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Preparation method for diphenylketone tetraformate serving as light-induced antibacterial finishing agent

A technology of benzophenone tetracarboxylate and benzophenone tetracarboxylic dianhydride is applied in the field of preparation of light-induced antibacterial finishing agent benzophenone tetracarboxylate, which can solve complex production process and harsh reaction conditions , Harmful skin and other problems, to achieve broad-spectrum antibacterial properties, mild reaction conditions, long-lasting antibacterial effect

Active Publication Date: 2017-12-29
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But these several types of polyester antibacterial agents all have deficiencies, for example, the affinity between inorganic nanoparticle antibacterial agents and polyester fibers is poor, the particle size is small, and it is easy to penetrate into the skin, which is harmful to the skin; quaternary ammonium salt antibacterial agents are less active low, and the durability is worse; while the synthetic raw materials of haloamines are more expensive, the reaction conditions are harsh, the production process is complicated, and the yield is low

Method used

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  • Preparation method for diphenylketone tetraformate serving as light-induced antibacterial finishing agent
  • Preparation method for diphenylketone tetraformate serving as light-induced antibacterial finishing agent
  • Preparation method for diphenylketone tetraformate serving as light-induced antibacterial finishing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In a 100mL three-necked flask equipped with a reflux condenser, a water separator and a thermometer, add 10.00g of 3,3',4,4'-benzophenone tetracarboxylic dianhydride and 15.00mL of n-butanol in sequence, 0.27mL of concentrated sulfuric acid was slowly added dropwise, stirred continuously, and the temperature was raised to 120°C for reaction. The reaction was observed to be complete by thin-layer chromatography. After the system was cooled to room temperature, the 2 CO 3 The solution was washed to neutrality, the organic phases were combined, dried with anhydrous sodium sulfate, filtered, and the filtrate was distilled under reduced pressure to obtain crude butyl 3,3',4,4'-benzophenone tetracarboxylate. The mixed solution of dichloromethane and methanol with a ratio of 7:1 was used as an eluent, and column chromatography was carried out for separation and purification to obtain 16.72 g of pure product 3,3',4,4'-benzophenone tetracarboxylate. The rate is 92.45%. The NMR...

Embodiment 2

[0039] In a 100mL three-neck flask equipped with a reflux condenser, a water separator and a thermometer, add 10.00g of 3,3',4,4'-benzophenone tetracarboxylic dianhydride and 8.70mL of ethanol in sequence, slowly Add 0.05mL concentrated sulfuric acid dropwise, stir continuously, heat up to 150°C for reaction, observe the reaction is complete by thin-layer chromatography, wait for the system to cool to room temperature, and use 15% Na 2 CO 3 The solution was washed to neutrality, and the organic phases were combined, dried with anhydrous sodium sulfate, filtered, and the filtrate was distilled under reduced pressure to obtain crude ethyl 3,3',4,4'-benzophenone tetracarboxylate. A mixture of dichloromethane and methanol at a ratio of 7:1 was used as the eluent, and column chromatography was performed for separation and purification to obtain 13.12 g of pure ethyl benzophenone tetracarboxylate with a yield of 90%. The NMR of the product 3,3',4,4'-ethyl benzophenone tetracarboxyl...

Embodiment 3

[0041] The 3,3',4,4'-benzophenone tetracarboxylate obtained in Example 1 is used for finishing polyester fabrics, the specific method is as follows:

[0042] (1) Add 1.5 g of emulsifier Tween 80 to 150 mL of distilled water, stir for 30 min to obtain an emulsifier solution, then slowly add 15 g of 3,3',4,4'-benzophenone tetracarboxylate in Example 1 Esters, stirred for 1h, to obtain a finishing working solution with an effective concentration of antibacterial agent of 100g / L.

[0043](2) Immerse the unfinished polyester fabric in the finishing working solution in step (1), use two dipping and two padding (the liquid-carrying rate is 90%), pre-bake at 80°C for 3min, and bake at 180°C for 2.5min, Get antibacterial polyester fabric. Take the antibacterial polyester fabric, and wash it 30 times with water according to the washing procedure of FZ / T73023-2006 "Antibacterial Knitwear Appendix C Antibacterial Fabric Sample Washing Test Method".

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Abstract

The invention relates to a preparation method for diphenylketone tetraformate serving as a light-induced antibacterial finishing agent. The preparation method comprises the following steps: adding 3,3',4,4'-benzophenonetetracarboxylic dianhydride and alcohol into a reaction kettle which is provided with a water distributor; stirring, slowly adding concentrated sulphuric acid dropwise for reacting, cooling to room temperature, washing, drying, filtering and separating to obtain the diphenylketone tetraformate serving as the light-induced antibacterial finishing agent. The method disclosed by the invention is simple and easy to operate; reaction conditions are mild, and the cost is low; the prepared diphenylketone tetraformate has high-efficiency, lasting and broad-spectrum anti-bacterial performance, has strong affinity with polyester fibres, and is used for finishing a polyester fabric; the finished fabric has high-efficiency and lasting anti-bacterial performance on staphylococcus aureus and Escherichia coli.

Description

technical field [0001] The invention belongs to the field of textile antibacterial, in particular to a preparation method of a light-induced antibacterial finishing agent benzophenone tetracarboxylate. Background technique [0002] In the past two decades, my country's chemical fiber industry has achieved rapid development. Among them, the output of polyester fiber accounts for three-quarters of the total output of chemical fiber. Because of its excellent performance, it is widely used in clothing, medical and other fields. [0003] Due to the high hydrophobicity and compact structure of polyester fabrics, there are no active groups that can react. Therefore, compared with natural fibers, the antibacterial finishing durability of polyester fabrics is poor, and the affinity between most antibacterial agents and polyester macromolecules is small. At present, the antibacterial modification of polyester is mainly realized through the blending method. For example, patent CN200510...

Claims

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Application Information

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IPC IPC(8): C07C69/80C07C67/08C07C67/56A01N37/42A01P1/00D06M13/224
CPCA01N37/42C07C67/08C07C67/56D06M13/224D06M16/006C07C69/80
Inventor 侯爱芹胡柳高爱芹张红娟谢孔良
Owner DONGHUA UNIV
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