CN101381963A - Salt free dyeing with reactive dye - Google Patents

Salt free dyeing with reactive dye Download PDF

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Publication number
CN101381963A
CN101381963A CNA2007101474109A CN200710147410A CN101381963A CN 101381963 A CN101381963 A CN 101381963A CN A2007101474109 A CNA2007101474109 A CN A2007101474109A CN 200710147410 A CN200710147410 A CN 200710147410A CN 101381963 A CN101381963 A CN 101381963A
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dyeing
agent
salt
dye
cotton fiber
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胡红湘
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胡红湘
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Abstract

The invention provides a reactive dye salt-free dyeing process for cotton fiber, which comprises the following steps of pre-treatment, modified treatment, dyeing, post-treatment and so on. The modified treatment is that a copolymer of poly epichlorohydrin and polyamine used for cotton fiber is pretreated and cleaned under high temperature and alkali conditions before a special reactive dye used for a leveling agent is added to dye the cotton fiber, and the dyeing process is completed under salt-free, alkali-free or low-alkali conditions, thereby improving dyeing and fixing rate of the dye. The reactive dye salt-free dyeing process simplifies the prior dyeing process, is simple and easy to understand for operators, reduces influences of human operation factors on dyeing process and dyeing quality, and lowers production cost and sewage treatment cost overall.

Description

Salt free dyeing with reactive dye
Technical field
The invention belongs to weaving and bleaching and dyeing industry, the dyeing that relates to the cotton fiber REACTIVE DYES, particularly a kind of dyeing of salt-free short REACTIVE DYES of dying, even can under neutrallty condition, dye, a kind of colouring method of fixation, this technology particularly suitable cotton fiber or the reactive dyeing technology of the textiles of any mode of appearance of blending with it.
Background technology
REACTIVE DYES is come out from first kind in 1956 and was developed into 1992 in year surplus tens, worldwide consumption reaches 6.3 ten thousand tons, 531 of kinds, especially new REACTIVE DYES exhausts and dyes method dyeing and more than 10 years recently exploitation and exhaust the REACTIVE DYES that the method for dying is used over past 20 years, and is significant to the structure of the class that improves textiles and product and multi-varieties and small-batch dyeing etc.
Reactive dyeing is generally through absorption, diffusion and set three phases, and the first two dyes the stage on being, is set stage (active group reacts with fiber under alkali condition in the dyestuff) at last.The substantivity of general REACTIVE DYES is lower, REACTIVE DYES and fiber affinity are less, dye-uptake is lower, needing to add a large amount of salt in dye bath urgees to dye, just can reach higher dye-uptake, therefore, the dyeing cost is heightened, contain the burden that a large amount of chlorions has increased wastewater treatment in Pai Fang the waste water simultaneously.For example: publication number CN1091819C authorizes in China, the patent No. 00103414.6 cotton loose-stock dyeing method, authorize publication number CN1584194 with China, the dyeing of the patent No. 200410025172.0 cotton fibers, both all disclose a kind of dyeing that cotton fiber uses REACTIVE DYES to dye, all need to use a large amount of salt agent to do short dying in the technology, and used more alkaline agent set.
The REACTIVE DYES set will be finished under alkali condition, and alkali also impels REACTIVE DYES and water reaction, and dyestuff is lost activity, and not only causes a large amount of dyestuff losses, also influences the Washing of printed fabrics.This is because hydrolised dye can be adsorbed onto on the fabric, in water-washing process, also be difficult for washing fully, especially special dark color is particularly serious, also therefore cause the REACTIVE DYES fixation rate on the low side, reach a kind of colour saturation balance for indivedual special dark colors owing to dying on dye liquor and the fiber, can't dye depth of color preferably, and problem such as textiles post processing burden is heavy, and chroma in waste water is big.The dye-uptake of general REACTIVE DYES is 70%, and fixation rate is between 45~55%.Even known newly developed exhausting at present dyed the REACTIVE DYES of usefulness under the set alkaline agent treatment conditions of a large amount of accelerant and the best, maximum dye-uptake is about 90~95%, and fixation rate is about about in the of 80%.
Existing cold-stacking dyeing method preferably resolves the cotton fiber reactive dyeing and dyes at less salt or salt-free short dying under the condition, to reach the highest fixation rate and best dyefastness, and realization energy saving purposes, but this technology has following deficiency: for example extremely strong to the selectivity of the mode of appearance of the type of dyestuff, fiber and dyeing installation, dyeing need be banked up 8-24 hour, time is long, and needs a large amount of problems such as alkaline agent set.
Summary of the invention
One of purpose of the present invention: be for solving REACTIVE DYES and the low problem of cotton fiber affinity, allow cotton fiber increase and REACTIVE DYES between the dyeing seat, under salt-free or the short condition of dying of less salt agent, improve the substantivity and the through-dyeing of dyestuff and fiber, dye-uptake and the fixation rate of REACTIVE DYES on cotton fiber brought up to the highest and best point, make REACTIVE DYES on the dark color that can reach the best on the cotton fiber, dye effect.Under the prerequisite that keeps existing dyeing quality, realize shirtsleeve operation method as far as possible, the colouring method of a kind of REACTIVE DYES of lowest energy consumption and time consumption produces alap production cost simultaneously, and the colourity of the dyeing waste-water of discharging and salt content etc. are dropped to minimum point.
The technical scheme of implementing this invention is:
The method of this invention comprises: pre-treatment, modification processing, dyeing, post processing, finishing process.Wherein: pre-treatment is cotton fiber to be handled with existing known pre-treating method make qualified semi-products, with existing known cotton fiber modification agent cotton fiber being carried out modification handles, make affinity and dyeing seat between cotton fiber increase and the REACTIVE DYES, thereby the realization reactive dyeing can be finished dyeing salt-free short dying under the condition.Wherein select the amine polymers of Polyglycol 166-450 for use, or with the copolymer of Polyglycol 166-450 and polyamine class under alkali condition 50~102 ℃ carry out modification to handle 30~75min be preferred modifier and preferred modified technique, and cotton fiber pre-treatment and modification are handled preferred two one-bath two-step process that divide and are finished, and the modification that is fit to any cotton textiles is handled.
Also can selectively select for use special-purpose special series of pretreatment auxiliary agent that the pre-treatment of cotton fiber is boiled floats operation and is undertaken with bath by existing known processing method with the modification treatment process, one bathes the one-step method processing, and completion of processing extremely changes the cotton fiber wash water over to dyeing process only by existing known method.
Cotton fiber and REACTIVE DYES affinity after modification is handled are good, cotton fiber can greatly increase and REACTIVE DYES between absorption affinity and increase certain dyeing seat, can under salt-free or the short condition of dying of less salt agent, improve the substantivity and the through-dyeing of dyestuff and fiber, thereby make dye-uptake and the fixation rate of REACTIVE DYES on cotton fiber bring up to peak, make REACTIVE DYES on the special dark color that can reach the best on the cotton fiber, dye effect, as select for use suitable specific REACTIVE DYES can allow REACTIVE DYES under salt-free alkali-free condition, finish dyeing and set operation.
During dyeing, can contaminate according to the mode of appearance of cotton fiber, with the type selecting of REACTIVE DYES or dye gigging method, cold dome dye method or roll-dry by the fire-the steaming method dyes, dyeing can be to have known any dyeing now.Wherein soak, preferred dying operation technology is during dye gigging: earlier with chelated dispersants and special-purpose slow dye buffer respectively input material cylinder pump into dye vat after diluting mixing, will through modification handle qualified cotton fiber in normal temperature~90 ℃ dimension preliminary treatment 10~30min, slowly adding the REACTIVE DYES that predissolve stirs afterwards under normal temperature condition again dyes, continue at normal temperature maintenance 10~60min after adding dyestuff, be warming up to 80-110 ℃ afterwards and handle 15~45min, sample cutting is checked colors afterwards; Or selectable a spot of salt and the alkaline agent of adding after dyestuff finishes 10~20min ℃ keeps 10~60min in normal temperature~80 again, and sample cutting is checked colors afterwards, does not meet the color and luster requirement and calculates the dyestuff deal of adding by existing known method; Meet the color and luster requirement, change the dyeing postprocessing working procedures over to.Soaking, preferably selecting the dyestuff model for use when salt-free non-alkali dyeing set technique is adopted in dye gigging is Argazol NF series of products.
During post processing, according in the dye process being the alkaline set or the technology of neutral set, optionally select: discharge opeing--wash water pickling-90~98 ℃ soap-wash pickling--color fixing agent Y or aldehyde-free colour stabilizer processing, or after the selectable discharge opeing not wash water add and directly add fastness to wet rubbing elevator or aldehyde-free colour stabilizer behind a spot of water and strengthen after the fixation wash water again, change finishing process afterwards over to, arrangement available existing known any afterfinish method in back is put in order.
The method of the fiber-reactive colorants dyeing after modification is handled, in whole dyeing course, can be according to selected dye species, dyeing quality requirement, selectively to select salt-freely shortly to dye, no alkaline agent set, normal temperature dyes, the technology of high temperature set; Also can select salt-freely short to dye, only add a spot of alkaline agent in 60~80 ℃ of sets, addition is 10~50% of existing dyeing alkaline agent that method consumes, finishes the technology of whole dyeing process under normal temperature~80 ℃; Can select also that small amounts of salts is short dyes and add a spot of alkaline agent set, addition is 10~50% of existing salt that colouring method consumes and alkaline agent, finishes the dyeing of whole dyeing process under normal temperature~80 ℃.
Concrete steps are:
1, according to the mode of appearance of fiber, for example (1) fibre or cheese loose; (2) knitting or tatting blank; Determine the type of supporting process equipment thus.
2, equipment can be existing known all continuously or batch (-type) bleaching and dyeing finishing equipment, for example (1) normal temperature and pressure or High Temperature High Pressure overflow machine or dye jigger; (2) cold rolling heap machine of continous mode etc.
3, determine the screening of interpolation auxiliary agent, dye species and dyeing of technological parameter, technology pairing of pre-treatment, modification processing, dyeing, post processing, the back arrangement series of cellulose fibre and the formulation of aftertreatment technology etc. according to preceding binomial.
A: wherein pre-treatment and modification are handled:
(1) optionally bathes one-step method and carry out processed by two one-bath two-step process or, when adopting one to bathe a step process, the used interpolation auxiliary agent of pre-treatment process is special, the not surfactant monomer or the complex of electronegative composition in neutral and alkalescent, surfactant can be for having all surface activating agent that known can be used for weaved and bleachinged and dyeing industry now, surfactant described below such as nothing are refered in particular to, and are this type.
(a) two one-bath two-step process pre-treatments can known anyly moved back, boil, float pre-treatment process and handle qualified cellulose semi-finished product with existing, afterwards with fiber impregnation or pad and contain the specific buffering retarding agents of 0.25~5 grams per liter, 0.5~8 grams per liter modifier, the solution of 1~8 grams per liter caustic soda, handle 30~60min in 50~102 ℃, wash water is to changing dyeing process only over to afterwards, and wherein modification processing the best is preferably carried out in two one-bath two-step process pre-treatments again after mercerizing process.
(b) one to bathe one-step method be with the fiber of destarch, flood or pad and contain the special buffering retarding agents of 0.25~5 grams per liter, 4~20 grams per liter hydrogen peroxide, 0.5~5 grams per liter hydrogen peroxide stabilizer, the chelated dispersants of 0.1~2 grams per liter, 0.5~8 grams per liter modifier, 0.5 the solution of~8 grams per liter caustic soda, in 95~102 ℃ of processing 30-60min, wash water is to changing dyeing process only over to afterwards, the method is fit to especially that pre-treatment need not through the mercerising operation, the textiles processing that fibrous structure is loose.
B: dyeing:
(a) will handle qualified cellulose fibre by existing known method through modification, dye respectively with what follows technology 3 and technology 4, and draw the dyeing rate curve map of each monogenetic dye of selected REACTIVE DYES on modified cotton fiber respectively, for example: two chloro-s-triazine base double-active group types, two ethene sulfuryl double-active group types, perhaps a chloro-s-triazine base and ethene sulfuryl double-active group type etc., this for existing known technology so do not add to describe in detail at this.
(b) the dyeing rate curve map of drawing according to above-listed (a) step is selected to dye the immediate tricolor dye of curve and is made up colorant match, produces greatly after modulating satisfactory color and luster.The cotton fiber that modification is qualified dyes respectively by following described technology with identical colorant match prescription, and do synchronous counterstain with the cotton fiber semi-products of similar unmodified processing with what follows traditional technology 1, technology 5 and the similar cotton fiber after modification is handled and test, be illustrated the characteristic of technology of the present invention.
Technology 1: normal temperature is gone into unmodified cotton 10min--levelling agent 15min--dyestuff 20min-at twice with salt levelling 15min---2 ℃ of/minute--pickling-95 20min--wash water pickling of ℃ soaping--40 ℃ wet friction fastness improving agent or color-fixing agent fixation PH=5.5-wash water--oven dry that rises to 60 ℃ * 10min-add at twice alkali, 60 ℃ * 45min-wash water behind the levelling 10min respectively respectively.
Technology 2: do counterstain with technology 1 through the cotton fiber that modification is handled.
--pickling-95 20min--wash water the pickling of ℃ soaping--40 ℃ wet friction fastness improving agent or color-fixing agent fixation PH=5.5-wash water--oven dry that technology 3: normal temperature goes into to handle cotton 10min-add levelling agent 15min-through modification and add dyestuff 20min--2 ℃/minute and rise to 60 ℃ * 15min-add, 60 ℃ * 45min-wash water of alkali.
Oven dry that technology 4: normal temperature goes into to handle cotton 10min-add levelling agent 15min--through modification and add dyestuff 20~45min--2 ℃/minute and be raised to 100 ℃ * 15~40min--wash water--40 ℃ wet friction fastness improving agent or color-fixing agent fixation PH=5.5-wash water--.
------wash water--pickling----wash water--pickling--40 ℃ wet friction fastness improving agent or the color-fixing agent fixation PH=5.5--wash water--oven dry of soaping for 95 ℃ that normal temperature was banked up 2 hours that normal temperature is gone into cloth (similar modification and unmodified cotton fiber pad respectively) one and soaked and roll (pick-up 85%) of technology 5: levelling agent+dyestuff+alkali mixing.
------wash water--pickling----wash water--pickling--40 ℃ wet friction fastness improving agent or the color-fixing agent fixation PH=5.5--wash water--oven dry of soaping for 95 ℃ that normal temperature was banked up 2 hours that normal temperature goes into to handle cotton two through modification and soak two and roll (pick-up 75%) of technology 6: levelling agent+dyestuff mixing.
Dyeing recipe (contaminating owf):
Dark using: red 239 3% C.I. of yellow 176 4.5% C.I. of C.I. black 50 0.5%
Light color is used: red 195 0.6% C.I. of yellow 145 0.1% C.I. of C.I. blue 194 0.3%
Wherein: technology 4 is selected Argazol NF series three-primary colours REACTIVE DYES for use, and consumption is with last identical, and above exhaust process bath raio is 1:10.
To dye simultaneously DYED FABRICS dry fastness, fastness to wet rubbing, the variable color fastness of soaping of test fabric respectively after handling, thereby the best dyeing of screening.
The result is as follows:
Table 1
It is standard that above crock fastness assessment method adopts GB3920-1987, and it is standard that the fastness to washing assessment method adopts GB3921-1987, and soaping fastness is pressed the evaluation of GB250 evaluation variable color gray scale natural daylight.By last tabulation as seen, new technology 3 of the present invention, technology 4, technology 6 are except that the dark fastness to wet rubbing of spy slightly descends, and all other fastness indexs all mass effect with existing traditional handicraft gained are identical.
Shown in last table, be that example is narrated cotton fiber after modification is handled with the characteristic and the advantage of new dyeing of the present invention with dip method dyeing more below.Dyeing color and luster with existing traditional handicraft 1 is a color standard, dye respectively and regulate prescription with technology 3 and technology 4, till depth of color and coloured light reach the color standard that technology 1 dyed, wherein technology 4 is selected Argazol NF series three-primary colours REACTIVE DYES for use, and adjusted prescription and cost of material valency are as shown in table 2 below:
Table 2
More than each cost of material calculate by the market price of present ordinary quality quality product.
As seen from the above table, meeting national standard in quality is prerequisite, under the condition of equal color and luster coloured light, technology 3 of the present invention and technology 4 can reduce the dyeing cost of material and are respectively 2734.4 yuan/ton and 1584 yuan/ton than traditional existing dyeing 1 processing cotton of bleachinging and dyeing per ton, time benefit and wastewater treatment benefit offset with the modification treatment process cost that has increased temporarily, ignore.
(c) filter out best dyeing and sample dyeing recipe according to above-mentioned serial correction data after, technology deal by the big production dyestuff of recipe calculation, stir standby by existing known method dissolving dyestuff, to handle satisfactory fiber through modification and produce dyeing greatly by above-mentioned technology 3 and technology 4 (or selectable) with technology six, sample cutting is checked colors, color and luster meets and does not require that it is reinforced to mix colours according to existing technology, continues dyeing by technology 3 or technology 4; Color and luster meets the requirements, carry out serial afterfinish method such as color-fixing agent fixation and soft treatment with existing known method behind the discharging dye liquor wash water and handle, as wash water is handled at serial afterfinish methods such as carrying out soft treatment after selecting for use the also selectable not discharge opeing of technology 4 dyeing directly to carry out wet friction fastness improving agent or color-fixing agent fixation.
Adopt the key of technology of the present invention to be:
(1) modification in the pretreatment procedure is handled, and selects suitable modification process for use, selects suitable modifier and series matching auxiliary agent for use according to the mode of appearance that boils the equipment of floating and fiber of fiber.Fabric after semi-finished product and modification are handled must not contain lubricant, slurry and bleaching agent, and requires whiteness and capillary effect uniformity, good hygroscopicity, and the pH value is neutral.The left, center, right of cloth cover contain damp rate unanimity when being used for pad dyeing, and cloth cover cools off fully;
Will be when (2) dyeing according to the dyeing installation of fiber, the color and luster depth of stock-dye product, select for use suitable, best dyeing, best dye species, dye combinations to carry out colorant match, the process water water quality requirement is colourless, tasteless, pH value 7~8, hardness (DH Defo hardness) is less than 3~5 (50~90mg/kg, must use soft water the best when USA), changing material;
When (3) dyeing post processing,, take the dyeing of coloured differently temperature, select for use different set temperature to carry out to change the operation of soaping over to after the post processing with wet friction fastness improving agent or color-fixing agent reinforcement fixation according to the technology of selected dyeing and the type of REACTIVE DYES.
Adopt the advantage and the beneficial effect of technology of the present invention:
1, reduces the consumption of salt and alkaline agent, improved dyestuff dye-uptake and fixation rate height, effectively reduced the burden of wastewater treatment and the cost of wastewater treatment.
2, reduced the input amount of salt, the technology of effective simplification dying operation and the labour intensity of operation, reduction in a big way simultaneously production cost.
The specific embodiment
Provide specific embodiments of the invention below in conjunction with accompanying drawing, described embodiment does not limit the scope of application of the present invention.
Example 1: the high temperature winch-beck batch (-type) is bleachinged and dyeing cotton knitting class embryo cloth,
(1) pre-treatment and one step one of modification bathe with bathing treatment process
Technical recipe (owf):
Hydrogen peroxide 8% caustic soda (36 ° of Bc) 3% hydrogen peroxide stabilizer 2%
Modifier 4% refining agent 1.5%
100 ℃ * 45min of bath raio: 1:10
(2) dyeing
Dyeing recipe (owf):
Dyestuff total amount 4% retarding agents 2~3%
Bleeding agent 1% chelated dispersants 0.5%
Dyeing and flow process: normal temperature go into through modification handle cotton (bath raio: 1:10) 15min--2 ℃/minute of 10--levelling agent 15min--dyestuff rise to 60 ℃ * 10min-add 60 ℃ * 45min-discharge opeing of alkali-heat to wash-temperature and wash-the cold wash pickling-95 20min-overflow temperature of ℃ soaping washes-the cold wash pickling--wet friction fastness improving agent or color-fixing agent fixation-dehydration--and dries.
Example 2: the open width continous mode is boiled and is floated the cotton tatting class of device processes embryo cloth,
Modification process prescription (g/l):
Modifier 4~6
Bleeding agent 1~3
Caustic soda (36 ° of Be) 4~6
Technological process: semi-products--soak more and roll modification work of treatment liquid (pick-up 85~110%) more--decatize (102 ℃ of X 30~60min)--heat washes-and temperature washes-pickling-cold wash-oven dry
Cold dome formula for dye liquor (g/l):
Dyestuff X caustic soda (36 ° of Be) 5~10
Urea 50~100 waterglass (38~40 ° of Bc) 20~50
The slow bleeding agent 2~4 that dyes
Technological process: one soaks one rolls (pick-up 75%, 25~30 ℃ of temperature,--clot normal temperature is banked up, and--50 ℃ of temperature are washed 2~4 lattice, and---90 ℃ of 2~4 lattice-70~80 ℃ temperature of soaping of 50 ℃ of acetic acid neutralizations are washed 2~4 lattice-40~50 ℃ cold wash, 2~4 lattice-40 ℃ pickling 1~2 lattice-cold wash 1~2 lattice-40 ℃ wet friction fastness improving agent or color-fixing agent fixation (PH=5.5)--wash water 1~2 lattice--oven dry-back arrangement to 2~4 hours-cold wash, 2~4 lattice to the speed of a motor vehicle 35~45m/min).

Claims (5)

1, the method for a kind of reactive dye salt-free or low salt dyeing comprises process such as pre-treatment to cotton fiber, modification processing, dyeing, post processing, and its feature comprises the following steps:
(1) mode of appearance and institute adapted different equipment processed different according to cotton fiber screens the technology that different pre-treatments and modification are handled;
(2) cotton fiber after modification is handled can hang down alkali with salt-free alkali-free or less salt, in normal temperature--finish dyeing process under 95 ℃ the condition.
2, according to claim 1, it is characterized in that: the pre-treatment of described step (1) cotton fiber and modified technique can also can be handled with bathing with a step single bath process with two step two-bath process substep operational processes.
3, according to, it is characterized in that according to claim 2:
(1) a described step single bath process is handled with bathing, be cellulosic pre-treatment to be boiled float required auxiliary agent raw material and the required auxiliary agent mixed diluting of modification is processed jointly to the required concentration of technology, interpolation auxiliary agent required in the boiling and bleaching process is elite, not electronegative composition or do not produce the surfactant monomer or the complex of negative electrical charge composition in neutral and alkaline bath, this law is preferably suitable need not carry out the processing of the textiles of mercerizing process.
(2) described two step two-bath process substep operational processes, be after cellulose is made the cellulose semi-products by existing known pre-treating method, the working solution that cellulose is flooded the mixed preparing of modifier, alkaline agent, penetration-assisting agent dilution is handled under 40-102 ℃ jointly again, and this law is preferably carried out behind mercerizing process.
4, according to according to claim 3, it is characterized in that: the described surfactant of step (1) can be existing all surface activating agent known, that can be used for weaving and bleaching and dyeing industry.
5, according to according to claim 1, it is characterized in that: the described dyeing of step (2) is:
(1) can preferably select following technology for use in the omnidistance operation of the dyeing of light kind, not add short salt agent of dying usefulness, add less or do not add the alkaline agent set, after dyeing, be raised to 90-105 ℃ and carry out the high-temperature process rear and change the discharge opeing flow process of soaping over to.
(2) the omnidistance operation of dark dyeing with special dark kind can preferably be selected existing known any dyeing for use, under the condition of the dye-uptake, fixation rate and the every crock fastness index that reach the best, reduces the short consumption that dyes salt agent, alkaline agent and the dyestuff of usefulness.
CNA2007101474109A 2007-09-09 2007-09-09 Salt free dyeing with reactive dye Pending CN101381963A (en)

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CN102199886A (en) * 2011-05-23 2011-09-28 东华大学 Reactive dye salt-free pad dyeing method
CN102558904A (en) * 2010-12-07 2012-07-11 佛山市宇丰染料有限公司 Low-alkali reactive dye and its dyeing method
CN102965977A (en) * 2012-11-20 2013-03-13 绍兴文理学院 High-temperature low-alkaline dyeing method for double-monochlorotriazine reactive dyes
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CN102115989B (en) * 2009-12-30 2013-07-10 浙江华孚色纺有限公司 Rapidly-dyeing process for cellulose loose fiber
CN102086600A (en) * 2010-04-10 2011-06-08 何鹰 New-type salt agent
CN102558904B (en) * 2010-12-07 2013-10-23 佛山市宇丰染料有限公司 Low-alkali reactive dye and its dyeing method
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