Summary of the invention
The object of this invention is to provide a kind of simple to operate, measure the degree of fixation of reactive dye continuous dyeing accurately method of testing.Its technical scheme is:
A reactive dye continuous dyeing degree of fixation method of testing, is characterized in that adopting following steps:
1) prepare reagent, comprise that massfraction is 40% urea liquid, acetum, fixation liquid and the reference fixation liquid that volume fraction is 0.1%, wherein soda ash 30 ~ 50g/L, NaOH 0 ~ 8g/L, glauber salt 180 ~ 260g/L, reservehao S 2 ~ 4g/L in fixation liquid, all the other are water, and reference fixation liquid adopts the solution that glauber salt concentration is 180 ~ 260g/L;
2) prepare wide one, the 30cm*25cm fabric that is not less than of long *, pad dye liquor post-drying, be then divided into three, be respectively not fixation sample, fixation sample, reference;
3) fixation cloth specimen is not inserted and filled in the conical flask that 80ml volume fraction is 0.1% acetum, sample is all immersed in wherein;
4) acetum of conical flask is transferred in 500mL volumetric flask, then to the urea liquid that adds 70ml ± 5ml in conical flask, conical flask is put in to the 3 ~ 6min that strips in boiling water;
5) liquid of stripping in conical flask in step 4) is moved in the volumetric flask in step 4), then in conical flask, add 70ml ± 5ml urea, 3 ~ 6min strips in continuation boiling water;
6) repeating step 5), until the liquid of stripping is colourless;
7) with the distilled water of 40ml, the sample in conical flask is washed 3 times respectively, after washing, all cleaning fluid is moved in the volumetric flask of step 5) at every turn, and solution in volumetric flask is settled to scale with distilled water, shake up, to be measured;
8) sample drying in taking-up conical flask, to constant weight, weighs its quality, is designated as m
1;
9) with softening water, make reference solution, get in step 7) volumetric flask the solution of constant volume and on spectrophotometer, measure maximum absorption wavelength, and under this maximum wavelength, measure the absorbance of this solution, be designated as A
1;
10) fixation sample is padded with fixation liquid 100ml on horizontal sample padding machine, then the cloth specimen padding after fixation liquid is suspended on to vapour steaming colour fixing 30 ~ 60s in 98 ~ 102 ℃ of sample steaming boxes;
11) the fixation sample through step 10) is operated by step 3) ~ step 9), record the m of sample
2and A
2numerical value;
12) reference is padded with reference fixation liquid 100ml on horizontal sample padding machine, pad the volumetric flask that raffinate in rear collection padding machine moves to 500ml, and shake up after being settled to volumetric flask scale with distilled water diluting, the absorbance of measuring reference solution under the measured maximum absorption wavelength of step 9), is designated as A
3;
13) the reference washing of padding reference fixation liquid is dried to constant weight, weigh its quality, be designated as m
3;
14) by data measured substitution formula
can calculate the dye fixing rate that obtains.
The present invention compared with prior art, its advantage is: the mensuration of degree of fixation of the present invention adopts the urea method of stripping, take pad dye liquor and dry after not before fixation the amount of dye on fabric be benchmark, calculate after vapour steaming colour fixing the ratio of the amount of dye on unit mass fabric before the amount of dye on unit mass fabric and fixation.For preventing that in fixation liquid, alkaline agent exerts an influence to dyestuff maximum absorption wavelength and absorbance, the dyestuff that this method comes off the cloth specimen padding after dye liquor is dried when padding fixation liquid is equal to calculating with the reference fixation liquid liquid that pads alkali-free agent, guaranteed the accuracy of test degree of fixation, the method that the method is measured pad dyeing degree of fixation with sulfuric acid dissolution method is simultaneously compared, avoided the damaging influence of the concentrated sulphuric acid to dyestuff maximum absorption wavelength and absorbance, test result is more accurate.
Embodiment
Embodiment 1: test the degree of fixation of certain dyestuff company single active base dye Blue CL-BR concentration while being 20g/L, fabric specification used is CPT40*CM80/2*130*86*56, half-bleached shirting after mercerising, plain weave.Concrete steps are:
1) prepare reagent, comprise that massfraction is 40% urea liquid, acetum, fixation liquid and the reference fixation liquid that volume fraction is 0.1%, wherein soda ash 30g/L, glauber salt 210g/L, reservehao S 2g/L in fixation liquid, all the other are water, and reference fixation liquid adopts the solution that glauber salt concentration is 210g/L;
2) extract dye liquor 250ml, preparing long * wide is one, 30cm*20cm fabric, on masis small model machine, pad dye liquor, then on masis automatic sizing dryer, dry, during oven dry, guaranteeing that cloth cover is smooth enters cloth, then the fabric after drying is divided into three, is respectively not fixation sample, fixation sample, reference;
3) fixation cloth specimen is not inserted in the conical flask that fills 80ml acetic acid, sample is all immersed in wherein;
4) acetum of conical flask is transferred in 500mL volumetric flask, then to the urea liquid that adds 65ml in conical flask, conical flask is put in to the 3min that strips in boiling water;
5) liquid of stripping in conical flask in step 4) is moved in the volumetric flask in step 4), then in conical flask, add 65ml urea, 3min strips in continuation boiling water;
6) repeating step 5), until the liquid of stripping is colourless;
7) with the distilled water of 40ml, the sample in conical flask is washed 3 times respectively, after washing, all cleaning fluid is moved in the volumetric flask of step 5) at every turn, and solution in volumetric flask is settled to scale with distilled water, shake up, to be measured;
8) sample drying in taking-up conical flask is to constant weight, and weighing its quality is 2.202g, is designated as m
1;
9) with softening water, make reference solution, getting in step 7) volumetric flask the solution of constant volume, on spectrophotometer, to measure maximum absorption wavelength be 595nm, and the absorbance of measuring this solution under this maximum wavelength is 0.389, is designated as A
1;
10) fixation sample is padded with fixation liquid 100ml on horizontal sample padding machine, then the cloth specimen padding after fixation liquid is suspended on to vapour steaming colour fixing 30s in 98 ℃ of sample steaming boxes;
11) the fixation sample through step 10) is operated by step 3) ~ step 9), record the m of sample
2and A
2numerical value is respectively 2.180g and 0.065;
12) reference is padded with reference fixation liquid 100ml on horizontal sample padding machine, pad the volumetric flask that raffinate in rear collection padding machine moves to 500ml, and shake up after being settled to volumetric flask scale with distilled water diluting, under the measured maximum absorption wavelength of step 9), measure the absorbance A of reference solution
3be 0.032.
13) reference washing is dried to constant weight, weighing its quality is 2.112g, is designated as m
3;
14) by data measured substitution formula
can calculate and obtain dye fixing rate F is 74.5%.
Embodiment 2: test the degree of fixation of certain dyestuff company single active base dye Blue CL-BR concentration while being 20g/L, fabric specification used is CPT40*CM80/2*130*86*56, half-bleached shirting after mercerising, plain weave.Concrete steps are
1) prepare reagent, comprise that massfraction is 40% urea liquid, acetum, fixation liquid and the reference fixation liquid that volume fraction is 0.1%, wherein soda ash 30g/L, caustic soda 4g/L, glauber salt 180g/L, reservehao S 2g/L in fixation liquid, all the other are water, and reference fixation liquid adopts the solution that glauber salt concentration is 180g/L;
2) extract dye liquor 250ml, preparing long * wide is one, 30cm*20cm fabric, on masis small model machine, pad dye liquor, then on masis automatic sizing dryer, dry, during oven dry, guaranteeing that cloth cover is smooth enters cloth, then the fabric after drying is divided into three, is respectively not fixation sample, fixation sample, reference;
3) fixation cloth specimen is not inserted in the conical flask that fills 80ml acetic acid, sample is all immersed in wherein;
4) acetum of conical flask is transferred in 500mL volumetric flask, then to the urea liquid that adds 70ml in conical flask, conical flask is put in to the 3min that strips in boiling water;
5) liquid of stripping in conical flask in step 4) is moved in the volumetric flask in step 4), then in conical flask, add 70ml urea, 3min strips in continuation boiling water;
6) repeating step 5), until the liquid of stripping is colourless;
7) with the distilled water of 40ml, the sample in conical flask is washed 3 times respectively, after washing, all cleaning fluid is moved in the volumetric flask of step 5) at every turn, and solution in volumetric flask is settled to scale with distilled water, shake up, to be measured;
8) sample drying in taking-up conical flask is to constant weight, and weighing its quality is 2.178g, is designated as m
1;
9) with softening water, make reference solution, getting in step 7) volumetric flask the solution of constant volume, on spectrophotometer, to measure maximum absorption wavelength be 595nm, and the absorbance of measuring this solution under this maximum wavelength is 0.376, is designated as A
1;
10) fixation sample is padded with fixation liquid 100ml on horizontal sample padding machine, then the cloth specimen padding after fixation liquid is suspended on to vapour steaming colour fixing 60s in 98 ℃ of sample steaming boxes;
11) the fixation sample through step 10) is operated by step 3) ~ step 9), record the m of sample
2and A
2numerical value is respectively 2.026g and 0.052;
12) reference is padded with reference fixation liquid 100ml on horizontal sample padding machine, pad the volumetric flask that raffinate in rear collection padding machine moves to 500ml, and shake up after being settled to volumetric flask scale with distilled water diluting, under the measured maximum absorption wavelength of step 9), measure the absorbance A of reference solution
3be 0.029;
13) reference washing is dried to constant weight, weighing its quality is 2.101g, is designated as m
3;
14) by data measured substitution formula
can calculate and obtain dye fixing rate F is 77.1%.
Embodiment 3: test the degree of fixation of certain company's one double-active radical dye Red HF-3B concentration while being 40g/L, fabric specification CPT40*CM30*114*70*55 used, partly floats mercerized cloth, plain weave.Concrete steps are
1) prepare reagent, comprise that massfraction is 40% urea liquid, acetum, fixation liquid and the reference fixation liquid that volume fraction is 0.1%, wherein soda ash 30g/L, caustic soda 4g/L, glauber salt 260g/L, reservehao S 2g/L in fixation liquid, all the other are water, and reference fixation liquid adopts the solution that glauber salt concentration is 260g/L;
2) extract dye liquor 250ml, preparing long * wide is one, 30cm*20cm fabric, on masis small model machine, pad dye liquor, then on masis automatic sizing dryer, dry, during oven dry, guaranteeing that cloth cover is smooth enters cloth, then the fabric after drying is divided into three, is respectively not fixation sample, fixation sample, reference;
3) fixation cloth specimen is not inserted in the conical flask that fills 80ml acetic acid, sample is all immersed in wherein;
4) acetum of conical flask is transferred in 500mL volumetric flask, then to the urea liquid that adds 75ml in conical flask, conical flask is put in to the 6min that strips in boiling water;
5) liquid of stripping in conical flask in step 4) is moved in the volumetric flask in step 4), then in conical flask, add 75ml urea, 6min strips in continuation boiling water;
6) repeating step 5), until the liquid of stripping is colourless;
7) with the distilled water of 40ml, the sample in conical flask is washed 3 times respectively, after washing, all cleaning fluid is moved in the volumetric flask of step 5) at every turn, and solution in volumetric flask is settled to scale with distilled water, shake up, to be measured;
8) sample drying in taking-up conical flask is to constant weight, and weighing its quality is 2.277g, is designated as m
1;
9) with softening water, make reference solution, get in step 7) volumetric flask the solution of constant volume and on spectrophotometer, measure maximum absorption wavelength 517nm, and the absorbance of measuring this solution under this maximum wavelength is 1.318, be designated as A
1;
10) fixation sample is padded with fixation liquid 100ml on horizontal sample padding machine, then the cloth specimen padding after fixation liquid is suspended on to vapour steaming colour fixing 60s in 102 ℃ of sample steaming boxes;
11) the fixation sample through step 10) is operated by step 3) ~ step 9), record the m of sample
2and A
2numerical value is respectively 2.281g and 0.081;
12) reference is padded with reference fixation liquid 100ml on horizontal sample padding machine, pad the volumetric flask that raffinate in rear collection padding machine moves to 500ml, and shake up after being settled to volumetric flask scale with distilled water diluting, under the measured maximum absorption wavelength of step 9), measure the absorbance A of reference solution
3be 0.054;
13) reference washing is dried to constant weight, weighing its quality is 2.250g, is designated as m
3;
14) by data measured substitution formula
can calculate and obtain dye fixing rate F is 89.7%.