CN107460557A - A kind of fibrous raw material coloring agent and preparation method thereof - Google Patents
A kind of fibrous raw material coloring agent and preparation method thereof Download PDFInfo
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- CN107460557A CN107460557A CN201710867531.4A CN201710867531A CN107460557A CN 107460557 A CN107460557 A CN 107460557A CN 201710867531 A CN201710867531 A CN 201710867531A CN 107460557 A CN107460557 A CN 107460557A
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- coloring agent
- carbon black
- raw material
- deionized water
- fibrous raw
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of fibrous raw material coloring agent and preparation method thereof, the fibrous raw material coloring agent is made up of the component of following mass percents：Carbon black 20-35%, lignosulphonates 3-8%, dispersant 3-8%, flow ability modifying agent 1-4%, carbon disulfide 5-13%, methacryloxypropyl 3-6%, surplus are deionized water.Of the invention one is that can prevent carbon black particle from flocculation and sedimentation occurs, and the fibrous raw material coloring agent of preparation can be made uniformly to be mixed before spinning with fiber stoste, solves the problems such as big, the scattered uneven and poor fluidity of carbon black particle particle in the prior art.Second, by the carbon black by Secondary Organicization processing has been carried out into addition fiber stoste, fiber stoste can more be dyed uniform high-efficiency, the fiber produced and the fiber into silk poststaining, it is completely the same with the intensity of silk and other physical and chemical performances on color, but the consumption of coloring agent and the pollution very little to environment.
Description
Technical field
The invention belongs to chemical field, relates in particular to a kind of fibrous raw material coloring agent and preparation method thereof.
Background technology
Traditional textile and dyeing industry will expend that a large amount of chemicals, supply and demand step are more, the process time is long, waste water is more, environment
It is seriously polluted.The 3E systems that Europe is advocated for many years（Efficiency, economy, ecology）, 3R production mechanisms（It is right-first-time, quick anti-
Ying Xing, reappear row）, 4R principles（Saving, recovery, reuse, circulation）The main flow of world's Dyeing ＆ Finishing Industry technology development is turned into.It is adjoint
Industrial development and caused a large amount of " three wastes " discharge causes serious destruction to human environment.Future society is wanted to textile industry
Ask in addition to the content of this invariability of product quality, more emphasize the ecological balance and the compatibility to environment." Green Textile Base
Product " and " green processing technologies " have turned into the key technology of this century printing and dyeing industry development.Solves the fundamental way of printing and dyeing pollution
It is the generation for reducing pollution, that is, reduces the generation of waste water, waste gas and harmful chemicals.This just needs to develop high-new textile dyeing and finishing
Process technology, while chemical fibre, weaving, printing and dyeing and chemical industry whole system should also be considered, it can be only achieved and effectively solve pollution problem.
Traditional colouring method is after fabric is made in fiber, is dyed by dyeing method.The coloring agent in China is most
Just it is applied to building coating industry, is progressively extended to the industries such as weaving, industrial coating, papermaking, latex later.As coloring agent is given birth to
Production enterprise constantly strengthens research and development and more progressively understandings of the downstream industry to coloring agent, the application field of coloring agent are constantly opened up
Exhibition.Appearance without dye fibre technology opens new application market for coloring agent.In recent years it is with high-quality slurry without dye fiber to rise
The dregs of rice and environment-friendly colorant are raw material, and coloring agent is uniformly mixed with spinning solution using injection technique before spinning, passes through Wet-spinning
A kind of natural, environmental protection colored fibre cellulose fiber of silk technique productions.Rich colors and clean manufacturing are realized without dye fiber
Highly merge, fundamentally realize green fiber, green production, guiding modern textile industry enters " no the to contaminate low dye " epoch.With
Traditional fibre staining technique is compared, the colored fiber that no dye fibre technology can not only assign preparation good sun-resistant, antifriction
Wipe, it is resistance to soap, the features such as permeability is high, and eliminate the dyeing link of downstream product, reduce the energy and water resource
Consumption, technique of no dye fiber in its whole production procedure all meet requirement of the world today to environmental protection.Without dye fiber
Yield makes great progress during " 11 " five.Original liquid coloring fiber total amount was brought up to by 114.8 tons in 2005
2010 242.2 ten thousand tons, account for the 7.8% of chemical fibre total amount at that time.Carbon black dyeing agent is dosage is bigger in all coloring agents one
Kind, if all tradition are all changed to use carbon black dyeing agent using carbon black toner to the enterprise of product coloring and improvement performance,
Carbon black dyeing agent dosage occupies primary position in all coloring agents.There are the very conservative prediction of data, the city of domestic carbon black
Field demand will increase to 1,220,000 tons by 630,000 in 2000 tons to 2015, and annual progressive increase rate is 6.2%, in fact by current
From the point of view of the usage amount of domestic carbon black, considerably beyond this amplification.
It will be applied to colour before fiber is spun without dye fiber carbon black dyeing agent, and realize fiber without dyeing technique, usual manner is logical
It is dispersed with stirring before crossing the preceding injection of spinning or stoste deaeration to reach, but it is big due to injecting coloring agent particle before spinning of the prior art,
And viscosity of viscose glue medium itself is high, the Brownian movement of carbon black particle is hindered again and slow down interparticle collision, causes to dye
Agent disperses and poor mobile performance, not only have impact on fibre staining uniformity, also results in fibre spinning and be difficult to, seriously constrain
Development without dye fiber industry.
For above-mentioned technical problem, propose in the prior art to the improvement without dye fiber carbon black dyeing agent, such as China specially
Sharp number " 201310742922.5 " disclosed fiber original liquid coloring superfine carbon black aqueous color paste, its technology on April 9th, 2014
Scheme is that the aqueous carbon black mill base is made up of modified carbon black, dispersant, organic solvent and deionized water, wherein the Modified Activated Carbon
It is black to account for the 15.0 ~ 40.0% of the fiber original liquid coloring superfine carbon black aqueous color paste gross mass, the dispersant and modified carbon black
Mass ratio is 0.15:1~0.3:1, the organic solvent accounts for the fiber original liquid coloring superfine carbon black aqueous color paste gross mass
5.0 ~ 15.0%, surplus is deionized water；Wherein described modified carbon black is modified by surface-modified dose of surface of carbon black and obtains, described
Surface modifier is at least one of 4- anilinesulfonic acids, stearmide and barbital, and its dosage is carbon black mass
2.0 ~ 5.0%；The dispersant be by N- dodecyls iminodipropionate and aliphatic amine polyoxyethylene ether in mass ratio
For 1:2~1:The mixture of 5 compositions.But in actual application, the carbon black color paste in the patent passes through repeatedly grinding to component
Grind, but it just for the sake of improving self-characteristic, when it is mixed with fiber stoste, carbon black particle can condense or roll into a ball
It is poly-, form the aggregated particle for being several times as much as primary partical size.And the spinneret orifice diameter of viscose rayon is 0.08-0.09 millimeter, phase
The solia particle critical dimension answered be 3-4 microns, when the particle size of cohesion exceedes critical dimension, will cause partly or
All block spray orifices, so cause to occur fiber number not uniform broken end the problem of.In addition, cohesion or the carbon black particle reunited occurs,
It can also influence to strive the mixed effect of each component in slurry and easily influence the uniformity coloured.
The content of the invention
It is an object of the invention to solve the above-mentioned problems in the prior art, there is provided a kind of fibrous raw material coloring agent and
Its preparation method, the present invention one is can to prevent carbon black particle from flocculation and sedimentation occurs, and can dye the fibrous raw material of preparation
Agent uniformly mixes with fiber stoste before spinning, solves that carbon black particle particle in the prior art is big, disperses uneven and mobility
The problems such as difference.Second, by the carbon black by Secondary Organicization processing has been carried out to adding in fiber stoste, can be more uniformly high
Effect ground dyes to fiber stoste, the fiber produced and the fiber into silk poststaining, the intensity with silk and other things on color
Physicochemical performance is completely the same, but the consumption of coloring agent and the pollution very little to environment.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of fibrous raw material coloring agent, it is characterised in that be made up of the component of following mass percents：Carbon black 20-35%, lignin
Sulfonate 3-8%, dispersant 3-8%, flow ability modifying agent 1-4%, carbon disulfide 5-13%, the second of methacryloxypropyl three
TMOS 3-6%, surplus are deionized water.
The dispersant is APEO.
The flow ability modifying agent is ethanol.
A kind of preparation method of fibrous raw material coloring agent, it is characterised in that comprise the following steps：
（1）Deionized water is divided into three parts, takes first part of deionized water to be connect with carbon black and lignosulphonates in twin-tub reactor
Branch is copolymerized into emulsion；
（2）Emulsion, second part of deionized water, dispersant and flow ability modifying agent are added in grinder and are ground into carbon black pellet
External diameter is 300-600nm thick liquid；
（3）3rd part of deionized water, carbon disulfide and methacryloxypropyl are added to thick liquid
In, and at normal temperatures, stirred 10-20 minutes with 800-1000 revs/min of rotating speed, obtain fibrous raw material coloring agent.
First part of deionized water accounts for 60-the 70% of ion water inventory, and second part of deionized water accounts for removing
40-the 45% of remaining deionized water total amount after a deionized water.
Using the advantage of the invention is that：
First, in the present invention, because carbon black particle generation flocculation is mainly molecular separating force, therefore appropriate gather is added in coloring agent
Oxygen vinethene is used as dispersant, and carbon black particle surface can be made to be wrapped up by dispersant, can be in carbon black particle and liquid circle
Form electric double layer on face, carbon black particle repels because of the charge consistent of surface, and flocculation ability and surely is reduced so as to reach
Surely scattered purpose.Add appropriate ethanol in coloring agent to use as flow ability modifying agent, it is possible to increase carbon black chemical modification
Effect.By the cooperation of APEO and ethanol, with regard to that can make coloring agent that there is good chemical stability, can improve and viscose glue
In the compatibility of other components and the ability of anti-external environment, so as to for dispersed in coloring agent of carbon black and realize fine
Tie up uniform coloring and powerful guarantee is provided.Also, carbon disulfide is the solvent of viscose rayon, it has good dissolubility, favorably
It in the quick dissolving of carbon black and scattered, while can ensure that the stabilization of the dispersion effect of carbon black is more preferable, therefore, add in coloring agent
Add appropriate carbon disulfide that coloring agent can be made uniformly to be mixed before spinning with fiber stoste, realize stoste and phase of the coloring agent without layering
Dissolubility.And appropriate lignosulphonates, methacryloxypropyl are added in coloring agent, then it can enter
The secondary carbon black of row is organised structure, and organic modification is carried out to carbon black, and then obtains appropriate amphipathic organic of organic degree
Change carbon black.And by carried out Secondary Organicization processing carbon black to add fiber stoste in, then can more uniform high-efficiency it is right
Fiber stoste dyes, the fiber produced and the fiber into silk poststaining, the intensity with silk and other physical chemistry on color
Performance is completely the same, but the consumption of coloring agent and the pollution very little to environment.With China Patent No. " 201310742922.5 "
Compared for the prior art of representative, the present invention not only solves that carbon black particle particle in the prior art is big, scattered uneven and stream
The problems such as dynamic property difference, also greatly improved dyeability.
2nd, in the present invention, graft copolymerization is carried out to inorganic matter carbon black so that the coloring agent to organise is easier with gluing
Glue fiber raw material merges, and coloring jail, is not easy to decolourize, in viscose glue during the stoste of liquid is transformed into silk, is not easily blocked spinneret
Hole, raising can anti-property, while formed silk strength will not reduce.
3rd, the present invention in, by grinder grind carbon black can to carbon black carry out physical modification, with it is above-mentioned can be to carbon black
The ethanol for carrying out chemical modification is engaged, it becomes possible to and it is dual modified to carbon black progress, by dual modified, it becomes possible to further carry
The preparation quality of high coloring agent.In addition, when the external diameter after carbon black grinding is more than 600nm, spinneret hole plug will likely result in；When
When external diameter after carbon black grinding is less than 300nm, milling time will be extended, grinding was both uneconomical for a long time excessively, also easily ground
Honed head, meanwhile, meticulous carbon black particle is very unstable, easily re-unites, re-forms aggregated particle.Therefore, by carbon black
It is 300-600nm particles to be ground into external diameter, both meets spinning requirement, and and can makes carbon black particle have good optical property.
4th, in the present invention, addition and lignosulphonates, carbon disulfide and methacryloxypropyl three in coloring agent
Ethoxysilane, the use of deionized water can be also reduced, for example, the carbon disulfide that addition mass percent is 5-13%, can subtract
Few mass percent is 5%-7% amount of deionized water, and adds the methacryloxypropyl that mass percent is 3-6%
Triethoxysilane, then it can reduce mass percent and be 15%-17% amount of deionized water, and add mass percent as 3-8%
, then the amount of deionized water that mass percent is 10% -15% can be reduced, significantly reduces the usage amount of water.
Embodiment
Embodiment 1
A kind of fibrous raw material coloring agent, is made up of the component of following mass percents：Carbon black 20%, lignosulphonates 3%, dispersant
3%, flow ability modifying agent 1%, carbon disulfide 5%, methacryloxypropyl 3%, surplus is deionized water, its
In, the dispersant is APEO, and the flow ability modifying agent is ethanol.
A kind of preparation method of fibrous raw material coloring agent, after being stocked up by above-mentioned mass percent, then prepare as follows
Fibrous raw material coloring agent：
（1）Deionized water is divided into three parts, first part of deionized water accounts for the 60% of ion water inventory, and second part of deionized water accounts for
The 40% of remaining deionized water total amount, then takes first part of deionized water and carbon black and lignin sulphur after first part of deionized water of removing
Hydrochlorate in twin-tub reactor graft copolymerization into emulsion；
（2）Emulsion, second part of deionized water, dispersant and flow ability modifying agent are added in grinder and are ground into carbon black pellet
External diameter is 300nm thick liquid；
（3）3rd part of deionized water, carbon disulfide and methacryloxypropyl are added to thick liquid
In, and at normal temperatures, stirred 10 minutes with 800 revs/min of rotating speed, obtain fibrous raw material coloring agent.
It the experiment proved that, after the component using above-mentioned extra fine quality percentage, the fibrous raw material coloring agent of preparation can reach
To following index：Solid content（%）：19-21, particle diameter（μm）：≤ 1.9, pH value：7-9, viscosity（mpa.s）：100-280, mistake
Filter the time (s)：≤ 10, filter residue（%）：≤ 3, the overall performance of fibrous raw material coloring agent greatly improves.
Embodiment 2
A kind of fibrous raw material coloring agent, is made up of the component of following mass percents：Carbon black 35%, lignosulphonates 8%, dispersant
8%, flow ability modifying agent 4%, carbon disulfide 13%, methacryloxypropyl 6%, surplus is deionized water,
Wherein, the dispersant is APEO, and the flow ability modifying agent is ethanol.
A kind of preparation method of fibrous raw material coloring agent, after being stocked up by above-mentioned mass percent, then prepare as follows
Fibrous raw material coloring agent：
（1）Deionized water is divided into three parts, first part of deionized water accounts for the 70% of ion water inventory, and second part of deionized water accounts for
The 45% of remaining deionized water total amount, then takes first part of deionized water and carbon black and lignin sulphur after first part of deionized water of removing
Hydrochlorate in twin-tub reactor graft copolymerization into emulsion；
（2）Emulsion, second part of deionized water, dispersant and flow ability modifying agent are added in grinder and are ground into carbon black pellet
External diameter is 600nm thick liquid；
（3）3rd part of deionized water, carbon disulfide and methacryloxypropyl are added to thick liquid
In, and at normal temperatures, stirred 20 minutes with 1000 revs/min of rotating speed, obtain fibrous raw material coloring agent.
It the experiment proved that, after the component using above-mentioned extra fine quality percentage, the fibrous raw material coloring agent of preparation can reach
To following index：Solid content（%）：20-21, particle diameter（μm）：≤ 2, pH value：7-9, viscosity（mpa.s）：100-300, filtering
Time (s)：≤ 10, filter residue（%）：≤ 3, the overall performance of fibrous raw material coloring agent greatly improves.
Embodiment 3
A kind of fibrous raw material coloring agent, is made up of the component of following mass percents：Carbon black 27%, lignosulphonates 5%, dispersant
5%, flow ability modifying agent 2%, carbon disulfide 9%, methacryloxypropyl 5%, surplus is deionized water, its
In, the dispersant is APEO, and the flow ability modifying agent is ethanol.
A kind of preparation method of fibrous raw material coloring agent, after being stocked up by above-mentioned mass percent, then prepare as follows
Fibrous raw material coloring agent：
（1）Deionized water is divided into three parts, first part of deionized water accounts for the 65% of ion water inventory, and second part of deionized water accounts for
The 42% of remaining deionized water total amount, then takes first part of deionized water and carbon black and lignin sulphur after first part of deionized water of removing
Hydrochlorate in twin-tub reactor graft copolymerization into emulsion；
（2）Emulsion, second part of deionized water, dispersant and flow ability modifying agent are added in grinder and are ground into carbon black pellet
External diameter is 450nm thick liquid；
（3）3rd part of deionized water, carbon disulfide and methacryloxypropyl are added to thick liquid
In, and at normal temperatures, stirred 15 minutes with 900 revs/min of rotating speed, obtain fibrous raw material coloring agent.
It the experiment proved that, after the component using above-mentioned extra fine quality percentage, the fibrous raw material coloring agent of preparation can reach
To following index：Solid content（%）：19-20, particle diameter（μm）：≤ 1.8, pH value：7-8, viscosity（mpa.s）：120-280, mistake
Filter the time (s)：≤ 10, filter residue（%）：≤ 3, the overall performance of fibrous raw material coloring agent greatly improves.
Claims (5)
1. a kind of fibrous raw material coloring agent, it is characterised in that be made up of the component of following mass percents：Carbon black 20-35%, wood
Plain sulfonate 3-8%, dispersant 3-8%, flow ability modifying agent 1-4%, carbon disulfide 5-13%, methacryloxypropyl three
Ethoxysilane 3-6%, surplus are deionized water.
A kind of 2. fibrous raw material coloring agent as claimed in claim 1, it is characterised in that：The dispersant is APEO.
A kind of 3. fibrous raw material coloring agent as claimed in claim 1, it is characterised in that：The flow ability modifying agent is ethanol.
A kind of 4. preparation method of fibrous raw material coloring agent as any one of claim 1-3, it is characterised in that including
Following steps：
（1）Deionized water is divided into three parts, takes first part of deionized water to be connect with carbon black and lignosulphonates in twin-tub reactor
Branch is copolymerized into emulsion；
（2）Emulsion, second part of deionized water, dispersant and flow ability modifying agent are added in grinder and are ground into carbon black pellet
External diameter is 300-600nm thick liquid；
（3）3rd part of deionized water, carbon disulfide and methacryloxypropyl are added to thick liquid
In, and at normal temperatures, stirred 10-20 minutes with 800-1000 revs/min of rotating speed, obtain fibrous raw material coloring agent.
A kind of 5. preparation method of fibrous raw material coloring agent as claimed in claim 4, it is characterised in that：Described first part go from
Sub- water accounts for 60-the 70% of ion water inventory, second part of deionized water account for remove residue after first part of deionized water go from
40-the 45% of sub- water inventory.
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| CN201710867531.4A CN107460557A (en) | 2017-09-22 | 2017-09-22 | A kind of fibrous raw material coloring agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084803A (en) * | 2017-12-25 | 2018-05-29 | 荆州市江汉精细化工有限公司 | A kind of preparation method of silane-modified carbon black color paste |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1465759A (en) * | 2002-06-28 | 2004-01-07 | 中国石化上海石油化工股份有限公司 | Method for preparing colorant used in mass coloration of acrylic fibre spinning |
| CN103556301A (en) * | 2013-10-18 | 2014-02-05 | 江南大学 | Method for coloring alginate fibers by nano pigment |
| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
-
2017
- 2017-09-22 CN CN201710867531.4A patent/CN107460557A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1465759A (en) * | 2002-06-28 | 2004-01-07 | 中国石化上海石油化工股份有限公司 | Method for preparing colorant used in mass coloration of acrylic fibre spinning |
| CN103556301A (en) * | 2013-10-18 | 2014-02-05 | 江南大学 | Method for coloring alginate fibers by nano pigment |
| CN105463601A (en) * | 2014-08-26 | 2016-04-06 | 中国石油化工股份有限公司 | Acrylic pigment slurry, preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084803A (en) * | 2017-12-25 | 2018-05-29 | 荆州市江汉精细化工有限公司 | A kind of preparation method of silane-modified carbon black color paste |
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