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Multi-functional-group high-absorption chrome tanning auxiliary agent as well as preparation method and application thereof

A multifunctional, high absorption technology, applied in the application, nitrile preparation, carboxylate/lactone preparation, etc., can solve the problems of poor chromium fixability, unable to meet the needs of high absorption chrome tanning process, etc. Promote cleaner production and improve the effect of coordination sites

Active Publication Date: 2021-05-14
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] With the continuous deepening of research on high-absorption chrome tanning technology, a single functional group additive can no longer meet the needs of high-absorption chrome tanning technology
For example, monobasic or dibasic carboxylic acid compounds can have a certain masking effect on chromium salts, but have poor fixation to chromium

Method used

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  • Multi-functional-group high-absorption chrome tanning auxiliary agent as well as preparation method and application thereof
  • Multi-functional-group high-absorption chrome tanning auxiliary agent as well as preparation method and application thereof
  • Multi-functional-group high-absorption chrome tanning auxiliary agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Synthesis of Polycarboxylic Ester

[0032] Add 0.1 mol of diethyl 3-ketoglutarate, ground and dried K 2 CO 3 (0.02mol), 1g tetrabutylammonium bromide and 500mL n-hexane, add dropwise 0.41mol methyl acrylate, about 20min to finish dripping, reflux reaction for 6h, stop, suction filtration, filter, extract n-hexane, precipitate solid, pump Filter polycarboxylate, product structural formula is as follows:

[0033]

[0034] (2) Hydrolysis of polycarboxylic acid ester

[0035] Add 0.1mol of polycarboxylic acid ester to a 500mL four-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 200mL of potassium hydroxide solution with a mass fraction of 20%, stir at 60°C for 2 hours, and then adjust the pH to 4-5. Filter to obtain the product, and dry it in a vacuum oven at 65°C for 4 hours. The structural formula of the product is as follows:

[0036]

[0037] H NMR spectra of polycarboxylates (DMSO-d6)

[0038] 4.08ppm (q,4H,-COOCH 2 CH ...

Embodiment 2

[0044] (1) Synthesis of tetravalent nitrile esters

[0045] Add 0.1 mol of diethyl 3-ketoglutarate, ground and dried K 2 CO 3 (0.02mol), 2g tetrabutylammonium bromide and 500mL n-hexane, add dropwise 0.41mol acrylonitrile, drop it for about 20min, reflux for 6h, stop, suction filter, filter, remove n-hexane, precipitate solid, suction filter Obtain tetravalent nitrile ester, product structural formula is as follows:

[0046]

[0047] (2) Hydrolysis of tetravalent nitrile ester

[0048] In a 500mL four-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.1mol of tetravalent nitrile ester, add 200mL of potassium hydroxide solution with a mass fraction of 20%, stir at 60°C for 2h, and adjust the pH to 4-5. Filter to obtain the product, and dry it in a vacuum oven at 65°C for 4 hours. The structural formula of the product is as follows:

[0049]

[0050] H NMR spectrum of tetravalent nitrile esters (DMSO-d6)

[0051] 4.08ppm (q,4H,-COOCH 2 C...

Embodiment 3

[0056] (1) Synthesis of Polycarboxylic Ester

[0057] Add 0.1 mol of diethyl dibenzoate acetone, ground and dried K 2 CO 3 (0.02mol), 3.2g polyethylene glycol 1000 (PEG1000) and 500mL petroleum ether, add 0.42mol methyl acrylate dropwise, drop it for about 20min, reflux for 5h, stop, filter with suction, filter, and let the filtrate stand and remove Sherwood oil, separate out solid, obtain polycarboxylate by suction filtration, product structural formula is as follows:

[0058]

[0059] (2) Hydrolysis of polycarboxylic acid ester

[0060] Add 0.1mol polycarboxylic acid ester to a 500mL four-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 250mL of a 25% sodium hydroxide solution, stir at 65°C for 7h, and then adjust the pH with acid To 4-5, filter to obtain the product, and dry it in a vacuum oven at 65°C for 4 hours. The structural formula of the product is as follows:

[0061]

[0062] H NMR spectrum of polycarboxylates (DMSO-d6)

...

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Abstract

The invention discloses a multi-functional-group high-absorption chrome tanning auxiliary agent and a preparation method and application thereof. The structure of the auxiliary agent is a polycarboxylic acid compound containing ketone carbonyl. The invention further discloses a preparation method and application of the high-absorption chrome tanning auxiliary. According to the invention, six-membered carboxyl can be introduced on leather collagen through ketone carbonyl, so that the number of collagen side chain carboxyl is increased, coordination groups of chromium are multiplied, the absorption of trivalent chromium is remarkably improved, the concentration of trivalent chromium in chrome tanning wastewater is reduced, the environmental pollution of the leather industry is reduced, and clean production of the leather industry is promoted. The method is easy to operate, and a new thought is provided for research of the high-absorption chrome tanning auxiliary agent.

Description

technical field [0001] The invention relates to a high-absorption chrome tanning auxiliary and its preparation method and application, in particular to a multifunctional high-absorption chrome tanning auxiliary and its preparation method and application. Background technique [0002] Chrome tanning is by far the most important and widely used tanning method in leather manufacturing. It endows leather with the highest thermal stability, comfortable handle and excellent leather performance. It currently occupies an absolute dominant position in the tanning industry and cannot be Alternatives to other tanning methods. However, in the traditional tanning process, the absorption rate of chrome tanning agent is usually only about 70%. After tanning, high-concentration chromium-containing wastewater will be produced, resulting in a large loss of chrome tanning agent. This not only increases the environmental pollution load and wastewater treatment costs, but also causes a great wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C14C3/08C14C3/06C14C1/08C07C59/347C07C65/34C07C51/09C07C51/08
CPCC14C3/08C14C3/06C14C1/08C07C59/347C07C65/34
Inventor 王国伟欧阳迈胡柯慧庄玲华
Owner NANJING UNIV OF TECH
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