir, main page]

CN102675916B - Nano disperse black combined dye and preparation method thereof - Google Patents

Nano disperse black combined dye and preparation method thereof Download PDF

Info

Publication number
CN102675916B
CN102675916B CN2012101352511A CN201210135251A CN102675916B CN 102675916 B CN102675916 B CN 102675916B CN 2012101352511 A CN2012101352511 A CN 2012101352511A CN 201210135251 A CN201210135251 A CN 201210135251A CN 102675916 B CN102675916 B CN 102675916B
Authority
CN
China
Prior art keywords
dye
nano
dyestuff
grinding
dyes
Prior art date
Legal status (The legal status 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 status listed.)
Active
Application number
CN2012101352511A
Other languages
Chinese (zh)
Other versions
CN102675916A (en
Inventor
刘越
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Shaoxing
Original Assignee
University of Shaoxing
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.)
Filing date
Publication date
Application filed by University of Shaoxing filed Critical University of Shaoxing
Priority to CN2012101352511A priority Critical patent/CN102675916B/en
Publication of CN102675916A publication Critical patent/CN102675916A/en
Application granted granted Critical
Publication of CN102675916B publication Critical patent/CN102675916B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Coloring (AREA)

Abstract

本发明公开了一种纳米分散黑组合染料及其制备方法，涉及染料及中间体工业加工领域。包括染料与助剂，染料与助的质量比为1:1-4.5，染料为式Ⅰ所示化合物的一种或几种；助剂为阴离子表面活性剂和非离子表面活性剂按照质量比100%—85%：0%—15%混合而成；

Figure 2012101352511100004DEST_PATH_IMAGE002
式Ⅰ；式Ⅰ中：R1为H、CI、Br或CN；R2为H、CI或NO2；R3为H或OCH3；R4为H或NHCOCH3；R5、R6分别为相互独立的C2H5、C2H4OCOCH3、C2H4OCH3或C2H4CN。本发明的纳米分散黑组合染料，同样染色条件下与常规黑色分散染料涤纶织物染色相比较：织物的L值减少了21.3%，K/S值提高了18.6%。The invention discloses a nano-disperse black combined dye and a preparation method thereof, and relates to the field of industrial processing of dyes and intermediates. Including dyes and auxiliaries, the mass ratio of dyes and auxiliaries is 1:1-4.5, the dyes are one or more of the compounds shown in formula I; the auxiliaries are anionic surfactants and nonionic surfactants according to the mass ratio of 100 %—85%: 0%—15% mixed;
Figure 2012101352511100004DEST_PATH_IMAGE002
Formula I; in formula I: R 1 is H, CI, Br or CN; R 2 is H, CI or NO 2 ; R 3 is H or OCH 3 ; R 4 is H or NHCOCH 3 ; R 5 and R 6 are respectively are independently C 2 H 5 , C 2 H 4 OCOCH 3 , C 2 H 4 OCH 3 or C 2 H 4 CN. Compared with the dyeing of polyester fabric with conventional black disperse dyes under the same dyeing conditions, the nano-disperse black combined dye of the present invention: the L value of the fabric is reduced by 21.3%, and the K/S value is increased by 18.6%.

Description

The black combination of a kind of nano-dispersed dye well its preparation method
Technical field:
The present invention relates to dye well intermediate industry manufacture field, be specially the black combination of a kind of nano-dispersed dye well its preparation method.
Background technology:
Polyster fibre (polyethylene terephthalate) macromolecular chain marshalling, degree of crystallinity is also larger, and do not contain hydroxyl, amino and sodium sulfonate class water absorbability group on macromolecular chain structure, the moisture regain of fiber is only 0.4%, therefore, polyester piece good can not dye with water-soluble dye, but adopts the dispersed dye of the nonpolar structure of small molecules to complete painted in modes such as high-temperature pressure dyeing, pad-dry-cure dyeing or carrier dyeings.
Polyester piece good dyes the dispersed black dye that black is used at present, mainly to be formed by several different dispersed dye blendings according to the dyestuff color matching theory, dye particle is larger, and how between 1 μ m-2 μ m, larger grain diameter is unfavorable for the adsorption and diffusion of dyestuff in polyster fibre.From dye level,, according to the dyeing of present routine, dye to obtain the darker color of the black degree of depth, larger difficulty is still arranged, can not meet the market requirement.
, for solving the problems of the technologies described above, make the present invention.
Summary of the invention:
Based on above-mentioned requirements, a first aspect of the present invention purpose is to provide the black combination of a kind of nano-dispersed dye well its preparation method, be intended to by forming the selection of each related component kind of black dyes and ratio, by the application of high temperature resistant composite dye dispersant and the improvement of processing technology, prepare a kind of nanoscale dispersed dye that can dye the higher black degree of depth of system, further increase the black expression power that dyes the black terylene fabric product.
For achieving the above object, the technical scheme of taking is as follows:
The black combination of a kind of nano-dispersed dyestuff is characterized in that: comprise dyestuff and auxiliary agent, dyestuff is 1:1-4.5 with the mass ratio that helps, and dyestuff is one or more of compound shown in the formula I; Auxiliary agent is that anion surfactant and nonionogenic tenside mix according to mass ratio 100%-85%:0%-15%;
Figure 2012101352511100002DEST_PATH_IMAGE001
The formula I;
In the formula I: R 1For H, CI, Br or CN; R 2For H, CI or NO 2R 3For H or OCH 3R 4For H or NHCOCH 3R 5, R 6Be respectively separate C 2H 5, C 2H 4OCOCH 3, C 2H 4OCH 3Or C 2H 4CN.
Further arrange and be:
Described dyestuff comprises dyestuff A, dyestuff B, dyestuff C, and the mass ratio of dyestuff A, dyestuff B, dyestuff C is 87.5%-57%:12%-35%:0.5%-8%; Wherein: dyestuff A is formed by the one or more combination in the dyestuff of following structure:
Figure 442196DEST_PATH_IMAGE002
A-Ⅰ；
Figure 2012101352511100002DEST_PATH_IMAGE003
A-Ⅱ；
Figure 549217DEST_PATH_IMAGE004
A-Ⅲ；
Dyestuff B is formed by the one or more combination in the dyestuff of following structure:
Figure 2012101352511100002DEST_PATH_IMAGE005
B-Ⅰ；
Figure 328954DEST_PATH_IMAGE006
B-Ⅱ；
Figure DEST_PATH_IMAGE007
B-Ⅲ；
Figure 661846DEST_PATH_IMAGE008
B-Ⅳ；
Figure DEST_PATH_IMAGE009
B-Ⅴ；
Dyestuff C is formed by the one or more combination in the dyestuff of following structure:
Figure 476219DEST_PATH_IMAGE010
C-Ⅰ；
Figure DEST_PATH_IMAGE011
C-Ⅱ；
Figure 485632DEST_PATH_IMAGE012
C-Ⅲ；
Figure DEST_PATH_IMAGE013
C-Ⅳ。
Described anion surfactant is selected from one or both in sulfonated lignin, naphthalenesulfonate formaldehyde condensation compound, methyl naphthalene sulfonic acid salt formaldehyde condensation products, benzyl naphthalene sulfonic formaldehyde condensation compound and phenolic condensation compound sulfonate; Be particularly preferably one or both of sodium lignosulfonate, dispersion agent NNO, Dispersant MF, dispersing agent C NF.
Described nonionogenic tenside is selected from any one in polyoxyethylene glycol, polyoxyethylene sorbitan fatty acid ester, Soxylat A 25-7 and oxyethane polycondensate.
A second aspect of the present invention purpose is to provide the preparation method of the black combination of a kind of nano-dispersed dyestuff, it is characterized in that: dyestuff is mixed with the mass ratio of auxiliary agent according to 1:1-4.5, through sizing mixing, ultrasonic, grinding, homogeneous, spraying drying process the black combination of nano-dispersed dyestuff.
Further:
Dyestuff is mixed according to mass ratio 1:1-4.5 with auxiliary agent, add pure water to be modulated into the pulpous state premix, after this premix supersound process 20min-60min, send into the grinding of Mechanical Sealed Type ball mill and coated dispersion processing in 4-6 hour, grind and adopt circulating grinding technics, screen cloth separation system screen cloth used is 0.13mm nickel material, grinding bead is the zirconium white of 0.5mm particle diameter, the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is completed, the lapping liquid high pressure homogenizing is processed, more spray-dried processing namely obtains the black combination of nano-dispersed dyestuff.
Beneficial effect of the present invention is as follows:
The black combination of nano-dispersed provided by the invention dyestuff, being conducive to terylene absorbs and can obtain more aterrimus Color, with the high-temperature pressure dyeing dyeing, compare with the conventional black disperse dye polyester piece good dyeing under same dyeing condition, having reduced 21.3%(with the black L value that makes up the polyester piece good of dyeing of nano-dispersed is that the black depth value has increased by 21.3%), the K/S value has improved 18.6%, and the polyester piece good dyeing uniformity is good, and coloured light is pure.The present invention, for exploitation nanometer particle size dispersed black dye, meets aterrimus Polyester Textiles dyeing processing and has higher realistic meaning with the demand of dyestuff.
The invention will be further described below in conjunction with embodiment.
Embodiment:
Preparation Example:
With dyestuff and auxiliary agent according to certain mass than mixing, add water and be modulated into the pulpous state premix, after this premix supersound process 20min-60min, send into the grinding of Mechanical Sealed Type ball mill and coated dispersion processing in 4-6 hour, grind and adopt circulating grinding technics, screen cloth separation system screen cloth used is 0.13mm nickel material, grinding bead is the zirconium white of 0.5mm particle diameter, the grinding bead consumption is the 200%-500% of grinding material quality, after grinding is completed, the lapping liquid high pressure homogenizing is processed, more spray-dried processing namely obtains the black combination of nano-dispersed dyestuff.
According to above-mentioned Preparation Example, adjust different dyes and auxiliary agent proportioning, obtain following embodiment:
Embodiment 1:
The component A, the 10.5g structural formula that with the 37.5g structural formula are (A-I) are component C, the 90g sodium lignosulfonate of (C-I) for B component, the 2g structural formula of (B-I), after adding water 260g mixing, make premix through stirring, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the nano-dispersed dyestuff of 15nm-100nm.
Embodiment 2-16:
According to each component concentration ratio data shown in table 1, with 50g component A, B component, component C and 90g auxiliary agent, add after water 260g mixes and make premix through agitation as appropriate, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the commercialization nano-dispersed dyestuff of 15nm-100nm.
Each component of table 1, embodiment 2-16 combination dyestuff forms.
Figure DEST_PATH_IMAGE015
Embodiment 17:
With the 34g structural formula for the component A of (A-I), 13g structural formula for the B component of (B-I), 3g structural formula for the mixture of the component C of (C-I), 90g sodium lignosulfonate and dispersion agent NNO, add water 260g and mix and make premix by stirring, afterwards according to Preparation Example, make that fastness is good, particle diameter is at the black combination of the nano-dispersed dyestuff of 15nm-100nm.
Performance Detection:
The black combination of nano-dispersed dyestuff with embodiment 1-17 preparation, dye according to following dyeing:
Dyeing flow process: polyester piece good → concise pre-treatment → dehydration → oven dry → pre-setting → dyeing → washing → reduction clearing → washing → oven dry.
Dyeing prescription:
The black combination of nano-dispersed dyestuff: 3.5%(owf, with respect to the quality of polyester piece good);
Acetic acid: 0.5g/l, the adjusting dye liquor pH value is 4.5-5.0;
Bath raio: 30:1;
Dyeing temperature: 130 ℃;
Dyeing time: 60min.
The dyeing aftertreatment: after dyeing polyester piece good first through washing, then use 1.0g/l concentration reduction clearing liquid at 80 ℃ of lower carrying out washing treatment 10 min, wash afterwards, dry.
The polyester piece good of with the nano-dispersed of the present invention's preparation, deceiving after tested, the combination dyeing: fastness to wet rubbing is 5 grades, and dry fastness is 5 grades, and soaping fastness is the 4-5 level, and the variable color fastness of soaping is the 4-5 level.Compare through the conventional black disperse dye polyester piece good dyeing with under same dyeing condition: it is that the black degree of depth has increased by 21.3% that the L value of fabric has reduced 21.3%(), the K/S value has improved 18.6%, and the polyester piece good dyeing uniformity is good, and coloured light is pure.

Claims (2)

1.一种纳米分散黑组合染料，其特征在于：包括染料与助剂，染料与助剂的质量比为1:1-4.5，所述染料包括染料A、染料B、染料C，染料A、染料B、染料C的质量比为87.5%—57%：12%—35%：0.5%—8%；所述助剂为阴离子表面活性剂和非离子表面活性剂按照质量比100%—85%：0%—15%混合而成； 1. a nano-disperse black combination dye is characterized in that: comprise dyestuff and auxiliary agent, the mass ratio of dyestuff and auxiliary agent is 1:1-4.5, and described dyestuff comprises dyestuff A, dyestuff B, dyestuff C, dyestuff A, The mass ratio of dye B and dye C is 87.5%-57%: 12%-35%: 0.5%-8%; the auxiliary agent is anionic surfactant and nonionic surfactant according to the mass ratio of 100%-85% : 0% - 15% mixed; 其中：染料A是由以下结构的染料中的一种或几种组合而成： Wherein: Dye A is formed by one or more combinations of dyes with the following structures:
Figure 2012101352511100001DEST_PATH_IMAGE002
Figure 2012101352511100001DEST_PATH_IMAGE002
   A-Ⅰ； A-I;
Figure 2012101352511100001DEST_PATH_IMAGE004
Figure 2012101352511100001DEST_PATH_IMAGE004
 A-Ⅱ； A-II;
Figure 2012101352511100001DEST_PATH_IMAGE006
Figure 2012101352511100001DEST_PATH_IMAGE006
 A-Ⅲ； A-Ⅲ; 染料B是由以下结构的染料中的一种或几种组合而成： Dye B is composed of one or a combination of dyes with the following structures:
Figure 2012101352511100001DEST_PATH_IMAGE008
 
Figure 2012101352511100001DEST_PATH_IMAGE008
  B-Ⅰ； B-I;
Figure DEST_PATH_IMAGE010
 
Figure DEST_PATH_IMAGE010
  B-Ⅱ； B-II;
Figure DEST_PATH_IMAGE012
 
Figure DEST_PATH_IMAGE012
  B-Ⅲ； B-Ⅲ;
Figure DEST_PATH_IMAGE014
Figure DEST_PATH_IMAGE014
 B-Ⅳ； B-IV;
Figure DEST_PATH_IMAGE016
Figure DEST_PATH_IMAGE016
 B-Ⅴ； B-V; 染料C是由以下结构的染料中的一种或几种组合而成： Dye C is composed of one or a combination of dyes with the following structures: C-Ⅰ； C-I; C-Ⅱ； C-II;
Figure DEST_PATH_IMAGE022
Figure DEST_PATH_IMAGE022
 C-Ⅲ； C-Ⅲ;
Figure DEST_PATH_IMAGE024
Figure DEST_PATH_IMAGE024
 C-Ⅳ。 C-IV. 2.根据权利要求1所述的一种纳米分散黑组合染料，其特征在于：所述的阴离子表面活性剂选自木质素磺酸盐、萘磺酸盐甲醛缩合物、甲基萘磺酸盐甲醛缩合物、苄基萘磺酸甲醛缩合物以及酚醛缩合物磺酸盐中的一种或两种。 2. a kind of nano-disperse black combined dye according to claim 1, is characterized in that: described anion surfactant is selected from lignosulfonate, naphthalenesulfonate formaldehyde condensate, methylnaphthalenesulfonate One or both of formaldehyde condensate, benzyl naphthalene sulfonic acid formaldehyde condensate and phenolic condensate sulfonate. 3、根据权利要求2所述的一种纳米分散黑组合染料，其特征在于：所述的阴离子表面活性剂选自木质素磺酸钠、分散剂NNO、分散剂MF、分散剂CNF的一种或两种。 3. A nano-disperse black combined dye according to claim 2, characterized in that: said anionic surfactant is selected from sodium lignosulfonate, dispersant NNO, dispersant MF, and dispersant CNF or two. 4、根据权利要求1所述的一种纳米分散黑组合染料，其特征在于：所述的非离子表面活性剂选自聚乙二醇、聚氧乙烯失水山梨醇脂肪酸酯、聚氧乙烯醚与环氧乙烷缩聚物中的任意一种。 4. A nano-disperse black combined dye according to claim 1, characterized in that: said nonionic surfactant is selected from polyethylene glycol, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene Any one of the condensation polymers of ether and ethylene oxide. 5、权利要求1-4任一项所述纳米分散黑组合染料的制备方法，其特征在于：将染料与助剂按照1:1-4.5的质量比混合，经调浆、超声、研磨、均质、喷雾干燥加工而成纳米分散黑组合染料。 5. The method for preparing the nano-disperse black combined dye according to any one of claims 1-4, characterized in that: the dye and the auxiliary agent are mixed according to the mass ratio of 1:1-4.5, and the mixture is mixed through pulping, ultrasonication, grinding, and homogenization. Quality, spray drying process into nano-disperse black combination dyes. 6、根据权利要求5所述纳米分散黑组合染料的制备方法，其特征在于：将染料与助剂按照质量比1:1-4.5混合，加入纯水调制成浆状预混合液，将该预混合液超声处理20min-60min后，送入机械密封式珠磨机研磨4-6小时进行包覆分散加工，研磨采用循环式研磨工艺，筛网分离系统所用筛网为0.13mm镍材质，研磨珠为0.5mm粒径的氧化锆，研磨珠用量为研磨物料质量的200%-500%，研磨完成后，将研磨液高压均质化处理，再经喷雾干燥加工即得纳米分散黑组合染料。 6. The preparation method of nano-disperse black combined dye according to claim 5, characterized in that: the dye and the auxiliary agent are mixed according to the mass ratio of 1:1-4.5, and pure water is added to prepare a slurry-like premixed liquid, and the premixed After ultrasonic treatment of the mixed solution for 20min-60min, it is sent to a mechanically sealed bead mill for grinding for 4-6 hours for coating and dispersion processing. The grinding adopts a circular grinding process. Zirconia with a particle size of 0.5mm, the amount of grinding beads is 200%-500% of the mass of the grinding material. After the grinding is completed, the grinding liquid is homogenized under high pressure, and then spray-dried to obtain the nano-dispersed black combined dye.
CN2012101352511A 2012-05-04 2012-05-04 Nano disperse black combined dye and preparation method thereof Active CN102675916B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2012101352511A CN102675916B (en) 2012-05-04 2012-05-04 Nano disperse black combined dye and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2012101352511A CN102675916B (en) 2012-05-04 2012-05-04 Nano disperse black combined dye and preparation method thereof

Publications (2)

Publication Number Publication Date
CN102675916A CN102675916A (en) 2012-09-19
CN102675916B true CN102675916B (en) 2013-11-20

Family

ID=46808496

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2012101352511A Active CN102675916B (en) 2012-05-04 2012-05-04 Nano disperse black combined dye and preparation method thereof

Country Status (1)

Country Link
CN (1) CN102675916B (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103937291B (en) * 2014-04-02 2016-07-27 上海贝通色彩科技有限公司 A kind of stamp Disperse black azo dye mixture and preparation method thereof
CN103965651B (en) * 2014-05-23 2016-04-20 约克夏染料（中山）有限公司 A kind of high washing fastness admixture of disperse dyes and application thereof
CN104151864A (en) * 2014-08-27 2014-11-19 广东省均安牛仔服装研究院 Preparation method of nano-scale indigo dye suspended matter
CN105113285B (en) * 2015-09-19 2018-01-05 苏州大学 A kind of pulp-shaped dispersed dyes and preparation method and application
CN105524487A (en) * 2015-12-03 2016-04-27 太湖亚太精化有限公司 Disperse dye composition and disperse dye and preparation method and application thereof
CN113831759A (en) * 2021-09-16 2021-12-24 浙江理工大学 A kind of liquid disperse dye for high temperature disperse dyeing and preparation method thereof

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0244337B2 (en) * 1983-07-22 1990-10-03 Mitsui Toatsu Chemicals MIZUFUYOSEIBUNSANSENRYOSOSEIBUTSU OYOBIKOREOMOCHIITAHORIESUTERUSENINOSENSHOKUMATAHANATSUSENHO
GB8805690D0 (en) * 1988-03-10 1988-04-07 Ici Plc Disperse dyes
US5505742A (en) * 1993-12-21 1996-04-09 Dystar Japan Ltd. Method for dyeing hydrophobic fibers black and dye useful for the method
DE19636380A1 (en) * 1996-09-09 1998-03-12 Dystar Textilfarben Gmbh & Co Disperse dye mixtures
CN100503740C (en) * 2007-01-05 2009-06-24 浙江龙盛染料化工有限公司 A kind of disperse black dye composition
CN102002259B (en) * 2010-11-04 2013-12-25 浙江闰土股份有限公司 High-fastness black and blue disperse dye composite
CN102653635A (en) * 2012-03-15 2012-09-05 江苏之江化工有限公司 Printing black disperse dyes

Also Published As

Publication number Publication date
CN102675916A (en) 2012-09-19

Similar Documents

Publication Publication Date Title
CN102675916B (en) Nano disperse black combined dye and preparation method thereof
CN101307191B (en) Disperse dye composition and disperse dyes
CN101792615A (en) Environment-friendly dark blue and black series compound disperse dye and production method thereof
CN103589190B (en) A kind of dispersion red dye composition
CN103740136A (en) High-fastness turquoise blue disperse dye composition
CN103113759A (en) Red disperse dye composition, and preparation method and application thereof
CN103571231A (en) Dark colored reactive dye with high fixation rate
CN106833018B (en) A kind of dispersed black dye mixture and its dye preparations
CN104530763B (en) Blue liquid disperse dyes and its preparation method and purposes
CN105111785A (en) Dark disperse dye composition and applications
CN111925667A (en) Dacron washing-free dye composition and preparation process and dyeing process thereof
CN102372932B (en) Disperse red dye composition
CN104087012B (en) The application of azo disperse dye goods
CN102516797B (en) Monoazo dye compound and orange to red dye composition
CN102443280B (en) Dispersed blue-to-black dye composition
CN100516144C (en) High humidity treatment fastness dispersible dye mixture and its product
CN105111787A (en) Disperse dye mixture and application thereof
CN107298875A (en) A kind of economic and environment-friendly type disperse dyes
CN103740135A (en) Low-temperature and environment-friendly disperse yellow dye composition
CN104448892B (en) A kind of sapphire blue dispersion dye of high washing fastness and sublimation reliability and preparation method thereof
CN104448926B (en) A kind of deep color dispersion dyes composition
CN104087013A (en) Preparation method of azo disperse dye product
CN100558821C (en) Composite disperse dye
CN107312357B (en) A kind of dark color azoic dye disperse dye composition
CN104448929A (en) Grey disperse dye compound, disperse dye and preparation method and usage of disperse dye

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant