CN109054442A - A kind of preparation method of environment-friendly high-intensity liquid disperse dyes - Google Patents
A kind of preparation method of environment-friendly high-intensity liquid disperse dyes Download PDFInfo
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- CN109054442A CN109054442A CN201811078650.2A CN201811078650A CN109054442A CN 109054442 A CN109054442 A CN 109054442A CN 201811078650 A CN201811078650 A CN 201811078650A CN 109054442 A CN109054442 A CN 109054442A
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- dyestuff
- disperse dyes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing 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
- C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
- C09B67/008—Preparations of disperse dyes or solvent dyes
- C09B67/0082—Preparations of disperse dyes or solvent dyes in liquid form
Abstract
The present invention relates to a kind of preparation methods of environment-friendly high-intensity liquid disperse dyes, belong to printing technology field.The present invention is concentrated by rotary evaporation dyestuff carrying out purification processes, remove the inorganic salts in dyestuff, stabilizing dye system, high strength fluid disperse dyes are prepared in conjunction with buffer solution, organic solvent and each analog assistant, a certain amount of nonionic surfactant is added in dyestuff, dye molecule can be made to form micella in water, there is preferable dispersibility, in the intermolecular netted solubilising of formation of cosolvent for constituting micella, dissolubility is improved;The catalyzing hydrolysis that proton reduces dyestuff can be absorbed in the addition of buffer solution, improves the stability of liquid dyes;The growth of dyestuff surface bacteria when chitosan effectively inhibits dyestuff to store in water is added in the present invention, prevent destruction of the bacterium to liquid disperse dyes, to stabilizing dye dispersion, the addition of anhydrous sodium sulphate, the intensity of dyestuff can be effectively improved, so that there is liquid disperse dyes high-intensitive and storage stability to improve.
Description
Technical field
The present invention relates to a kind of preparation methods of environment-friendly high-intensity liquid disperse dyes, belong to printing technology field.
Background technique
In recent years, as environmental problem is got worse, country is higher and higher to the requirement in terms of environmental protection, to textile printing and dyeing row
The regulation of industry is also increasingly stringenter, and there is an urgent need to the high-intensitive dyestuffs of energy-saving and emission-reduction for textile printing and dyeing enterprises.
Liquid dyes are to develop to process dosage form than faster dyestuff in recent years, since it is easy with production method, uses
The advantages that dyeability can be improved in easy to operate, energy-saving and emission-reduction, and by the great attention of printing and dyeing mill, development speed is very fast.
Liquid dyes are prepared with following features: 1, liquid dyes do not need the process such as dry, granulation, molding, therefore
Process equipment greatly simplifies, and production process is obviously shortened;2, the storage stability of liquid dyes is poor, is easy to produce precipitating, because
This requires reasonable selection dispersant with high efficiency and other matched addition auxiliary agents, more needs to the formulating of commodity, preparation process
It keeps on improving;3, it needs using advanced microemulsified, pulverize dispersion suspended substance processing technology, for water-insoluble dye
Material, can also produce and process stable liquid dyes dispersion by wet type superfine communication technique;4, it is particularly suitable for dispersion dye
The production and processing of material reduces impurity so that disperse dyes be made further to be purified processing, improves purity.
Liquid disperse dyes have following items basic demand: 1, the dispersion of liquid should be more stable, can be in longer-term
Time lower storage;2, there is good mobility, pump conveying can be used, can toppled over;3, it is easy at normal temperature or in cold water
It disperses or dissolves, it can or blending miscible with similar or other dyestuffs;4, noxious material is free of, PH is neutrality;5, it should mention as far as possible
High dye strength;6, a variety of dyeing and printing process are applicable to.
The advantages of liquid disperse dyes: 1, good application performance uses always powder in printing and dyeing industry for a long time
Shape, granular dyes, when sizing mixing or preparing dye liquor, dyestuff dust is most troubling problem, not only influences environment, hinders labor
Dynamic protection, and be often attached on the apparatus of ingredient or suspend in the dye liquor foam of preparation.Big not be dispersed or dissolved
The grain dyestuff that dyestuff, especially solubility are small, dispersion performance is poor, wettability and dispersion performance are all poor, are easy mutually to cohere
At agglomerate, it is easy that fabric is made to form fault in dyeing, influences product quality.And the above problem is substantially not present in liquid dyes,
The generation of dyeing defect can be significantly reduced.2, migration phenomenon is reduced, the migration of dyestuff is a problem deserving of attention, dyestuff
Migration degree is related with perhaps various factors.It is again mainly related with the content of auxiliary agent in dyestuff.It is related studies have shown that many points
Powder, wetting agent have the tendency that increasing dyestuff occurs migration.In liquid dyes processing formula, due to dispersing agent dosage compared with
Solid fraction dyestuff substantially reduce (as soon as correspond generally to liquid dyes five/or less), so also effectively reducing dyeing
Migration degree when post-process treatment;3, dye-uptake can be improved, some non-water soluble dyes, especially disperse dyes are washed in dye
When synthetic fibre or other synthetic fibers, grain fineness is important.Usual powdery, granular dyes are needed after being pulverized by drying process,
This just inevitably makes partial particulate generate cohesion, dispersion performance decline.Therefore, solid fraction dyestuff is thick compared with the particle of liquid dyes
Greatly, same amount of powder dye and liquid dyes hot melt dye terylene, as a result, upper dye of the liquid dyes than powder dye
Rate is high, and maximum differential can reach 50% or more sometimes.And hot melt when dyeing powder dye be also easy to produce fault, and liquid dyes
It but can be to avoid such problems;4, liquid dyes reduce production cost, and liquid dyes compare with solid fraction dyestuff, do not need drying
Process, also do not need dry grinding and dry blending process: this just substantially reduces the technological process of production.Drying is one in production
Highly energy-consuming operating process eliminates drying and just saves production cost, in addition, with water instead of part of auxiliary in liquid dyes
Use, largely also reduce cost of material, thus liquid dyes can be effectively reduced dyestuff cost of material and
Production cost;5, the COD in dyeing residual liquid is reduced, the dye dispersant as used in liquid dyes and other auxiliary agents are relatively
Few, allowing for COD content in dyeing residual liquid naturally reduces;6, the coloration for reducing dyeing residual liquid, due to liquid dyes dye uptake
Higher than powder dye, dyestuff remaining in raffinate is less after dyeing, and the coloration of raffinate is substantially reduced;7, with present labour city
The increased costs of field, more and more printing and dyeing enterprises have used automation process equipment, and liquid disperse dyes are particularly suitable for automatic
Change metering, obtains a large amount of application therewith.
The former dyestuff weight percent control range of liquid disperse dyes on existing market is 17.9%~36%, auxiliary agent
Weight percent control range is 4.5%~14.4%, auxiliary agent and former dyestuff weight percent control range are 0.25~0.4:
1, there are liquid dyes low strength, in application, there are a little limitations for printing and dyeing mill, and auxiliary agent content is higher, the color of raffinate after dyeing
Degree abs value, COD are higher, and there are no the purposes for really realizing optimal energy-saving and emission-reduction.
Summary of the invention
The technical problems to be solved by the invention: steady for the liquid disperse dyes low strength on existing market, storage
The problem of qualitative difference provides a kind of preparation method of environment-friendly high-intensity liquid disperse dyes.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
(1) in mass ratio 1: 6 dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered, obtain filtrate, filtrate is placed in rotation
Turn on evaporimeter, be concentrated by evaporation, obtain concentrate, acetone is added, be uniformly mixed, obtain precipitated liquid, filters to obtain precipitating, precipitating is placed in
It dries in 60~80 DEG C of baking oven to constant weight, is cooled to room temperature, grind up to sublimation dye;
(2) according to parts by weight, weigh respectively 50~60 parts of sublimation dyes, 10~16 parts of buffer solutions, 20~40 parts it is organic molten
Agent, 1~10 portion of nonionic surfactant, 1~5 part of ethylene glycol, 10~12 parts of mass fractions be 2% chitosan-acetic acid solution,
10~30 parts of anhydrous sodium sulphate, 80~100 parts of deionized waters mix sublimation dye, nonionic surfactant and deionized water, sand
Mill processing, obtains suspension, and buffer solution, organic solvent, ethylene glycol and anhydrous sodium sulphate is added, and low whipping speed is 200~300r/
1~2h is stirred under min, obtains mixed liquor, and addition mass fraction is 2% chitosan-acetic acid solution, continues 20~30min of stirring, i.e.,
Obtain environment-friendly high-intensity liquid disperse dyes.
Dyestuff described in step (1) is disperse red 60, Red 167, disperse red 356, disperse yellow 54, disperse orange 29, divides
Dissipate one of indigo plant 56, Disperse Blue-79, disperse blue 183 or a variety of combinations.
It is 50~160r/min that evaporation and concentration described in step (1), which is in rotation speed, and pressure is 400~600mmHg, temperature
Degree is that 10~15min is concentrated by evaporation at 80~100 DEG C.
The mass ratio of acetone described in step (1) and concentrate is 1: 2.
Sanded treatment condition described in step (2) is that mixing speed is 50~60r/min, ratio of grinding media to material 10: 1, using straight
Diameter is the bead of 2~3mm, and 30~40min is sanded.
Buffer solution described in step (2) be one of citric acid, acetic acid, triethanolamine, succinic acid and adipic acid or
A variety of combinations.
Organic solvent described in step (2) is that isopropanol and n,N-Dimethylformamide in mass ratio 1: 1 mix.
One of nonionic surfactant Sorbitan alcohol ester, sucrose fatty ester described in step (2).
The present invention is compared with other methods, and advantageous effects are:
(1) dyestuff is carried out purification processes by rotary evaporation concentration by the present invention, removes the inorganic salts in dyestuff, stabilizing dye body
System, prepares high strength fluid disperse dyes, nonionic surfactant pair in conjunction with buffer solution, organic solvent and each analog assistant
The raising of dye stability mainly shows solubilising, wetting, dispersion etc., when dyestuff enters nonionic surfactant
Micella, colorant dissolubility increase, and a certain amount of nonionic surfactant is added in dyestuff, it can weaken dye molecule
It is interior, due to the presence of nonionic surfactant, dye molecule to be made in water to accelerate to ionize with intermolecular binding force
Micella is formed, there is preferable dispersibility, and can make that there is polar dyestuff, in the intermolecular formation net of cosolvent for constituting micella
Shape solubilising, improves dissolubility;The catalyzing hydrolysis that proton reduces dyestuff can be absorbed in the addition of buffer solution, improves liquid dyes
Stability can prevent dye molecule autocatalysis from hydrolyzing, keep the reactivity of dyestuff;
(2) growth of dyestuff surface bacteria when chitosan effectively inhibits dyestuff to store in water is added in the present invention, prevents thin
Destruction of the bacterium to liquid disperse dyes, so that stabilizing dye dispersion, the addition of anhydrous sodium sulphate can effectively improve the intensity of dyestuff,
So that there is liquid disperse dyes high-intensitive and storage stability to improve.
Specific embodiment
Dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered by mass ratio 1: 6, obtain filtrate, and filtrate is placed in rotation
Turn on evaporimeter, is 50~160r/min in rotation speed, pressure is 400~600mmHg, and temperature is to evaporate at 80~100 DEG C
10~15min is concentrated, obtains concentrate, in mass ratio 1: 2 is added acetone, is uniformly mixed, obtains precipitated liquid, filters to obtain precipitating, will sink
Shallow lake is placed in 60~80 DEG C of baking oven and dries to constant weight, is cooled to room temperature, and grinds up to sublimation dye;According to parts by weight, divide
Also known as take 50~60 parts of sublimation dyes, 10~16 parts of buffer solutions, 20~40 parts of organic solvents, 1~10 part of non-ionic surface living
Property agent, 1~5 part of ethylene glycol, 10~12 parts of mass fractions be 2% chitosan-acetic acid solution, 10~30 parts of anhydrous sodium sulphate, 80~100
Part deionized water, sublimation dye, nonionic surfactant and deionized water are mixed, and low whipping speed is 50~60r/min,
Under ratio of grinding media to material is 10: 1, use diameter for the bead of 2~3mm, 30~40min be sanded, obtains suspension, be added buffer solution,
Organic solvent, ethylene glycol and anhydrous sodium sulphate, low whipping speed are that 1~2h is stirred under 200~300r/min, obtain mixed liquor, matter is added
Amount score is 2% chitosan-acetic acid solution, continues 20~30min of stirring to get environment-friendly high-intensity liquid disperse dyes.
Dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered by mass ratio 1: 6, obtain filtrate, and filtrate is placed in rotation
Turn on evaporimeter, is 50r/min in rotation speed, pressure 400mmHg, temperature is to be concentrated by evaporation 10min at 80 DEG C, must be concentrated
Liquid, in mass ratio 1: 2 is added acetone, is uniformly mixed, obtains precipitated liquid, filters to obtain precipitating, precipitating is placed in 60 DEG C of baking oven and is done
It is dry to be cooled to room temperature to constant weight, it grinds up to sublimation dye;According to parts by weight, weigh respectively 50 parts of sublimation dyes, 10 parts it is slow
Rushing solution, 20 parts of organic solvents, 1 portion of nonionic surfactant, 1 part of ethylene glycol, 10 parts of mass fractions is 2% chitosan-acetic acid
Sublimation dye, nonionic surfactant and deionized water are mixed, are being stirred by solution, 10 parts of anhydrous sodium sulphate, 80 parts of deionized waters
Speed is 50r/min, under ratio of grinding media to material 10: 1, uses diameter for the bead of 2mm, and 30min is sanded, and obtains suspension, is added slow
Solution, organic solvent, ethylene glycol and anhydrous sodium sulphate are rushed, low whipping speed is to stir 1h under 200r/min, obtains mixed liquor, quality is added
Score is 2% chitosan-acetic acid solution, continues to stir 20min to get environment-friendly high-intensity liquid disperse dyes.
Dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered by mass ratio 1: 6, obtain filtrate, and filtrate is placed in rotation
Turn on evaporimeter, is 105r/min in rotation speed, pressure 500mmHg, temperature is to be concentrated by evaporation 13min at 90 DEG C, is obtained dense
Contracting liquid, in mass ratio 1: 2 is added acetone, is uniformly mixed, obtains precipitated liquid, filters to obtain precipitating, precipitating is placed in 70 DEG C of baking oven
Drying is cooled to room temperature, grinds up to sublimation dye to constant weight;According to parts by weight, 55 parts of sublimation dyes, 13 parts are weighed respectively
Buffer solution, 30 parts of organic solvents, 6 portions of nonionic surfactants, 3 parts of ethylene glycol, 11 parts of mass fractions are 2% chitosan-second
Sublimation dye, nonionic surfactant and deionized water are mixed, are being stirred by acid solution, 20 parts of anhydrous sodium sulphate, 90 parts of deionized waters
Speed is mixed as 55r/min, under ratio of grinding media to material 10: 1, uses diameter for the bead of 2.5mm, 35min is sanded, obtains suspension, adds
Enter buffer solution, organic solvent, ethylene glycol and anhydrous sodium sulphate, low whipping speed is to stir 1.5h under 250r/min, obtains mixed liquor, adds
Entering mass fraction is 2% chitosan-acetic acid solution, continues to stir 25in to get environment-friendly high-intensity liquid disperse dyes.
Dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered by mass ratio 1: 6, obtain filtrate, and filtrate is placed in rotation
Turn on evaporimeter, is 160r/min in rotation speed, pressure 600mmHg, temperature is to be concentrated by evaporation 15min at 100 DEG C, is obtained dense
Contracting liquid, in mass ratio 1: 2 is added acetone, is uniformly mixed, obtains precipitated liquid, filters to obtain precipitating, precipitating is placed in 80 DEG C of baking oven
Drying is cooled to room temperature, grinds up to sublimation dye to constant weight;According to parts by weight, 60 parts of sublimation dyes, 16 parts are weighed respectively
Buffer solution, 40 parts of organic solvents, 10 portions of nonionic surfactants, 5 parts of ethylene glycol, 12 parts of mass fractions are 2% chitosan-
Acetic acid solution, 30 parts of anhydrous sodium sulphate, 100 parts of deionized waters mix sublimation dye, nonionic surfactant and deionized water,
Low whipping speed is 60r/min, under ratio of grinding media to material 10: 1, uses diameter for the bead of 3mm, and 40min is sanded, obtains suspension,
Buffer solution, organic solvent, ethylene glycol and anhydrous sodium sulphate is added, low whipping speed is to stir 2h under 300r/min, obtains mixed liquor, adds
Entering mass fraction is 2% chitosan-acetic acid solution, continues to stir 30min to get environment-friendly high-intensity liquid disperse dyes.
Environment-friendly high-intensity liquid disperse dyes prepared by the present invention and commercially available degree liquid disperse dyes are detected, are had
Body testing result such as following table table 1:
Detection method:
The liquid disperse dyes of embodiment 1-3 and comparative example are tested for the property.The specific test method is as follows: weighing 1.0 grams
The liquid disperse dyes and commercially available powder dye of embodiment 1-3 and comparative example are respectively placed in the water of 5000mL, are made point
Dissipate dye suspensions.It draws 50mL disperse dyes suspension to mix with the water of 50mL, adjusts dye bath pH to 5 with acetic acid, then rise
Temperature is respectively put into 2g polyester fiber and carries out high-temperature pressure dyeing to 60 DEG C, 130 DEG C is warming up in 35 minutes, heat preservation 45
Minute, it is cooled to 80 DEG C of samplings.
Observation cloth specimen coloured light simultaneously surveys its dye strength using method specified in GB/T6688-2008, with UV, visible light point
Light photometer UV-2550 surveys its dyeing residual liquid in the coloration abs value that wavelength is 380-750nm, with GB11914-89 chemical oxygen demand
It measures a dichromate titration and measures its dyeing residual liquid COD, data measured is shown in Table 1.
1 environment-friendly high-intensity liquid disperse dyes performance characterization of table
Environment-friendly high-intensity liquid disperse dyes prepared by the present invention as shown in Table 1, staining power is high, stability is good, is not easy to precipitate,
And dyeing residual liquid COD is low, more environmentally-friendly, environment-friendly high-intensity liquid disperse dyes prepared by the present invention are worthy to be popularized.
Claims (8)
1. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes, it is characterised in that specific steps are as follows:
(1) in mass ratio 1: 6 dyestuff and n,N-Dimethylformamide are uniformly mixed and are filtered, obtain filtrate, filtrate is placed in rotation
Turn on evaporimeter, be concentrated by evaporation, obtain concentrate, acetone is added, be uniformly mixed, obtain precipitated liquid, filters to obtain precipitating, precipitating is placed in
It dries in 60~80 DEG C of baking oven to constant weight, is cooled to room temperature, grind up to sublimation dye;
(2) according to parts by weight, weigh respectively 50~60 parts of sublimation dyes, 10~16 parts of buffer solutions, 20~40 parts it is organic molten
Agent, 1~10 portion of nonionic surfactant, 1~5 part of ethylene glycol, 10~12 parts of mass fractions be 2% chitosan-acetic acid solution,
10~30 parts of anhydrous sodium sulphate, 80~100 parts of deionized waters mix sublimation dye, nonionic surfactant and deionized water, sand
Mill processing, obtains suspension, and buffer solution, organic solvent, ethylene glycol and anhydrous sodium sulphate is added, and low whipping speed is 200~300r/
1~2h is stirred under min, obtains mixed liquor, and addition mass fraction is 2% chitosan-acetic acid solution, continues 20~30min of stirring, i.e.,
Obtain environment-friendly high-intensity liquid disperse dyes.
2. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(1) dyestuff described in is disperse red 60, Red 167, disperse red 356, disperse yellow 54, disperse orange 29, Disperse Blue-56, disperse blue
79, one of disperse blue 183 or a variety of combinations.
3. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(1) it is 50~160r/min that the evaporation and concentration described in, which is in rotation speed, and pressure is 400~600mmHg, and temperature is 80~100
10~15min is concentrated by evaporation at DEG C.
4. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(1) mass ratio of acetone and concentrate described in is 1: 2.
5. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(2) the sanded treatment condition described in is that mixing speed is 50~60r/min, and ratio of grinding media to material 10: 1 uses diameter for 2~3mm's
30~40min is sanded in bead.
6. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(2) buffer solution described in is one of citric acid, acetic acid, triethanolamine, succinic acid and adipic acid or a variety of combinations.
7. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(2) organic solvent described in is that isopropanol and n,N-Dimethylformamide in mass ratio 1: 1 mix.
8. a kind of preparation method of environment-friendly high-intensity liquid disperse dyes according to claim 1, it is characterised in that: step
(2) one of nonionic surfactant Sorbitan alcohol ester, sucrose fatty ester described in.
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Cited By (1)
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CN111234563A (en) * | 2020-03-30 | 2020-06-05 | 南通纺织丝绸产业技术研究院 | Water-based disperse dye for water and oil resistance and application thereof |
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