Preparation method of carboxyl-containing epoxy resin tanning agent

An epoxy resin and carboxyl-containing technology, which can be used in animal husbandry, small raw hide/large raw hide/leather skin/fur chemical treatment, application, etc., can solve the problem of slow development of epoxy resin tanning agents, long reaction time, and the amount of organic solvents Large and other problems, to achieve excellent tanning effect, the effect of shortening the tanning time

Active Publication Date: 2014-04-23
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the research of epoxy resin tanning agents in the leather industry has been in a slow and almost stagnant state, mainly because the reaction time between epoxy resin and collagen is long (generally 3-5 days), the dosage is large, and the shrinkage temperature is relatively high. Low, in addition, R.J.Heath et al. believe that leather researchers lack a deep understanding of epoxy chemistry is also a reason for the slow development of epoxy resin tanning agents (Heath R.J., Di Y., Clara S., et al.Epoxide tannage: a way forward[J].Journal of the Society of Leather Technologists and Chemists,2005,89(5):186-193;Heath R.J.,Di Y.,Clara S.,et al.The optimization of epoxy-based tannage systems -an initial study[J].Journal of the Society of Leather Technologists and Chemists,2005,89(3):93-102)
[0004] Most of the traditional epoxy resins are solvent-based, which will release a large amount of organic pollutants during use, causing pollution to the environment; at the same time, the amount of organic solvents is large, and the price is much higher than that of water, which is extremely important in industrial production. Not advisable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Dissolve 0.9g of sodium bisulfite in 69g of distilled water to prepare an aqueous solution of sodium bisulfite; add the aqueous solution of sodium bisulfite into a 250ml three-necked flask, then heat it in a water bath to 65°C, and at the same time start stirring with the mixer at 300rpm, and turn on the condensate , dropwise while stirring therein the mixed monomer that is made up of the allyl glycidyl ether of 11.25g and the methacrylic acid of 29.25g and the ammonium persulfate aqueous solution prepared by the ammonium persulfate of 3.6g and the distilled water of 36g, The dropping time is controlled at 1 hour, and the temperature is kept at 65°C for 3 hours, and finally cooled to room temperature, and the pH value of the reaction system is adjusted to 5.0 with a 30% NaOH aqueous solution to obtain a carboxyl-containing epoxy resin tanning agent.

Embodiment 2

[0020] Dissolve 1.237g of sodium bisulfite in 55.5g of distilled water to prepare an aqueous solution of sodium bisulfite. Add the aqueous solution of sodium bisulfite into a 250ml three-neck flask, then heat it in a water bath to 60°C, and start stirring at 400rpm with the mixer, and turn on the condensation Water, while stirring, dropwise dropwise therein the ammonium persulfate prepared by the allyl glycidyl ether of 15.75g and the methacrylic acid of 23.06g and the ammonium persulfate prepared by the ammonium persulfate of 4.95g and the distilled water of 49.5g Aqueous solution, the dropping time is controlled at 2h, react at a constant temperature at 60°C for 4.5h, and finally cool to room temperature, use NaOH aqueous solution with a mass concentration of 30% to adjust the pH value of the reaction system to 4.0 to obtain carboxyl-containing epoxy resin tanning agent.

Embodiment 3

[0022] Dissolve 1.01g of sodium bisulfite in 64.5g of distilled water to prepare an aqueous solution of sodium bisulfite. Add the aqueous solution of sodium bisulfite into a 250ml three-necked flask, then heat it in a water bath to 58°C, and start stirring at 450rpm with the mixer, turn on Condensed water, while stirring, dropwise dropwise therein the ammonium persulfate prepared by the allyl glycidyl ether of 9g and the methacrylic acid of 31.5g and the ammonium persulfate prepared by the ammonium persulfate of 4.05g and the distilled water of 40.5g Aqueous solution, the dropping time is controlled at 1.8h, constant temperature reaction at 58°C for 4.2h, and finally cooled to room temperature, using NaOH aqueous solution with a mass concentration of 30% to adjust the pH value of the reaction system to 3.5 to obtain carboxyl-containing epoxy resin Tanning agent.

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Abstract

A preparation method of a carboxyl-containing epoxy resin tanning agent comprises the steps: adding a sodium hydrogen sulfite aqueous solution into a reactor, then heating to 50-65 DEG C, dropwise adding allyl glycidyl ether, methacrylic acid and an ammonium persulfate aqueous solution with stirring, followed by carrying out a constant temperature reaction for 3-5 h at the temperature of 50-65 DEG C, finally, cooling to the room temperature, regulating the pH value of the obtained reaction system to 2.0-5.5, and thus obtaining the carboxyl-containing epoxy resin tanning agent. The preparation method of the tanning agent is simple and convenient in operation process; the tanning agent has a certain tanning effect and is combined with 3% of a chromium powder to tan sheep skin acid skin, the shrinkage temperature of crust leather after being tanned is allowed to reach about 110 DEG C, and the thickening rate is allowed to reach about 105%; and at the same time, compared with a 8% chromium powder traditional tanning method, the Cr2O3 content in waste liquid after chrome tanning is reduced by about 77.5%.

Description

technical field [0001] The invention belongs to the technical field of leather chemical synthesis, relates to a tanning agent used in the leather tanning process and a preparation method thereof, in particular to a preparation method of a carboxyl-containing epoxy resin tanning agent. Background technique [0002] In the tanning industry, chrome tanning agent is currently the most widely used and the largest amount of tanning agent due to its excellent leather performance, low cost and mature technology. However, chromium is a scarce resource. According to surveys, chromium resources are currently in short supply. At the same time, the absorption and utilization rate of chromium in bare leather in the traditional chrome tanning method is relatively low, only about 70%, and a large amount of unabsorbed chromium Compounds are discharged along with tannery wastewater, causing serious pollution to the environment. At present, tanning workers have begun to focus on research on c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F216/14C08F4/40C14C3/22
Inventor 高党鸽李蕊吕斌马建中
Owner SHAANXI UNIV OF SCI & TECH
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