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A kind of preparation method of pulp, fabric bleaching catalyst ligand

A technology for fabric bleaching and catalyst, which is applied in the field of preparation of bleaching catalyst ligands, can solve problems such as environmental protection restrictions, and achieve the effects of less three wastes, simple preparation method, and easy-to-obtain raw materials

Active Publication Date: 2016-04-27
苏州正济药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But compared with the patent application of Donghua University, which used p-toluenesulfonyl chloride, 1mol of 1,4,7-trimethyl-1,4,7-triazacyclononane used at least 5mol of p-toluenesulfonate Acyl chlorides will produce a large amount of high-salt wastewater of sodium p-toluenesulfonate and sodium chloride, which has great environmental protection restrictions in industrial applications

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 100 grams of diethylenetriamine, 390 grams of sodium carbonate, 520 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 4 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 - 482 grams of triphenylsulfonyl-diethylenetriamine, yield 96.7%, HPLC purity 97.3%.

[0018] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 482 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 480 grams of potassium carbonate, the temperature is controlled at 75°C to 90°C, 115 grams of ethylene glycol dicarboxylate is added dropwis...

Embodiment 2

[0021] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 100 grams of diethylenetriamine, 380 grams of sodium carbonate, 520 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 5 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 - 482 grams of triphenylsulfonyl-diethylenetriamine, yield 96.7%, HPLC purity 97.3%.

[0022] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 482 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 480 grams of sodium bicarbonate, the temperature was controlled at 75 ° C ~ 90 ° C, 115 grams of ethylene glycol diacetate was added dropwis...

Embodiment 3

[0025] Ⅰ, Synthesis of 1,4,7-triphenylsulfonyl-diethylenetriamine, add 2000ml of clear water, 150 grams of diethylenetriamine, 600 grams of sodium carbonate, 780 grams of benzenesulfonyl chloride pre-melted liquid in a 5000ml four-necked flask (melting point 14.5°C). Under stirring, react at 60°C for 2 hours, 80°C for 7 hours, cool down to 40°C, filter out the white solid with suction, rinse twice with an appropriate amount of water to obtain the white solid of sulfonylated diethylenetriamine 1,4,7 -724 grams of triphenylsulfonyl-diethylenetriamine, yield 96.8%, HPLC purity 97.3%.

[0026] Ⅱ. Synthesis of 1,4,7-triphenylsulfonyl-1,4,7-triazacyclononane, in a 3000ml four-neck flask equipped with a stainless steel turbine stirring paddle, adding 1500ml of N,N-diethyl base formamide, 724 grams of 1,4,7-triphenylsulfonyl-diethylenetriamine, 750 grams of sodium bicarbonate, the temperature is controlled at 75 ° C ~ 90 ° C, 173 grams of ethylene glycol dicarboxylate is added dropwi...

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PUM

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Abstract

The invention discloses a method for preparing a ligand of a pulp and fabric low-temperature bleaching catalyst. The main steps include: dissolving diethylenetriamine with a sulfonyl group in an organic solvent, adding an alkaline reagent and ethylene glycol dicarboxylic acid ester, react at 80-150°C for 6-20 hours, after the reaction, cool to room temperature and filter to obtain 1,4,7-trisulfonyl-1,4,7-triazacyclononane; Add the solid to sulfuric acid, stir at 80-130°C for 2-12 hours, add alkali to neutralize after cooling down, then add formaldehyde and formic acid to reflux to obtain 1,4,7-trimethyl-1,4,7-triaza Cyclononane. The preparation method of the invention is simple, the raw materials are easy to obtain, and the three wastes are less, which is suitable for industrial production and meets the environmental protection requirements of the current industrial production.

Description

technical field [0001] The invention belongs to the field of preparation of bleach catalyst ligands, in particular to the preparation of low-temperature bleach catalyst ligands. Background technique [0002] The fabric and pulp are bleached with hydrogen peroxide, with pure whiteness, no yellowing, no corrosion and no pollution to the equipment, but the high bleaching temperature will cause the fabric and pulp fibers to be partially broken, resulting in loss of strength. [0003] Manganese complex catalyst using 1,4,7-trimethyl-1,4,7-triazacyclononane as a ligand, Mn 2 (μ-O) 3 (MeTACN) 2 m 2 ·nH 2 O, where M is PF 6 , Cl or CH 3 COO is a kind of high-efficiency oxidation catalyst, which enables hydrogen peroxide to effectively bleach fabrics and pulp at relatively low temperature (50-70°C) and low alkalinity (pH9-10) in a short period of time (5-8 hours). The bleached fabric has high whiteness, less fiber breakage and high strength. [0004] However, the current prod...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D255/02B01J31/22
Inventor 蒋勇徐仁华
Owner 苏州正济药业有限公司
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