CN101736613B - Aid for dyeing cotton textiles, preparation method and dyeing method thereof - Google Patents
Aid for dyeing cotton textiles, preparation method and dyeing method thereof Download PDFInfo
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- CN101736613B CN101736613B CN2009102544540A CN200910254454A CN101736613B CN 101736613 B CN101736613 B CN 101736613B CN 2009102544540 A CN2009102544540 A CN 2009102544540A CN 200910254454 A CN200910254454 A CN 200910254454A CN 101736613 B CN101736613 B CN 101736613B
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Abstract
The invention discloses an aid for dyeing cotton textiles shown in a structural formula (I), and also discloses a method for preparing the aid. The method comprises the following steps: weighing 7.0 to 8.0 percent of 3-chloro-2-hydroxypropyl trimethylammonium chloride, 1.0 to 2.0 percent of sodium hydroxide, 1.0 to 4.0 percent of polyamine, 3.0 to 4.0 percent of cyanuric chloride, 0 to 2.0 percent of aniline, 0.5 to 1.0 percent of sodium carbonate, 11 to 12 percent of normal temperature deionized water a, 4.0 to 5.0 percent of normal temperature deionized water b, and 65.5 to 67.5 percent of deionized water c at 1 to 2 DEG C; dissolving the sodium carbonate in the deionized water b to prepare aqueous solution of sodium carbonate; adding the deionized water a, the 3-chloro-2-hydroxypropyl trimethylammonium chloride and the sodium hydroxide to a reaction kettle, and stirring the mixture; adding the polyamine to the reaction kettle, and heating the kettle to 85 to 90 DEG C to perform reaction for 3 to 5 hours; adding the deionized water c and the cyanuric chloride to perform reaction for 2 to 4 hours, dripping the aqueous solution of sodium carbonate to enable the pH value to be between 4 and 6 so as to prepare the aid. The aid can be used for performing pad dyeing and dip dyeing on the cotton textiles. The aid, the preparation method and the dyeing method improve the dyeing percentage and fixation percentage of active pigment for cotton, and reduce the discharge value of waste pigment.
Description
Technical field
The invention belongs to the textile material technical field, be specifically related to a kind of auxiliary agent that is used for cotton textiles dyeing, the invention still further relates to the preparation method of this auxiliary agent and utilize this auxiliary agent to carry out the method for cotton textiles dyeing.
Background technology
Cotton reactive dye is the topmost dyestuff of cotton fiber textile dyeing.Cotton reactive dye has chromatogram broadness, lovely luster, excellent performance and characteristic of strong applicability, has obtained using widely in the dyeing industry.The annual production of whole world cotton reactive dye is about 250,000 tons, accounts for about 20% of dyestuff total output.The annual production of the present cotton reactive dye of China is about 190,000 tons, accounts for 25% of world's dyestuff total output.
Cotton reactive dye can be dyed fiber by the dye species that covalent cross-linking combines with quilt, and the wet fastness of dying product is fine.But REACTIVE DYES not only can be reacted with fiber generation covalent cross-linking, and (especially under the required alkaline environment of fixation) is easy to and water generation hydrolysis in dyeing course.In addition, in order to improve the level dyeing performance of cotton reactive dye, the molecular weight of this type of dyestuff is less relatively, and its dye uptake to cotton fiber is relatively low.Hydrolised dye, not on dyestuff and the dyestuff that do not react with fiber just formed discarded dyestuff after dyeing finishes.Therefore, the utilization rate of REACTIVE DYES is not high, generally about 50-80%.The formation of discarded dyestuff can produce a large amount of colorful wastewaters, and environment structure is threatened.In traditional dyeing course,, when dyeing, must use a large amount of inorganic salts to urge to dye in order to improve the dye uptake of cotton reactive dye.Cotton reactive dye dyeing processing may cause the discharging of the main cause of environmental hazard for discarded dyestuff, inorganic salts and dyeing assistant.In order to reduce the dyeing processing cost and to reduce the harm of dyeing processing, just must improve the dye uptake and the fixation percentage of cotton reactive dye to environment.Relatively more outstanding research at above-mentioned two problems is exactly to adopt the quaternary ammonium compound of response type by dip-dye and pad dyeing mode COTTON FABRIC to be carried out preliminary treatment in recent years, promptly cotton fiber is carried out cation-modified " salt-free dyeing of cationic crosslinked dose of modification cotton of multi-active base " and (Sun Yan, thank to Kong Liang, Zhejiang printing and dyeing information and technology, 2006,11-12:22～25) " cotton cation-modified and dyeing research " (Jia Weini, Li Jingchuan, Zhou Junfeng, Wang Xueyan, printing and dyeing assistant, 2003,20 (3): 23～26).Cotton fiber through modification presents positive electric charge, can adsorb the dyestuff ion of electric charge that is negative by electrostatic attraction, thereby dyestuff is improved the dye uptake and the fixation percentage of fiber.
The cation modifier that adopts in the cation-modified research of cotton fiber is mainly quaternary amine or the aminated compounds with reactive group, and common reactive group is an epoxychloropropane and a chloro-s-triazine etc.This compounds good penetrability is beneficial to level dyeing, and molecular weight is little, substantivity is poor, consumption reaches shortcomings such as application cost height greatly but exist.In recent years, the researcher has also developed azetidine cationic compound, N hydroxymethyl acrylamide and cationic acrylamide base co-polymer, hydroxyalkyl ammonium salt compounds and living beings cationic reagent.Facts have proved that above-claimed cpd all can play effect more significantly to dye uptake and the fixation percentage that improves cotton reactive dye.But adopting a basic prerequisite of the cation-modified technology of cotton fiber is to finish fibre modification by special preliminary treatment link, promptly must increase the dyeing and finishing processing link of enterprise.As everyone knows, because the influence of various factors, textile dyeing and finishing processing enterprise is a traditional processing industry that profit is relatively low, increases the raising that the dyeing and finishing processing link will inevitably cause processing cost.According to preresearch estimates, in many cases, be difficult to remedy the economic benefit of losing owing to the increase of processing link by adopting the cation-modified technology of cotton fiber to improve REACTIVE DYES economic benefit that utilization rate obtains.In addition, find under study for action that the cation-modified look of fabric in the dyeing course that also often causes of cotton fiber becomes.Therefore, although the research staff has carried out deep research to the cation-modified technology of cotton, do not find that so far this technology forms the application of scale in the whole enterprise of cotton.
So, develop a kind of auxiliary agent, its consumption is few and need not to increase specially cotton textiles modification preliminary treatment link and improve the cotton reactive dye degree of fixation, has very important realistic meaning.
Summary of the invention
The purpose of this invention is to provide a kind of auxiliary agent that is used for cotton textiles dyeing, it is lower to have solved existing cotton reactive dye dye uptake, the colorful wastewater problem of environment pollution caused of generation.
Another object of the present invention provides the preparation method of above-mentioned auxiliary agent.
A further object of the invention provides the method for utilizing above-mentioned auxiliary agent to carry out cotton textiles dyeing, cotton fiber is not carried out the cationization preliminary treatment when pad dyeing is dyeed, and exists with bathing with cotton reactive dye; Before exhaust dyeing, it is cation-modified to adopt this auxiliary agent that cotton textiles are carried out in the last washing stage of cotton textiles pre-treatment, processes according to traditional exhaust dyeing method afterwards; Adopt said method dyeing can improve dye uptake and the fixation percentage of dyestuff to cotton fiber, when dying the equal depth of color of system, can reduce the consumption of dyestuff, can reduce simultaneously the discharge capacity of discarded dyestuff, solve the cation-modified technical costs height of existing employing cotton fiber and easily caused the problem that fabric generation look becomes in the dyeing course.
First technical scheme of the present invention is, a kind of auxiliary agent that is used for cotton textiles dyeing, and its molecular formula is:
Second technical scheme of the present invention is that a kind of preparation is used for the method for the auxiliary agent of cotton textiles dyeing, specifically implements according to following steps:
Step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water at normal temperature a of 11%-12%, the deionized water at normal temperature b of 4.0%-5.0%, 1 ℃-2 ℃ the deionized water c of 65.5%-67.5%, the total amount of above-mentioned each component is 100%, sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate;
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxyl third class trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes;
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h;
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6.
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains the auxiliary agent that the present invention is used for cotton textiles dyeing.
The 3rd technical scheme of the present invention is that a kind of auxiliary agent that utilizes is specifically implemented according to following steps the method that cotton textiles carry out pad dyeing dyeing:
Step 1: adopt soft water that cotton reactive dye is dissolved, obtain the dye solution that concentration is 0.001g/l-120g/l; The auxiliary agent of 1.0g/l-5.0g/l and the alkyl polyoxyethylene class non-ionic surface active agent of 0.3g/l-1.5g/l are added in the dye solution that obtains, and stirring obtains the dyestuff padding liquid; 3.0g/l-6.0g/l NaOH, 15g/l-25g/l sodium carbonate, 150g/l-250g/l sodium chloride and 2.0g/l-5.0g/l reservehao S are dissolved with soft water, obtain fixation liquid;
Step 2: pad dyeing dyeing, specifically implement: pad dye liquor, infrared preliminary drying according to following steps, the oven dry of hot blast drying case, fixation liquid is padded in the drying cylinder oven dry, decatize case decatize, the washing of flowing, 50 ℃ of washings, 50 ℃ of washings, 80 ℃ of washings, soap steam box decatize, 90 ℃ of washings, 70-80 ℃ of washing, 40 ℃ of washings, the drying cylinder oven dry, cropping is promptly finished the pad dyeing dyeing of COTTON FABRIC.
The 4th technical scheme of the present invention is that a kind of auxiliary agent that utilizes carries out the exhaust dyeing method to cotton textiles, specifically implements according to following steps:
Step 1: cotton textiles are carried out cation-modified,
Cotton textiles are carried out pre-treatment, add the auxiliary agent of 5%-30%owf and the alkyl polyoxyethylene class non-ionic surface active agent of 0.1%-3.0%owf in the washing stage, in temperature is under 30 ℃ of-50 ℃ of conditions circular flow 5-15 minute, add caustic soda when waiting to be warming up to 80 ℃-90 ℃, make and handle to bathe the pH value and reach 10.5-11.5, carry out cold wash after being incubated 15-25 minute again;
Step 2: cotton textiles are carried out exhaust dyeing, specifically implement according to following steps: the cotton textiles after cation-modified are inserted dyeing installation, add soft water, making bath raio is 6: 1-50: 1, open dyeing installation, and make water circulation; Under cycling condition, with soft water an amount of cotton reactive dye is dissolved, form dye bath; Under 30 ℃ of-50 ℃ of conditions circulation 5-10 minute; With 0.5 ℃/minute-2.0 ℃/minute heating rates dye bath is warming up to 60 ℃-90 ℃, insulation is 3-6 minute under the condition that keeps the dye bath circulation, the anhydrous sodium sulfate that adds 25%-45%owf, circulation 3-6 minute, the anhydrous sodium sulfate that adds 25%-45%owf again, insulation is 15-30 minute under cycling condition, adds the sodium carbonate of 15%-25%owf, be incubated 40-70 minute, emit dye liquor;
Step 3: the cotton textiles after the dyeing that step 2 is obtained are soaped and are washed, and promptly finish the exhaust dyeing of cotton textiles.
The invention has the beneficial effects as follows:
1. adopt auxiliary agent to carry out the pad dyeing and the dip-dye of cotton textiles, improve dye uptake and the fixation percentage of cotton reactive dye to pure cotton fabric, solve the low problem of degree of fixation that cotton reactive dye is low because of dye uptake and the percent hydrolysis height causes, and reduced the discharge capacity of discarded dyestuff.Every COLOR FASTNESS of cotton textiles after the dyeing and physicochemical property all can reach relevant national standard.
2. need not to be provided with specially the cation-modified link of cotton textiles, realized one-step method pad dyeing and need not the special cation-modified pretreated dip-dye processing that increases, make the convenient economy of production and processing.
3. adopt above-mentioned dyeing assistant and colouring method, can reduce dye dosage 15%-35%, reduce discarded dyestuff discharging 15%-30%, have remarkable economic efficiency and social benefit.
Description of drawings
Fig. 1 utilizes auxiliary agent to carry out the preceding cation-modified pretreated heating curve of exhaust dyeing in the embodiment of the invention 3, wherein A is auxiliary agent and alkyl polyoxyethylene class non-ionic surface active agent, and B is a NaOH;
Fig. 2 utilizes auxiliary agent to carry out the heating curve of exhaust dyeing in the embodiment of the invention 3, wherein A is a REACTIVE DYES, and B is the Na of total amount 1/2
2SO
4, C is the Na of total amount 1/2
2SO
4, D is Na
2CO
3
The specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The present invention is used for the auxiliary agent of cotton textiles dyeing, and its molecular formula is:
The present invention is used for the preparation method of the auxiliary agent of cotton textiles dyeing, specifically implements according to following steps:
Step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water a (room temperature) of 11%-12%, the deionized water b (room temperature) of 4.0%-5.0%, the deionized water c of 65.5%-67.5% (1 ℃-2 ℃), the total amount of above-mentioned each component is 100%, polyamine is wherein selected ethylenediamine for use, diethylenetriamine, tetraethylene pentamine, a kind of in the polyethylene polyamine etc.Sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate.
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxyl third class trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes.
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h.
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6.
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains the auxiliary agent that the present invention is used for cotton textiles dyeing.
The present invention utilizes above-mentioned auxiliary agent to the method that cotton textiles dye, and is divided into pad dyeing colouring method and exhaust dyeing method,
The pad dyeing colouring method is specifically implemented according to following steps:
Step 1: the preparation dye solution, adopt soft water that cotton reactive dye is dissolved, obtain the dye solution that concentration is 0.001g/l-120g/l; Preparation dyestuff padding liquid adds the auxiliary agent of 1.0-5.0g/l and the alkyl polyoxyethylene class non-ionic surface active agent of 0.3-1.5g/l in the 0.001-120g/l dye solution that obtains, and stirs, and obtains the dyestuff padding liquid; Preparation fixation liquid dissolves 3.0-6.0g/l NaOH, 15-25g/l sodium carbonate, 150-250g/l sodium chloride and 2.0-5.0g/l reservehao S with soft water, obtain fixation liquid;
Step 2: pad dyeing dyeing, pad dyeing dyeing processing is carried out on common pad dyeing combination machine, specifically implement: pad dye liquor (pick-up is 60%-70%), infrared preliminary drying, (99 ℃ of hot blast drying case oven dry according to the consistent step of following and traditional knot dyeing technology, 1-1.5 minute), drying cylinder oven dry (the drying cylinder internal vapor pressure is 0.2MPa, and the drying cylinder surface temperature is 110-115 ℃, and drying time is 3 minutes), pad fixation liquid (pick-up is 60%-70%), decatize case decatize (vapor (steam) temperature is 100-102 ℃, and steaming time is 1.5-2min), the washing of flowing, 50 ℃ of washings, 50 ℃ of washings, 80 ℃ of washings, soap steam box decatize (decatize case internal temperature is 90 ℃), 90 ℃ of washings, 70-80 ℃ of washing, 40 ℃ of washings, drying cylinder oven dry, cropping is promptly finished the pad dyeing dyeing of COTTON FABRIC.
Adopt dyeing assistant of the present invention that pure cotton fabric is carried out pad dyeing dyeing, can make the dyestuff in the pad dyeing bath produce aggtegation by the effect of dyeing assistant, form the dye granule of extremely tiny and stable dispersion, because the surface tension of dye granule and the surface tension of cotton fiber are approaching, it has absorption more fully than the common dye molecule to the cotton fiber surface.After preliminary drying and drying course in, along with the volatilization of moisture on the fabric, dyestuff fine suspension particle is further strengthened the absorption of fiber surface.Follow-up when rolling the alkali fixation and since have a considerable amount of dye molecules by " embedding " among dye granule, these dye molecules do not contact with alkaline agent in the fixation liquid substantially.After the decatize initial stage, still limited by contacting of alkaline agent in the dye molecule of " embedding " and the fixation liquid.Continuation rising along with the fabric system temperature, dye granule disintegrates under the molecular thermalmotion effect, the dye molecule that is discharged inorganic salts " saltouing " effect and with the intrinsic graviational interaction of fiber under can enter fibrous inside on the spot, fibrous inside take place diffusion and by with the fiber macromolecular chain in primary hydroxyl on the glucose ring form ehter bond and set.Based on above-mentioned pad dyeing dyeing mechanism, REACTIVE DYES reduces at the hydrolysis degree in fixation stage, and the dye fixing rate is improved.
The exhaust dyeing method is specifically implemented according to following steps:
Step 1: carry out cation-modified to cotton textiles (Quality Pure Cotton Yarn Production or pure cotton fabric)
Cotton textiles are carried out pre-treatment, add auxiliary agent (5%-30% in the last washing stage, owf) and alkyl polyoxyethylene class non-ionic surface active agent (0.1%-3.0%, owf), in temperature is under 30 ℃ of-50 ℃ of conditions circular flow 5-15 minute, add caustic soda when waiting to be warming up to 80-90 ℃, make to handle and bathe the pH value and reach 10.5-11.5, carry out cold wash after being incubated 15-25 minute again; Owf refers to the ratio of dyestuff weight and lining weight.
Step 2: cotton textiles are carried out exhaust dyeing
With step 1 obtain cation-modified after cotton textiles insert dyeing installation, add soft water, making bath raio is 6: 1-50: 1, open dyeing installation, make water circulation; Under cycling condition, with soft water an amount of cotton reactive dye is dissolved, add in the above-mentioned bath, form dye bath; Under 30 ℃ of-50 ℃ of conditions circulation 5-10 minute; With 0.5-2.0 ℃/minute heating rate dye bath is warming up to 60 ℃-90 ℃, insulation is 3-6 minute under the condition that keeps the dye bath circulation, add 25%-45% (owf) anhydrous sodium sulfate, circulation 3-6 minute, add 25%-45% (owf) anhydrous sodium sulfate again, insulation is 15-30 minute under cycling condition, adds 15%-25% (owf) sodium carbonate, be incubated 40-70 minute, emit dye liquor;
Step 3: the cotton textiles after the dyeing that step 2 is obtained are soaped and are washed, and promptly finish the exhaust dyeing of cotton textiles.
The cation-modified preliminary treatment of adopting dyeing assistant of the present invention that cotton textiles are carried out is actually last one high-temperature water in the cotton textiles pretreatment procedure and washes and finish in the process.Utilize this operation to adopt dyeing assistant of the present invention that cotton textiles are carried out preliminary treatment, and pretreated cotton textiles are carried out exhaust dyeing, do not increase the actual work flow and the operation of cotton textiles according to traditional dyeing technology.Contain abundant hydroxyl and amino and cation group in the dyeing assistant molecule of the present invention, cotton fiber is through after its preliminary treatment, REACTIVE DYES is to the dyeing capacity of cotton fiber when having improved dyeing, the dye uptake of dyestuff is than the high 10%-20% of traditional handicraft before adding the alkali fixation, this has reduced the hydrolysis of fixation stage dyestuff in dye bath, improve the dye fixing rate, reduced the discharging of discarded dyestuff, can produce remarkable economic efficiency and social benefit.
Embodiment 1
Step 1: with 18.8 kilograms of 3-chloro-2-hydroxypropyl trimethyl ammonium chlorides and 4 kilograms of dissolution of sodium hydroxide in 30 kilograms of deionized waters, under 30 ℃ of conditions, stirred 30 minutes, add 3.05 kilograms of ethylenediamines afterwards, under stirring condition, system temperature is risen to 90 ℃, be incubated 4 hours; In above-mentioned system, add 9.2 kilograms of Cyanuric Chlorides, adding temperature after the dissolving again is 177.75 kilograms of frozen water of 1 ℃-2 ℃, system temperature is remained on below 5 ℃, carry out with process, slowly add 7 kilograms of aqueous sodium carbonates (be dissolved in 12.75 kilograms of deionized waters make 2.25 kilograms of sodium carbonate), about regulation system pH value to 5.0; When the pH value substantially constant for the treatment of system does not change, the aniline that adds 4.7 kilograms, system temperature is remained on about 40 ℃, carry out with reaction, slowly add 8 kilograms of above-mentioned aqueous sodium carbonates, system pH is remained on about 5.0, when the pH value substantially constant of question response thing does not change, whole synthetic reaction finishes, and promptly makes dyeing assistant.
Step 2: prepare pad dyeing bath and fixation bath according to table 1 and table 2:
The composition that table 1 pad dyeing is bathed
The composition that table 2 fixation is bathed
Adopting above-mentioned two kinds of pad dyeing baths and fixation to bathe specification on common pad dyeing combination machine respectively is that the textile corduroy fabric of 14W carries out pad dyeing dyeing, concrete dyeing flow process is: pad dye liquor (pick-up is 60%-70%), infrared preliminary drying, hot blast drying case oven dry (99 ℃, 1-1.5 minute), (the drying cylinder internal vapor pressure is 0.2MPa in the drying cylinder oven dry, the drying cylinder surface temperature is 110-115 ℃, drying time is 3 minutes), pad fixation liquid (pick-up is 60%-70%), (vapor (steam) temperature is 100-102 ℃ to decatize case decatize, steaming time is 1.5-2min), flow and wash 50 ℃ of washings, 50 ℃ of washings, 80 ℃ of washings, soap steam box decatize (decatize case internal temperature is 90 ℃), 90 ℃ of washings, 70-80 ℃ of washing, 40 ℃ of washings, the drying cylinder oven dry, cropping is promptly finished the dyeing of cotton textiles.
Table 3 is the chromatism test results that adopt traditional pad dyeing dyeing and pad dyeing dyeing of the present invention to dye the textile corduroy fabric of system respectively.
Table 3 chromatism test result
As can be seen from Table 3, even reduce dye dosage 15%, adopts pad dyeing dyeing of the present invention also can dye color and luster and the consistent fabric of the traditional pad dyeing dyeing of employing.
Table 4 is to adopt traditional pad dyeing dyeing and pad dyeing dyeing of the present invention to dye the COLOR FASTNESS of textile corduroy fabric of system and the test result of physical and chemical index respectively.
Table 4 is by dyeing and weaving matter sample COLOR FASTNESS and physical and chemical index test result
As can be seen from Table 4, adopt the COLOR FASTNESS and the physical and chemical index basically identical of two kinds of pad dyeing dyeing gained fabrics.
Embodiment 2
Step 1: with 18.8 kilograms of 3-chloro-2-hydroxypropyl trimethyl ammonium chlorides and 4 kilograms of dissolution of sodium hydroxide in 30 kilograms of deionized waters, under 30 ℃ of conditions, stirred 30 minutes, add 3.05 kilograms of ethylenediamines afterwards, under stirring condition, system temperature is risen to 90 ℃, be incubated 4 hours; In above-mentioned system, add 9.2 kilograms of Cyanuric Chlorides, adding temperature after the dissolving again is 177.75 kilograms of frozen water of 1 ℃-2 ℃, system temperature is remained on below 5 ℃, carry out with process, slowly add 7 kilograms of aqueous sodium carbonates (be dissolved in 12.75 kilograms of deionized waters make 2.25 kilograms of sodium carbonate), about regulation system pH value to 5.0; When the pH value substantially constant for the treatment of system does not change, the aniline that adds 4.7 kilograms, system temperature is remained on about 40 ℃, carry out with reaction, slowly add 8 kilograms of above-mentioned aqueous sodium carbonates, system pH is remained on about 5.0, when the pH value substantially constant of question response thing does not change, whole synthetic reaction finishes, and promptly makes dyeing assistant.
Step 2: prepare pad dyeing bath and fixation bath according to table 5 and table 6:
The composition that table 5 pad dyeing is bathed
The composition that table 6 fixation is bathed
Adopting above-mentioned two kinds of pad dyeing baths and fixation to bathe specification on common pad dyeing combination machine respectively is that the textile corduroy fabric of 21W carries out pad dyeing dyeing, concrete dyeing flow process is: pad dye liquor (pick-up is 60%-70%), infrared preliminary drying, hot blast drying case oven dry (99 ℃, 1-1.5 minute), (the drying cylinder internal vapor pressure is 0.2MPa in the drying cylinder oven dry, the drying cylinder surface temperature is 110-115 ℃, drying time is 3 minutes), pad fixation liquid (pick-up is 60%-70%), (vapor (steam) temperature is 100-102 ℃ to decatize case decatize, steaming time is 1.5-2min), flow and wash 50 ℃ of washings, 50 ℃ of washings, 80 ℃ of washings, soap steam box decatize (decatize case internal temperature is 90 ℃), 90 ℃ of washings, 70-80 ℃ of washing, 40 ℃ of washings, the drying cylinder oven dry, cropping is promptly finished the dyeing of cotton textiles.
Table 7 is the chromatism test results that adopt traditional pad dyeing dyeing and pad dyeing dyeing of the present invention to dye the textile corduroy fabric of system respectively.
Table 7 chromatism test result
As can be seen from Table 7, even reduce dye dosage 25%, adopts pad dyeing dyeing of the present invention also can dye color and luster and the consistent fabric of the traditional pad dyeing dyeing of employing.
Table 8 is to adopt traditional pad dyeing dyeing and pad dyeing dyeing of the present invention to dye the COLOR FASTNESS of textile corduroy fabric of system and the test result of physical and chemical index respectively.
Table 8 is by dyeing and weaving matter sample COLOR FASTNESS and physical and chemical index test result
As can be seen from Table 8, adopt the COLOR FASTNESS and the physical and chemical index basically identical of two kinds of pad dyeing dyeing gained fabrics.
Embodiment 3
Step 1: textile cheese is carried out cation-modified preliminary treatment according to as shown in Figure 2 curve: synthetic 3% (owf) auxiliary agent of step 1 in the last washing stage of 100 kilograms of textile cheese pre-treatments adds according to embodiment 1; bath raio is 7: 1; initial temperature is 40 ℃; circulate after 10 minutes; make to handle to bathe by 2 ℃/minute speed to be warming up to 85 ℃, add NaOH makes and handles the pH value of bathing and reach 11; is incubated and emits treatment fluid after 20 minutes, the end preliminary treatment;
Step 2: according to as shown in Figure 3 curve 1 textile cheese after cation-modified is set by step carried out exhaust dyeing: the bath raio of dye bath is 7: 1, initial dyeing temperature is 40 ℃, in dye bath, add 2% (owf) Shen new M series cotton reactive dye and (be the new red M-2B in Shen, new yellow M-5R in Shen and the M-2GE's of Shen Xinlan is any), be incubated the anhydrous sodium sulfate that adds 25g/l after 10 minutes, being incubated the speed that begins with 1 ℃/minute after 10 minutes makes dye bath be warming up to 60 ℃, the anhydrous sodium sulfate that adds 25g/l, be incubated the sodium carbonate that adds 20g/l after 20 minutes, be incubated 30 minutes, bleed off remaining dye liquor, washing finishes dyeing by soaping.
Table 9 is for adopting the dye fixing rate and the depth of color (with the K/S value representation) of the resulting sample of coloured differently technology
The dye fixing rate of the resulting sample of table 9 coloured differently technology and sample K/S value
As can be seen from Table 9, adopt auxiliary agent that textile cheese is carried out can making at the fixation percentage of exhaust dyeing process middle cotton with REACTIVE DYES after the cation-modified processing and increase significantly, the depth of color that dyes product also increases significantly.
Claims (7)
1. one kind is used for the auxiliary agent that cotton textiles dye, and it is characterized in that its molecular formula is:
Described auxiliary agent adopts following method to be prepared from: step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water at normal temperature a of 11%-12%, the deionized water at normal temperature b of 4.0%-5.0%, 1 ℃-2 ℃ the deionized water c of 65.5%-67.5%, the total amount of above-mentioned each component is 100%, sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate;
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes;
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h;
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6;
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains being used for the auxiliary agent of cotton textiles dyeing.
2. a method for preparing the described auxiliary agent of claim 1 is characterized in that, specifically implements according to following steps:
Step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water at normal temperature a of 11%-12%, the deionized water at normal temperature b of 4.0%-5.0%, 1 ℃-2 ℃ the deionized water c of 65.5%-67.5%, the total amount of above-mentioned each component is 100%, sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate;
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxypropyl trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes;
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h;
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6;
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains being used for the auxiliary agent of cotton textiles dyeing.
3. method according to claim 2 is characterized in that, described polyamine is selected a kind of in ethylenediamine, diethylenetriamine, the tetraethylene pentamine for use.
4. one kind is utilized the described auxiliary agent of claim 1 to the method that cotton textiles carry out pad dyeing dyeing, it is characterized in that, specifically implements according to following steps:
Step 1: adopt soft water that cotton reactive dye is dissolved, obtain the dye solution that concentration is 0.001g/l-120g/l; The auxiliary agent of 1.0g/l-5.0g/l and the alkyl polyoxyethylene class non-ionic surface active agent of 0.3g/l-1.5g/l are added in the dye solution that obtains, and stirring obtains the dyestuff padding liquid; 3.0g/l-6.0g/l NaOH, 15g/l-25g/l sodium carbonate, 150g/l-250g/l sodium chloride and 2.0g/l-5.0g/l reservehao S are dissolved with soft water, obtain fixation liquid;
Step 2: pad dyeing dyeing, specifically implement: pad dye liquor, infrared preliminary drying according to following steps, the oven dry of hot blast drying case, fixation liquid is padded in the drying cylinder oven dry, decatize case decatize, the washing of flowing, 50 ℃ of washings, 50 ℃ of washings, 80 ℃ of washings, soap steam box decatize, 90 ℃ of washings, 70-80 ℃ of washing, 40 ℃ of washings, the drying cylinder oven dry, cropping is promptly finished the pad dyeing dyeing of COTTON FABRIC.
5. the method that cotton textiles are carried out pad dyeing dyeing according to claim 4 is characterized in that described auxiliary agent prepares according to following steps:
Step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water at normal temperature a of 11%-12%, the deionized water at normal temperature b of 4.0%-5.0%, 1 ℃-2 ℃ the deionized water c of 65.5%-67.5%, the total amount of above-mentioned each component is 100%, sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate;
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxyl third class trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes;
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h;
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6;
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains being used for the auxiliary agent of cotton textiles dyeing.
6. one kind is utilized the described auxiliary agent of claim 1 that cotton textiles are carried out the exhaust dyeing method, it is characterized in that, specifically implements according to following steps:
Step 1: cotton textiles are carried out cation-modified,
Cotton textiles are carried out pre-treatment, add the auxiliary agent of 5%-30%owf and the alkyl polyoxyethylene class non-ionic surface active agent of 0.1%-3.0%owf in the washing stage, in temperature is under 30 ℃ of-50 ℃ of conditions circular flow 5-15 minute, add caustic soda when waiting to be warming up to 80 ℃-90 ℃, make and handle to bathe the pH value and reach 10.5-11.5, carry out cold wash after being incubated 15-25 minute again;
Step 2: cotton textiles are carried out exhaust dyeing, specifically implement according to following steps: the cotton textiles after cation-modified are inserted dyeing installation, add soft water, making bath raio is 6: 1-50: 1, open dyeing installation, and make water circulation; Under cycling condition, with soft water an amount of cotton reactive dye is dissolved, form dye bath; Under 30 ℃ of-50 ℃ of conditions circulation 5-10 minute; With 0.5 ℃/minute-2.0 ℃/minute heating rates dye bath is warming up to 60 ℃-90 ℃, insulation is 3-6 minute under the condition that keeps the dye bath circulation, the anhydrous sodium sulfate that adds 25%-45%owf, circulation 3-6 minute, the anhydrous sodium sulfate that adds 25%-45%owf again, insulation is 15-30 minute under cycling condition, adds the sodium carbonate of 15%-25%owf, be incubated 40-70 minute, emit dye liquor;
Step 3: the cotton textiles after the dyeing that step 2 is obtained are soaped and are washed, and promptly finish the exhaust dyeing of cotton textiles.
7. according to claim 6 cotton textiles are carried out the exhaust dyeing method, it is characterized in that described auxiliary agent prepares according to following steps:
Step 1: according to mass percent, take by weighing the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride of 7.0%-8.0%, the NaOH of 1.0%-2.0%, the polyamine of 1.0%-4.0%, the Cyanuric Chloride of 3.0%-4.0%, the aniline of 0%-2.0%, the sodium carbonate of 0.5%-1.0%, the deionized water at normal temperature a of 11%-12%, the deionized water at normal temperature b of 4.0%-5.0%, 1 ℃-2 ℃ the deionized water c of 65.5%-67.5%, the total amount of above-mentioned each component is 100%, sodium carbonate is dissolved in deionized water b, obtains aqueous sodium carbonate;
Step 2: under stirring condition, add the deionized water a that step 1 takes by weighing in reactor, 3-chloro-2-hydroxyl third class trimethyl ammonium chloride and NaOH that step 1 is taken by weighing add reactor, at room temperature stir 30 minutes to 60 minutes;
Step 3: under stirring condition, in the mixed solution that step 2 obtains, add the polyamine that step 1 takes by weighing, be warming up to 85 ℃-90 ℃ reaction 3h-5h;
Step 4: under stirring condition, the deionized water c control mixed solution temperature that adding step 1 takes by weighing in the mixed solution that step 3 obtains is below 5 ℃, add the Cyanuric Chloride reaction 2h-4h that step 1 takes by weighing, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6;
Step 5: under stirring condition, in the mixed solution that step 4 obtains, add the aniline that step 1 takes by weighing, be warming up to 35 ℃-45 ℃ reaction 2h-3h, in course of reaction, drip the aqueous sodium carbonate that step 1 obtains, make the pH value of reaction solution be 4-6, reaction finishes the back and continues to drip aqueous sodium carbonate, makes that the pH value of reaction solution is 7, promptly obtains being used for the auxiliary agent of cotton textiles dyeing.
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| CN101929084B (en) * | 2010-08-26 | 2012-05-09 | 东华大学 | Method for dyeing slubby yarn cotton fabrics into raindrop or silk rain style |
| CN102134806B (en) * | 2011-04-27 | 2012-10-03 | 广州湘中纺织助剂有限公司 | Salt-free rolling, baking, dying and low-temperature soaping method for fiber reactive dyes |
| CN102418248A (en) * | 2011-08-04 | 2012-04-18 | 江苏金辰针纺织有限公司 | Sample duplicating technology for combination containing turquoise blue dye during cotton fiber dyeing |
| CN103485203A (en) * | 2013-09-11 | 2014-01-01 | 昆山市万丰制衣有限责任公司 | Modifying and dyeing process of cotton fabric |
| CN104294590B (en) * | 2014-09-30 | 2016-09-28 | 西安工程大学 | Raw cotton fiber dyeing and finishing auxiliaries and application for colour-spun yarns processing |
| CN106245364A (en) * | 2016-08-24 | 2016-12-21 | 常熟市新华源有色毛条厂 | The colouring method of superfine wool fiber top |
| CN106427364B (en) * | 2016-08-26 | 2019-12-24 | 绍兴文理学院 | Method for making vein decorative picture combined with painting |
| CN106638036A (en) * | 2016-12-19 | 2017-05-10 | 华南理工大学 | Method for cation modification and salt-free dyeing of cellulose fabric through one bath |
| CN110369733B (en) * | 2019-08-15 | 2022-05-27 | 盐城工学院 | Preparation and dyeing method of self-dispersing silver-carbon powder |
| CN111440317A (en) * | 2020-05-22 | 2020-07-24 | 四川德赛尔化工实业有限公司 | Melamine resin and amino resin leather retanning agent and preparation method thereof |
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