CN101560736A - Accelerant for textile dyeing, preparation method and applications thereof - Google Patents
Accelerant for textile dyeing, preparation method and applications thereof Download PDFInfo
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Abstract
The invention discloses an accelerant for textile dyeing, which is prepared by the following raw materials by weight portions: 2-5 portions of rare earths (calculated by rare earth element), 10-20 portions of organic phenol halide, 1-10 portions of organic acid, 1-5 portions of modifier A and 1-5 portions of leveling agent B; the preparation method of the accelerant comprises the following steps of (1) preparing the rare earths into a chloride solution, heating the chloride solution and adding the organic acid into the chloride solution, keeping the temperature and obtaining an intermediate A; (2) mixing the organic phenol halide and the modifier A to obtain an intermediate B; and (3) adding the intermediate B into the intermediate A, keeping the temperature and adding the leveling agent B and water; mixing the solution and obtaining the accelerant; the accelerant can be used for cotton fiber active dyes, can greatly reduce the use of sodium sulfate in the dyeing process of the active dye, is beneficial for environmental protection and reduces the production cost of the dyeing enterprises.
Description
Technical field
The present invention relates to the textile printing and dyeing field, be specifically related to a kind of environment-friendly type accelerant for textile dyeing.
Background technology
Cotton fiber occupies an important position in textile industry, accounts for 65% of fiber total output greatly.Most important, the most potential dyestuff that is applied in the cotton fiber dyeing aspect at present is a REACTIVE DYES.REACTIVE DYES and cotton fiber have fundamentally solved the problem of coloured fibre wet colour fastness difference by covalent bonds.Simultaneously because REACTIVE DYES to have chromatogram complete, lovely luster, advantage such as technique for applying is easy, and applicability is strong, and price is relatively cheap, it had become the dyestuff of cotton fiber with output in the dyestuff and output value maximum in recent years.Must add a large amount of sodium chloride or sodium sulphate in traditional reactive dyeing technology, after adding salt in the dye bath, the hydrauture of dyestuff reduces, and dyestuff is just increased to the tendency that fiber surface shifts by the aqueous solution like this, and the amount of dying just increases on the balance.The use of a large amount of inorganic salts had both increased labour intensity, cause chlorine ion concentration in the waste water up to more than 10 ten thousand ppm again, and the REACTIVE DYES utilization rate was lower, generally have only 60%～70%, produce a large amount of coloured sewage, its colourity exceeds standard several thousand times, and the COD value is generally at 0.8 ten thousand～30,000 ppm.Administer a large amount of coloured sewage difficulty of saliferous like this and well imagine that this is not only a kind of wasting of resources, and cause serious environmental to pollute.Calculate with the Dyeing of Cotton Fabric with Reactive Dyes knitwear, whenever dye 1 ton of a large amount of cotton knitwear, produce 150 tons of waste water.Dyeing waste water not only produces environment and pollutes, and also makes printing and dyeing enterprise increase production cost and processing cost.So along with people's environmental consciousness constantly strengthens, the country relevant laws and regulations perfect day by day, reactive dyeing salt pollution problem is extremely to be solved, and from the generation of source control dyeing waste water, the printing and dyeing chemicals that adopts environmental protection is an inevitable direction of printing and dyeing assistant exploitation.
Salt pollution problem in the elimination activity dyeing, at present mainly by two kinds of methods, the one, be the cotton fiber cationization from increasing that REACTIVE DYES and cotton fiber affinity sets about, method by chemistry and physics is carried out modification to cotton fiber, make fiber surface positively charged, by the affinity of increase fiber of the electrostatic interaction between the positive and negative charge and dyestuff, reach short effect of dying.Research about the cotton fiber cationization is progressively goed deep into, wherein cationic reagents that adopt response type more, comprise: epoxies nitrogen-containing compound, equal three crash type seasons an of chlorine are pressed salt compound, azetidine cationic compound etc., the cotton fiber of cationization, can under few salt even salt-free condition, be used for reactive dyeing, degree of exhaustion and degree of fixation are better, greatly reduce the salt pollution problem.But also all there is weak point in existing various cationic reagent, as can not recycle, performance to fiber itself is influential, the micromolecule reagent dosage is big, and the toxic side effect that has, problem such as polymer reactant is unfavorable for dyestuff penetration, and coloured fibre coloured light is not bright-coloured, but maximum problem is that level-dyeing property is bad, and therefore the salt-free dyeing technology does not also have a large amount of suitability for industrialized production and application at present.
It two is to substitute the salt technology, promptly uses pollution-free, environment amenable compound and substitutes glauber salt (chemical name: anhydrous sodium sulfate, another name: glauber salt, thenardite), and these compound great majority remain salt, substitute salt so be called.People know by research, unary carboxylation's salt effect is stronger than NaCl, polybasic carboxylic acid is stronger than the unary carboxylation, with their instead of table salt and glauber salt, the salt consumption can significantly reduce, but these so-calledly substitute the same salt of salt price at present, glauber salt is compared is too expensive really, therefore also can't promotion and application.
Disclose such as, Chinese patent application CN98120798.7 and a kind ofly to contain the method for Polyester Fibers, select for use to be selected from the aliphatic glycol ether derivant and to do accelerant with disperse dyeing; CN97105300.6 discloses a kind of alkali dyeing assistant, and it is made up of sodium carbonate 2～26wt%, borax 20～23wt%, calgon 54～55wt%; CN03117696.8 discloses a kind of multifunctional inorganic dyeing assistant, and it extracts slag preparation behind potassium, magnesium, the aluminium by the mesoporous mineral material of the natural nano that contains silicate or this mineral material, and these auxiliary agents all are different with the present patent application.
Summary of the invention
The present invention adopts the new technology that is different from the cation-modified of above-mentioned fiber and substitutes two kinds of thinkings of salt technology, develop a kind of accelerant of novel alternative glauber salt, it can reduce significantly salt consumption in the cotton fiber REACTIVE DYES (use the accelerant of minute quantity just can make glauber salt drop to original consumption 50%), be a kind ofly both to help environmental protection, can reduce the environment-friendly type auxiliary agent of printing and dyeing enterprise production cost simultaneously again.
The objective of the invention is to be implemented by the following technical programs:
The inventor at first provides a kind of accelerant for textile dyeing, and it is mainly obtained by the feedstock production of following weight portion: 2～5 parts of rare earths (in rare earth element), 10～20 parts in organic phenol halide, 1～10 part of organic acid, 1～5 part of modifier A, 1～5 part of levelling agent B.
Further, according to accelerant of the present invention, wherein, described rare earth is selected from rare earth chloride, nitric acid rare earth, carbonated rare earth or the rare earth oxide at least a, and is for example at least a in neodymia, yittrium oxide, yttrium chloride, selenium chloride, lanthanum nitrate, cerous nitrate, yttrium nitrate, europium nitrate, lanthanum carbonate, cerous carbonate, europium oxide, dysprosia, the praseodymium oxide etc.; Organic phenol halide is selected from 2,4,6-trichlorophenol, 2,4,6,-T, 2,4,5-trichlorophenol, 2,4,6,-T or 2,3,6-trichlorophenol, 2,4,6,-T etc.; Organic acid is selected from fumaric acid, citric acid, acrylic acid or DTPA (diethylene triamine pentacetic acid (DTPA)) etc.; Modifier A is non-ion fluorin carbon surface active agent (also being called the Organic fluoride surfactant); Levelling agent B adopts high temperature levelling agent, as adopts the high temperature levelling agent of commercially available styrene phenol polyoxyethylene ether ammonium sulfate salt.
Further, according to accelerant of the present invention, wherein, described rare earth chloride comprises lanthanum concentrate rare earth chloride, rich cerium rare earth chloride etc.; Nitric acid rare earth comprises lanthanum nitrate, cerous nitrate, yttrium nitrate, europium nitrate etc.; Carbonated rare earth comprises lanthanum carbonate, cerous carbonate etc.; Rare earth oxide comprises europium oxide, dysprosia, praseodymium oxide etc.
The present invention also provides the preparation method of above-mentioned accelerant, specifically comprises following several steps:
(1) rare earth is dissolved in obtains rare-earth chloride solution in the hydrochloric acid solution, then, add organic acid again, and in 75～85 ℃ of insulations 2～5 hours, obtaining intermediate A was rare earth organic acid complex compound after this solution heating;
(2) organic phenol halide is mixed with modifier A obtain intermediate B;
(3) intermediate B is added in the intermediate A, generate semi-finished product C after 1～3 hour, add levelling agent B and water again, both got accelerant after the stirring in reaction under 40～80 ℃.
Further, according to preparation method of the present invention, wherein, described rare earth is selected from rare earth chloride, nitric acid rare earth, carbonated rare earth or the rare earth oxide at least a, as at least a in neodymia, yittrium oxide, yttrium chloride, selenium chloride, lanthanum nitrate, cerous nitrate, yttrium nitrate, europium nitrate, lanthanum carbonate, cerous carbonate, europium oxide, dysprosia, the praseodymium oxide etc.; Organic phenol halide is selected from 2,4,6-trichlorophenol, 2,4,6,-T, 2,4,5-trichlorophenol, 2,4,6,-T or 2,3,6-trichlorophenol, 2,4,6,-T etc.; Organic acid is selected from fumaric acid, citric acid, acrylic acid or DTPA (diethylene triamine pentacetic acid (DTPA)) etc.; Modifier A adopts the non-ion fluorin carbon surface active agent; Levelling agent B adopts high temperature levelling agent, as high temperature levelling agent of commercially available styrene phenol polyoxyethylene ether ammonium sulfate salt etc.
Further, according to preparation method of the present invention, wherein, concentration of hydrochloric acid solution is 0.5～2mol/L in the described step (1), and its consumption is 10～40 weight portions; Rare-earth chloride solution is heated to 60～90 ℃.
Further, according to preparation method of the present invention, wherein, organic phenol halide and modifier A weight ratio are 10: 1～0.5 in the described step (2).
Further, according to preparation method of the present invention, wherein, mixing time is 30～60min in the described step (3).
The present invention also provides the application of above-mentioned accelerant in the cotton fiber reactive dyeing.
Further, according to application of the present invention, wherein, the concentration of accelerant is 0.1～0.3g/L in the described cotton fiber reactive dyeing.
In the above-mentioned raw materials, organic phenol halide is the various organic matters that fiber had expanded effect; Organic acid, as fumaric acid, citric acid, acrylic acid, DTPA etc. as catalyst or complexing agent.
Compared with prior art, the present patent application has the following advantages:
The change of (1) reactive dyeing mode
Must add a large amount of glauber salt in traditional reactive dyeing technology, product of the present invention has been saved a large amount of inorganic salts (about 50% glauber salt), need not change original technology custom simultaneously again, helps the popularization of product.
(2) be beneficial to environmental protection
In traditional reactive dyeing technology, must add a large amount of salts substances such as glauber salt and do accelerant, and salts such as dissolving glauber salt need the water of flood tide, usually the salt consumption is 80～150g/L, then average computation is the consumption of 1.3 tons of left and right sides salt/ton cloth, more need consume 100 tons～150 tons in water and dye one ton of cloth, the use of a large amount of inorganic salts had both increased labour intensity, the concentration that causes chlorion in the waste water again is up to more than 10 ten thousand ppm, produce a large amount of coloured sewage, its colourity exceeds standard several thousand times, the CODcr value is generally at 0.8 ten thousand～30,000 ppm, this is not only a kind of wasting of resources, and more causing serious environmental to pollute, product of the present invention can effectively reduce salt pollution in the dyeing waste water, and saves a large amount of dyeing waters.
(3) reduce dye-works's production cost and enhancing productivity
Can the saving material time after a large amount of glauber salt are substituted, the while has been reduced workman's workload again, has improved production efficiency, has also reduced production cost.
(4) good economic and social benefit is arranged
China is a textile exports big country, and textile industry realized 1,471 hundred million dollars of outlets in 2006, increased by 25.1% on a year-on-year basis.Zhejiang Province is the big province of textile printing and dyeing in the whole nation, and dyeing industry accounts for nearly 1/2 of the whole nation.Cotton system textile dyeing and finishing industry is quite flourishing, and with regard to the Ningbo City, there are family more than 50, about more than 30000 tons of month dyeing fabric in medium-sized or above printing and dyeing mill.Greater than 10000 tons/month,, can reduce 6000 tons/month of glauber salt consumptions once tame medium-sized its glauber salt consumption of printing and dyeing enterprise if substitute glauber salt with the novel accelerant XK-08 of the present invention.And according to statistics, the consumption of other regional glauber salt such as Guangdong, Fujian, Jiangsu is just bigger.Middle-size and small-size printing and dyeing mill with 50～60 tons of day dyeing is an example, can economize on water more than 500,000 tons in year, is beneficial to environmental protection and cleaner production.Therefore product economy of the present invention and social benefit are very optimistic.
Description of drawings
Fig. 1 is an accelerant preparation method's of the present invention process flow diagram;
Fig. 2-the 1st, traditional dyeing process curve figure;
Fig. 2-the 2nd adds the dyeing curve map after the accelerant of the present invention.
The specific embodiment
Below in conjunction with embodiment, be described more specifically content of the present invention.Should be appreciated that enforcement of the present invention is not limited to the following examples, the content of foregoing invention content part record is adjusted composition of raw materials in the proportion that discloses according to the present invention, can realize purpose of the present invention.
In the present invention, if not refer in particular to, all part, percentages are unit of weight, and all equipment and raw material etc. all can be buied from market or the industry is commonly used.
The embodiment part
Embodiment 1
(1) with on the 10g purity 99.9% with neodymia, yittrium oxide do the rare earth source, they are dissolved in the 100ml 2mol/L hydrochloric acid obtain rare-earth chloride solution, rare-earth chloride solution is heated to 80 ℃, 5% the aqueous solution that adds 50g complexing agent diethylene triamine pentacetic acid (DTPA) (DTPA) simultaneously, 80 ℃ of insulation reaction 3 hours, generate a kind of rare earth organic acid complex compound;
(2) with 15g 2,4,6-trichlorophenol, 2,4,6,-T and 1g modifier A (non-ion fluorin carbon surface active agent, The Dow Chemical Co.'s product) the abundant mixing adds step (1) and reacted in the rare earth organic acid complex compound well, again after reacting 1 hour under 60 ℃, add a small amount of 2g levelling agent B (styrene phenol polyoxyethylene ether ammonium sulfate salt) again, and add distilled water to 500ml, and fully stir discharging behind the 30min, promptly get final products liquid environment-friendly accelerant-accelerant XK08A.Its fastness index and quality index see Table 1.
Embodiment 2
Change rare earth source neodymia, yittrium oxide among the embodiment 1 into mixed rare-earth oxide (purity＞85%), complexing agent changes citric acid (CA) into, and other are operated with embodiment 1, promptly get liquid environment-friendly accelerant-accelerant XK08B.Its fastness index and quality index see Table 1.
Embodiment 3
Change rare earth source neodymia, yittrium oxide among the embodiment 1 into yttrium chloride, selenium chloride, complexing agent changes fumaric acid into, and other are operated with embodiment 1, both required accelerant.
Embodiment 4
Change rare earth source neodymia, yittrium oxide among the embodiment 1 into lanthanum carbonate, complexing agent changes acrylic acid into, and other are operated with embodiment 1, both required accelerant.
Embodiment 5
Change rare earth source neodymia, yittrium oxide among the embodiment 1 into yttrium nitrate, complexing agent changes acrylic acid into, and other are operated with embodiment 1, both required accelerant.
Table 8 embodiment 1-5 composition of raw materials (g of unit)
Fastness index and the quality index of table 1 accelerant XK08A, XK08B
Quality index
The fastness index
The experimental example part
The variation of experimental example 1 dyeing
Accompanying drawing 2-1 and 2-2 are contrasted as can be seen, the more traditional traditional dyeing technology of dyeing curve after the interpolation accelerant, can add 50% glauber salt use amount less, and other conditions are without any variation, this greatly big workload and working time that has reduced when dyeing, reduce production cost again, and do not changed original technology custom at the same time, helped the popularization of product.
Experimental example 2 glauber salt technologies and the contrast of accelerant technology of the present invention dyeing cost
Contrast with using accelerant XK-08 dyeing cost with glauber salt technology
Annotate: water, electric consumption refer to dyeing process consumption in the above cost, do not comprise pre-treatment consumption, and 337 yuan of/ton cloth reduce cost.
COD (COD) test of experimental example 3 dyeing waste-waters
About the feature of environmental protection problem of technology dyeing waste-water, the inventor has done the COD test.Tradition soda ash technology and its dyeing waste-water of dyeing COD contrast of adding accelerant of the present invention, test result sees Table 2.
The COD of table 2 dyeing waste-water (COD) test result
Annotate: above data are to get the mean value that three cylinder raffinates are measured.
Table 2 result shows that add accelerant technology dyeing residual liquid chemical oxygen demand COD value of the present invention and obviously reduce than traditional glauber salt technology, the application of this auxiliary agent has alleviated the burden of wastewater treatment greatly.
Experimental example 4XK～08 consumption test
Determine the consumption of glauber salt and accelerant to see Table 3 according to dye strength.
Table 3 glauber salt and the accelerant process auxiliaries consumption table of comparisons
| Dye dosage % | Glauber salt g/l | Soda ash | Glauber salt/XK-08g/L |
| 0.5 below | 8-15 | 5-8 | 4-8/0.04-0.08 |
| 0.5-1.5 | 20-30 | 10-15 | 10-15/0.1-0.15 |
| 1.5-3.0 | 30-50 | 15-25 | 15-25/0.1-0.17 |
| 3.0-5.0 | 60-80 | 25-30 | 30-40/0.15-0.2 |
| 5.0 more than | 80-100 | 30 | 40-50/0.2-0.25 |
Experimental example 5 accelerant XK～08 level-dyeing property, diffusivity little sample testing
At the 50mL dye strength is in the blank dye liquor of 10g/L, adds the glauber salt of different amounts and the alkaline agent of specified volume, puts into 60 ℃ of model machines then and moves.Dye liquor when getting operation 10min and 20min respectively drips dye liquor on 2# filter paper, treat that it dries the back naturally and measures it and spread maximum gauge and minimum diameter, averages and observes and ooze the circle effect, the results are shown in Table 4, table 5.
Table 4 glauber salt and the contrast of accelerant XK-08 technology diffusion diameter
Table 5 glauber salt and accelerant technology are oozed circle effect contrast (getting operation 20min sample)
Oozing the circle effect from dye liquor, to add the area of accelerant as can be seen big, and diffusion evenly, and level-dyeing property, diffusivity are obviously good than conventional amount glauber salt, and particularly gorgeous blue BRV effect is more remarkable.
Experimental example 6 traditional dyeing technologies and the dyefastness contrast of adding accelerant dyeing of the present invention
The dyefastness contrast is carried out soaping fastness, crock fastness, perspiration fastness contrast respectively with four dark colours (reactive dyeing), the results are shown in Table 6.
The table 6 different cultivars fixation alkali dyefastness table of comparisons
Table 6 has compared the Color that uses two kinds of different amounts glauber salt, and every dyefastness is basic identical, but have one different be fastness to wet rubbing, accelerant XK～08 technology generally improves half grade than glauber salt technology.
Experimental example 7 uses the big sample chromatism test of accelerant of the present invention result, sees Table 7
Table 7 uses the big sample value of chromatism of accelerant XK-08 test result
Annotate: 1, Δ E, Δ L, Δ a, Δ b are standard specimen with the sample, are spline with the full-page proof, survey color matching instrument, test result under the D65 standard sources with Italian Orintex.
2, aberration computing formula: CMC is 1: 1.
Claims (10)
1. accelerant for textile dyeing, it is mainly obtained by the feedstock production of following weight portion:
2～5 parts of rare earths (in rare earth element);
10～20 parts in organic phenol halide;
1～10 part of organic acid;
1～5 part of modifier A;
1～5 part of levelling agent B.
2. accelerant as claimed in claim 1 is characterized in that described rare earth is selected from rare earth chloride, nitric acid rare earth, carbonated rare earth or the rare earth oxide at least a; Organic phenol halide is selected from 2,4,6-trichlorophenol, 2,4,6,-T, 2,4,5-trichlorophenol, 2,4,6,-T or 2,3,6-trichlorophenol, 2,4,6,-T; Organic acid is selected from fumaric acid, citric acid, acrylic acid or DTPA; Modifier A adopts the Organic fluoride surfactant; Levelling agent B adopts high temperature levelling agent.
3. accelerant as claimed in claim 2 is characterized in that, described rare earth chloride comprises lanthanum concentrate rare earth chloride, rich cerium rare earth chloride; Nitric acid rare earth comprises lanthanum nitrate, cerous nitrate, yttrium nitrate, europium nitrate; Carbonated rare earth comprises lanthanum carbonate, cerous carbonate; Rare earth oxide comprises europium oxide, dysprosia, praseodymium oxide.
4. the preparation method of the described accelerant of one of claim 1-3 is characterized in that, described preparation method comprises following several steps:
(1) rare earth is dissolved in obtains rare-earth chloride solution in the hydrochloric acid solution, then, add organic acid again, and in 75～85 ℃ of insulations 2～5 hours, obtaining intermediate A was rare earth organic acid complex compound after this solution heating;
(2) organic phenol halide is mixed with modifier A obtain intermediate B;
(3) intermediate B is added in the intermediate A, add levelling agent B and water again after 1～3 hour, both got accelerant after the stirring in reaction under 40～80 ℃.
5. preparation method as claimed in claim 4 is characterized in that described rare earth is selected from rare earth chloride, nitric acid rare earth, carbonated rare earth or the rare earth oxide at least a; Organic phenol halide is selected from 2,4,6-trichlorophenol, 2,4,6,-T, 2,4,5-trichlorophenol, 2,4,6,-T or 2,3,6-trichlorophenol, 2,4,6,-T; Organic acid is selected from fumaric acid, citric acid, acrylic acid or DTPA; Modifier A adopts the Organic fluoride surfactant; Levelling agent B adopts high temperature levelling agent.
6. preparation method as claimed in claim 4 is characterized in that, concentration of hydrochloric acid solution is 0.5～2mol/L in the described step (1), and its consumption is 10～40 weight portions; Rare-earth chloride solution is heated to 60～90 ℃.
7. preparation method as claimed in claim 4 is characterized in that, organic phenol halide and modifier A weight ratio are 10: 1～5 in the described step (2).
8. preparation method as claimed in claim 4 is characterized in that, mixing time is 30～60min in the described step (3).
9. the application of the described accelerant of one of claim 1-3 in the cotton fiber reactive dyeing.
10. application as claimed in claim 9 is characterized in that, the concentration of accelerant is 0.1～0.3g/L in the described cotton fiber reactive dyeing.
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| CN1081731A (en) * | 1992-10-20 | 1994-02-09 | 宝鸡市电化厂 | High-efficient level-dyeing fixing and hyperchromicity agent for leather |
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