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A kind of preparation method of cationic fluorescent fatliquoring agent
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A cationic, fatliquoring technology used in leather chemicals to achieve good compatibility
Active Publication Date: 2022-06-03
QILU UNIV OF TECH
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[0004] At present, there is no report about cationic fluorescent-labeled fatliquor for studying the mass transfer and distribution of cationic fatliquor in leather
Method used
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Embodiment 1
[0033] 28.4 parts of stearic acid, 28.2 parts of palmitic acid and 14.9 parts of triethanolamine were reacted at 120° C. for 8 h under nitrogen protection to obtain intermediate product A. Take 71.5 parts of A, add 9.8 parts of maleic anhydride, and react at 105° C. for 3 hours to obtain intermediate product B. Add 0.813 parts of B to 50 parts of dimethylformamide, then add 0.35 parts of 5-aminofluorescein and 0.48 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, Reaction at 40 ° C for 5 h to obtain product C. Add C into 100 parts of dichloromethane, then add 50 parts of water, mix evenly, and let stand for stratification. Collect the organic phase, then add 100 parts of water, mix well, and then let stand for layers. The organic phase was collected, 150 parts of water was added, and the mixture was evenly mixed and then allowed to stand for layers. Take 1 part of D, dissolve it in 20 parts of absolute ethanol, add benzyl chloride in an equimolar ratio ...
Embodiment 2
[0035] 25.6 parts of palmitic acid and 14.9 parts of triethanolamine were taken and reacted at 180° C. for 3 h under nitrogen protection to obtain intermediate product A. Take 40.5 parts of intermediate product A, add 12.8 parts of adipic anhydride and 11.2 parts of itaconic anhydride, and react at 105° C. for 1.5 h to obtain intermediate product B. Take 0.6 part of B and add it to 30 parts of dimethyl sulfoxide, then add 0.35 part of 5-aminofluorescein and 0.48 part of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride. Reaction at 20°C for 10h to obtain product C. Add C into 50 parts of dichloromethane, then add 50 parts of water, mix evenly, and then let stand for stratification. Collect the organic phase, then add 100 parts of water, mix well, and then let stand for layers. The organic phase was collected, 150 parts of water was added, and the mixture was evenly mixed and then allowed to stand for layers. Take 1 part of D, dissolve it in 100 parts of absolute e...
Embodiment 3
[0037] 30 parts of lauric acid and 14.9 parts of triethanolamine were reacted at 160° C. for 4 h under nitrogen protection to obtain intermediate product A. Take 44.9 parts of A, add 7.4 parts of phthalic anhydride and 9.8 parts of maleic anhydride, and react at 75° C. for 3.5 hours to obtain intermediate product B. Take 1 part of B and add it to 100 parts of dimethylformamide, then add 1.2 parts of 5-aminofluorescein and 2 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride, Reaction at 20 ° C for 10 h to obtain product C. Add C into 100 parts of dichloromethane, then add 100 parts of water, mix evenly, and let stand for layers. Collect the organic phase, then add 200 parts of water, mix well, and then let stand for stratification. The organic phase was collected, 200 parts of water was added, mixed evenly, and then allowed to stand for layers. Take 1 part of D, dissolve it in 50 parts of absolute ethanol, add benzyl chloride in an equimolar ratio with D, ...
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Abstract
The invention relates to a preparation method of a cationic fluorescent fatliquoring agent. The steps are as follows: (1) using a fatty acid and triethanolamine to react under nitrogen protection to obtain an intermediate product A; (2) taking the intermediate product A to react with an acid anhydride to obtain an intermediate product B , then B was dissolved in dimethylformamide or dimethyl sulfoxide and added 5-aminofluorescein and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride for reaction, Obtain product C, (3) add dichloromethane and water in reaction product C, leave standstill layering after fully mixing, collect organic phase; Dichloromethane is removed by organic phase decompression distillation, obtain intermediate product D, ( 4) Take the intermediate product D and dissolve it in absolute ethanol, add benzyl chloride, condense and reflux the reaction, and remove the ethanol by rotary evaporation under reduced pressure to obtain the fluorescent marker E. (5) Take E and add ethylene glycol monobutyl ether, and mix well Add them together to the commercial cationic fatliquoring agent, that is. The invention can well reflect the distribution status of the fatliquor in the leather.
Description
technical field [0001] The invention belongs to the field of leather chemicals, in particular to a preparation method of a cationic fatliquoring agent with fluorescent properties. Background technique [0002] With the development of chrome-free tanning technology, the development and application of cationic fatliquor are becoming more and more extensive. Studying the structure-activity relationship of cationic fatliquor has important theoretical guiding significance for its development and application, but there is still no effective technical method to analyze the mass transfer and distribution of cationic fatliquor in leather. Fluorescent tracer technology is an effective means to monitor the mass transfer and distribution of target substances, which provides the possibility to analyze the mass transfer and distribution of chemical materials in leather. [0003] The patent document JP2017082355A discloses a synthetic leather and a manufacturing method thereof. The synthe...
Claims
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