GB/T 5541-1985 Disperse dyes high temperature dispersion stability determination method GB/T5541-1985 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Method for determination of stability of disperse dyes at high temperature for dispersed dyes UDC 666. 8 : 535.6
GB5541-85
This standard is applicable to the determination of the stability of disperse dyes in the process of high temperature and high pressure dyeing. The filtration method and the cycle dyeing method are adopted. The former filters the dye liquor after high temperature treatment and rates the filtration speed and filter paper residue. The latter dyes the polyester strips and rates the change of dye liquor flow rate and dye agglomerates in the dyeing process. The two methods are paralleled as the determination methods for the high temperature dispersion stability test of disperse dyes.
Filtration method
Materials and instruments
Porcelain funnel: Buchner funnel with an inner diameter of 110mm. b.
Filter paper, double bad brand 11mm fast qualitative filter paper and medium-speed qualitative filter paper. Stainless steel ring: outer diameter 11omm, inner diameter 102mm, thickness 8mm. Beaker: 40ml,
cylinder: 200ml.
stopwatch.
day: sensitivity less than 0.18.
electromagnetic stirrer.
acidity meter.
high temperature and high pressure dyeing machine.
filtering device
vacuum beam.
suction filter bottle: 100ml.
Buffer bottle: 200(ml.
Vacuum control tube.
Vacuum-resistant pipe.
The installation of vacuum flow device is shown in the figure!.
Filter bottle
National Bureau of Standards 1985-10-29 Issued
Light measurement limit
Screw flushing bottle
Vacuum gauge
Screw flushing torque
Vacuum pump
1986-08-01 Implementation
GB 5641--85
1.3 Reagents and solutions
#. Disodium ethylenediaminetetraacetic acid (EDTA): (GB 1401-78); chemically pure, 0.25g/L solution. b. Glacial acetic acid: (GB 676-78): Chemically pure, 10% solution. 1.4. Test method
1.4.1 Preparation of disperse dye suspension (hereinafter referred to as dye liquor) Weigh 2.0±0.1g of dye (based on 100 points of dye strength) and place it in a beaker, add EDTA hot solution (50℃, 0.25g/L) 5m) to make a slurry, and then dilute it to 200ml with the same EDTA solution. Stir with an electromagnetic stirrer for 1-2min, and then adjust the pH value to 4.5-5.0l with 10% acetic acid solution.
1.4.2 Heat treatment of dye liquor
Put the dye liquor in a high-temperature and high-pressure dyeing machine, heat it to 130 in 30-40min, then keep it warm for 30min, cool the dye liquor to 85-90℃, and prepare for filtration.
1.4.3 Dyeing process
First, preheat the funnel and stainless steel ring in 90℃ hot water, take them out and wipe them with a towel. Put the qualitative filter paper on the qualitative filter paper, put them into the funnel together, and press them with a steel ring. Turn on the vacuum, pour 85-90% dye solution into the funnel for filtration, and start timing with a stopwatch at the same time. The vacuum degree should be maintained at 560±100mmHg. When the appearance of the filter paper changes from wet to white, it reaches the end point, record the filtration time, stop vacuuming, take out the filter paper, and let the upper filter paper dry for rating. 1.5 Rating
The high temperature stability of the sensitive dye is expressed as "filtration time level-residue level". The filtration time is rated according to the following regulations:
25～495
-50~745
-—75 ～ 12(
120s or more
The residue on the filter paper is compared with the "residue classification" and is rated according to the following regulations: excellent
-poor
1 Grade——worst
2 Cyclic dyeing method
Materials and instruments
Automatic dyeing instrument.
Acidity meter.
Electromagnetic stirrer.
Analysis day and a half: Sensitivity 0.0001g.
Beaker: 400ml.
Graduating cylinder: 300ml.
Polyester strip: Fiber fineness i.5H Niel number, fiber length 38mm. Schematic diagram of dyeing principle of automatic dyeing instrument
2.3 Reagents and solutions
GB 564185
Glacial acetic acid (GB676-78): chemically pure, 10% solution. 2.4 Test method
2.4.1 Filling polyester strips
According to the effective volume of the dyeing glass tube equipped with the dyeing device, weigh the wool strips at a density of 0.3g/cm (for example, if the inner diameter of the glass tube is 17.5mm and the length is 150mm, minus the space for the stainless steel mesh and rubber ring, the effective length is 135mm, and the effective volume is 32.5cm, so 9.7 polyester strips should be weighed). Fold the polyester strips into the required length and pull them into the glass material with a tie. When filling the polyester strips, Try to ensure that the packing density is uniform, then install two rubber rings at each end of the glass tube, and a piece of stainless steel mesh between the two rubber rings. Finally, install the Bonnau tube on the tube rack of the dyeing instrument and prepare for dyeing. 2.4.2 Preparation of dye solution
Weigh the dye according to the dyeing depth of 3% (such as 9.78 polyester strips, weigh 291g of dye), and the weighing error should be less than 0.01. Add a small amount of distilled water to the beaker, adjust the dye into a slurry, and then dilute it with water. The total amount of water is 1000 times the amount of dye. Stir on the electromagnetic stirrer for 5 minutes, and adjust the pH value of the dye to 4.5-5 with acetic acid. 0a2.4.3 Dyeing
Before heating and dyeing, pre-circulate the dye solution. The dye solution circulates in reverse for 5 minutes at the maximum flow rate (turn the stepless speed motor to the maximum), and then stops circulating for 5 minutes. Then adjust the flow rate to 250ml/min, and supply a small amount of compressed air to the dyeing system. Heat up from 40C to 130℃ at a rate of 3℃/min, keep warm for 15 minutes, and quickly cool down to 90℃. If the dye flow rate drops below 40ml/min during the dyeing process, dyeing should be stopped. Record the dyeing time, dyeing temperature and dye flow rate from the beginning of heating. After dyeing, take out the dyed polyester strips and dry them naturally for rating. 2.5 Rating
The high-temperature dispersion stability of disperse dyes is measured by "dye flow rate change level in the heating stage - dye flow rate change level in the insulation stage - The dye flow rate change is rated according to the following provisions: Grade A
230~250ml/min
160~230ml/min
100~16(ml/min
40~100ml/min
Below 40ml/min
Dye agglomerates are rated with reference to Appendix A "Dye agglomerates standard color sample card", and the grade of the sample card is as follows: Grade 5
No agglomeration
Slightly agglomerated
Agglomerated
More obvious agglomeration
Extremely obvious agglomeration
GB5541—B5bzxz.net
Note: When the dye flow rate change grade is Grade E, the agglomerate rating does not need to be carried out because dyeing cannot continue. The text and rating cards of this standard are issued separately. The Chinese part is printed by China Standard Publishing House and issued by Xinhua Bookstore. The rating card for the filtration method adopts the five-level card for residual impurities in the dispersion performance determination method of disperse dyes; the rating card for the cycle dyeing method is produced and issued by Dagang Dye Industry Research Institute.
Additional Notes:
GB5541--85
Appendix A
Standard color sample card for dye sample agglomeration
(Supplement)
Grade 5—slight agglomeration
Grade 4—slight agglomeration
Grade 3—agglomeration
Grade 2—obvious agglomeration
Grade 1—extremely obvious agglomeration
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and was submitted by the Ministry of Chemical Industry of China. The drafting of this standard was contributed by Dagang Dye Industry Research Institute. The drafter of this standard was Zhou Erming.
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