A kind of preparation method of polyaldehyde-based polymer tanning agent

A technology of polymer and polyaldehyde group, applied in the field of preparation of polyaldehyde-based polymer tanning agent, can solve the problems of low aldehyde group content and low aldehyde group density, and achieve high aldehyde group content, high aldehyde group density, excellent water soluble effect

Active Publication Date: 2021-05-18
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a polyaldehyde tanning agent for the problems of low aldehyde group content, low aldehyde group density, and use of organic solvents or strong irritating aldehyde group-containing monomers in the preparation process in the prior art. The preparation method of polymer-based tanning agent is characterized in that a polyaldehyde-based polymer tanning agent with high aldehyde group content, high aldehyde group density and good water solubility is prepared through two-step reaction of free radical homopolymerization and TEMPO catalytic oxidation. The preparation process It is carried out in the water phase, under mild conditions, without the use of organic solvents or strong aldehyde-containing monomers

Method used

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  • A kind of preparation method of polyaldehyde-based polymer tanning agent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 744 g of water and 3 g of sodium hypophosphite are placed in the reactor, stirred to dissolve and heated to 70 o C, dissolve 3 g of ammonium persulfate with 100 g of water, drip the initiator solution and 150 g of hydroxyethyl acrylate into the above-mentioned sodium hypophosphite solution synchronously and uniformly within 2 h, and then keep warm for 6 h to obtain Hydroxyethyl acrylate polymer; cool the above polymer solution to 10 o C, add 0.36 g (accounting for 0.1mol% of hydroxyethyl acrylate) 4-benzoyloxy-2,2,6,6-tetramethylpiperidine-oxyl radical and 13 g (accounting for 10mol% of hydroxyethyl acrylate) %) sodium bromide, and adjust the pH to 9.4 with sodium hydroxide solution, then dropwise add 169 g (accounting for 30 mol% of hydroxyethyl acrylate) potassium hypochlorite solution, and keep warm for 90 min to obtain a polyaldehyde-based polymer tanning agent.

[0025] The aldehyde group content of polyaldehyde-based polymer tanning agent was determined by potent...

Embodiment 2

[0030] Place 600 g of water and 3 g of sodium hypophosphite in the reactor, stir to dissolve and heat up to 85 o C, dissolve 9 g of potassium persulfate with 100 g of water, drip the initiator solution and 300 g of hydroxyethyl acrylate into the above-mentioned sodium hypophosphite solution synchronously and uniformly within 3 h, and then keep warm for 6 h to obtain Hydroxyethyl acrylate polymer; cool the above polymer solution to 5 o C, add 0.40 g (accounting for 0.1 mol% of hydroxyethyl acrylate) 2,2,6,6-tetramethylpiperidine-oxyl radical and 26.6 g (accounting for 10 mol% of hydroxyethyl acrylate) sodium bromide, and use hydrogen Sodium oxide solution was used to adjust the pH to 9.4, and then 278.3 g (accounting for 30 mol% of hydroxyethyl acrylate) sodium hypochlorite solution was added dropwise and kept for 90 min to obtain a polyaldehyde-based polymer tanning agent.

[0031] Measure the aldehyde group content of this tanning agent with the method described in Example 1...

Embodiment 3

[0033] 690 g of water and 4 g of sodium hypophosphite were placed in the reactor, stirred to dissolve and heated to 85 o C, dissolve 6 g of ammonium persulfate with 100 g of water, drip the initiator solution and 200 g of hydroxypropyl acrylate into the above-mentioned sodium hypophosphite solution synchronously and uniformly within 3 h, and then keep warm for 4 h to obtain Hydroxypropyl acrylate polymer; cool the above polymer solution to 5 o C, add 0.33 g (accounting for 0.1 mol% of hydroxypropyl acrylate) 4-acetamido-2,2,6,6-tetramethylpiperidine-oxyl radical and 16 g (accounting for 10 mol% of hydroxypropyl acrylate) bromine sodium chloride, and adjust the pH to 8 with sodium hydroxide solution, then dropwise add 166g (accounting for 30mol% of hydroxypropyl acrylate) sodium hypochlorite solution, and keep warm for 90 minutes to obtain a polyaldehyde-based polymer tanning agent.

[0034] Measure the aldehyde group content of this tanning agent with the method described in ...

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Abstract

The invention discloses a preparation method of a polyaldehyde-based polymer tanning agent, which is characterized in that a polyhydroxy polymer with excellent water solubility is firstly homopolymerized by hydroxyl acrylate free radicals, and then the hydroxyl group is efficiently oxidized into Aldehyde group, to prepare a polyaldehyde-based polymer tanning agent with high aldehyde group content and high aldehyde group density. The preparation process is carried out in an aqueous solution under mild conditions, which is safe and environmentally friendly. The invention can solve the problems of low aldehyde group content and low aldehyde group density of the polymer tanning agent in the prior art, and the use of organic solvents or strong irritating aldehyde group-containing monomers in the preparation process.

Description

technical field [0001] The invention belongs to a preparation method of a leather tanning agent, in particular to a preparation method of a polyaldehyde-based polymer tanning agent. Background technique [0002] Aldehyde tanning agents have become a class of chrome-free tanning agents that have attracted much attention because of their good tanning properties. However, the existing small molecule aldehyde tanning agents, such as modified glutaraldehyde, oxazolidine and organic phosphonium salts, generally have the problem of releasing free formaldehyde during storage and use of tanned leather, which is difficult to meet the requirements of ecological leather. Therefore, it is of great significance to develop a polymer aldehyde tanning agent whose aldehyde group is located on the polymer chain and will not decompose to generate formaldehyde. [0003] The key to the preparation of polymer aldehyde tanning agents is to introduce aldehyde groups into their polymer chains. Luan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F8/06C08F120/20C14C3/22
CPCC08F8/06C08F120/20C14C3/22
Inventor 王亚楠刘宝华石碧曾运航周建飞
Owner SICHUAN UNIV
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