Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of hindered amine alkoxylated intermediate

A technology of oxygenation and intermediates, applied in the field of preparation of intermediates, can solve the problems of complex hindered amine synthesis process and low yield, and achieve the effect of low reaction temperature, high yield and rapid reaction temperature

Active Publication Date: 2019-05-31
宿迁联盛科技股份有限公司
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the weathering test, it was found that N-alkoxylated hindered amines are not only acid-resistant, but also have a better light stabilizing effect than hindered amine light stabilizers with secondary amine structures, but conventional N-alkoxylated hindered amines are synthesized The process is more complicated and the yield is low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of hindered amine alkoxylated intermediate
  • Preparation method of hindered amine alkoxylated intermediate
  • Preparation method of hindered amine alkoxylated intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put 50g of raw material A into the electrolysis reaction bottle, and then put in 4g of water, 60g of methanol, 3g of potassium carbonate, and 40g of acetic acid respectively. The electrolysis temperature is 60°C, at 800A / m 3 Electrolytic catalytic oxidation under current density, the anode material is graphite, the cathode material is stainless steel, after 12 hours of electrolysis, the electrolyte solution is filtered to obtain 44g of the methoxy product of tetramethylpiperidine, the content (GC) is 98.5%, and the yield is about 80 %.

[0032]

[0033] raw material A

Embodiment 2

[0035] Put 50g of raw material B into the electrolysis reaction bottle, and then put in 15g of water, 100g of methanol, 5g of potassium hydroxide, and 60g of propionic acid respectively. The electrolysis temperature is 60°C, and at 1000A / m 3 Electrolytic catalytic oxidation under current density, the anode material is graphite, and the cathode material is stainless steel. After 12 hours of electrolysis, the electrolyte is filtered to obtain 49g of the ethoxy product of tetramethylpiperidone, with a content (GC) of 98.2%, and a yield of about 78%.

[0036]

[0037] raw material B

Embodiment 3

[0039] Put 50g of raw material C into the electrolysis reaction bottle, and then put in 30g of water, 200g of methanol, 4g of potassium hydroxide, and 100g of propionic acid respectively. The electrolysis temperature is 60°C, and at 1000A / m 3 Electrolytic catalytic oxidation under current density, the anode material is graphite, and the cathode material is stainless steel. After electrolysis for 12 hours, filter the electrolyte solution to obtain 90g of tetramethylpiperidine ethoxy product with a content (GC) of 99.1% and a yield of about 76 %.

[0040]

[0041] raw material C

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention belongs to the technical field of preparation of photostabilizers and particularly relates to a preparation method of a hindered amine alkoxylated intermediate. The hindered amine alkoxylated intermediate is prepared by subjecting tetramethylpiperidine nitroxide free radicals, tetramethylpiperidone nitroxide free radicals or tetramethyl-4-piperidinol nitroxide free radicals to electrocatalytic oxidation in the presence of water, an alcohol, a base and RCOOH. A NOR (N-alkoxy) type hindered amine light stabilizer intermediate is synthesized herein through electrocatalytic oxidationfor the first time; the preparation method has the advantages of low reaction temperature, high speed, high yield and the like; the preparation materials are widely resourceful and low in price.

Description

technical field [0001] The invention belongs to the technical field of light stabilizer preparation, in particular to a method for preparing an intermediate of hindered amine alkoxylation. Background technique [0002] Adding hindered amine light stabilizers is a mature and stable method in the process of plastic weather resistance, which can effectively improve the weather resistance of plastic products. The secondary amine structure of conventional hindered amine light stabilizers has a relatively high basicity, which limits the application under acidic conditions. Generally speaking, the alkalinity of N-alkoxylated hindered amines is significantly lower, and representative varieties such as light stabilizer 371, light stabilizer 123, etc. In the weathering test, it was found that N-alkoxylated hindered amines are not only acid-resistant, but also have a better light stabilizing effect than hindered amine light stabilizers with secondary amine structures, but conventional...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C25B3/02C25B3/23
Inventor 王晶韩炎张超胡方洲杜伟伟胡新利项瞻峰项瞻波
Owner 宿迁联盛科技股份有限公司