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Preparation method of alkoxylation intermediates on the basis of diester-sebacate nitroxyl radicals

A technology of sebacic acid diester nitroxide free radicals and nitroxide free radicals, which is applied in the field of preparation of alkoxylated intermediates, can solve the problems of complex process, low yield, and reduced yield, and achieve wide source of raw materials , low reaction temperature, rapid reaction effect

Active Publication Date: 2019-07-23
宿迁联盛科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the hindered amine synthesis of this N-alkoxylation is a substitution reaction under the action of a catalyst, which makes the process more complicated and the yield is low
If a more complex group is used for substitution, other N-alkoxylated light stabilizers with significant effects are synthesized by experiment, and the difficulty of substitution is proportional to the complexity of the substituent group, which makes the yield even lower

Method used

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  • Preparation method of alkoxylation intermediates on the basis of diester-sebacate nitroxyl radicals
  • Preparation method of alkoxylation intermediates on the basis of diester-sebacate nitroxyl radicals
  • Preparation method of alkoxylation intermediates on the basis of diester-sebacate nitroxyl radicals

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Effect test

Embodiment 1

[0028] Put 100g of bis(2,2,6,6-tetramethyl-4-hydroxypiperidine) sebacic acid nitroxide free radicals into the electrolytic reaction bottle, and then add 30g of water, 60g of methanol, and 16g of hydroxide Sodium, 30g formic acid, at 800A / m 3 Electrolytic catalytic oxidation under current density, the anode material is BDD electrode, and the cathode material is titanium plate. After 24 hours of electrolysis, the electrolyte solution is filtered to obtain 97g of alkoxylated intermediate product of sebacic acid diester nitroxide free radical, the content (GC) 97.40%, the yield is about 89%.

[0029]

[0030] figure 1 It is the infrared spectrogram of the product prepared under formic acid environment; before electrolysis, there is no characteristic peak of hydroxyl (νOH) in the functional group region, and the infrared peak of the product after electrolysis corresponds to 3405 (νOH) with a characteristic peak of hydroxyl; it shows that in the electrolysis reaction, nitrogen ...

Embodiment 2

[0033] Put 100g of bis(2,2,6,6-tetramethyl-4-hydroxypiperidine) sebacic acid nitroxide free radicals into the electrolytic reaction bottle, and then add 15g of water, 40g of methanol, and 8g of hydroxide Sodium, 30g formic acid, at 300A / m 3 Electrolytic catalytic oxidation under current density, the anode material is BDD electrode, the cathode material is titanium plate, after 24 hours of electrolysis, the electrolyte solution is filtered to obtain 88g of alkoxylated intermediate product of sebacic acid diester nitroxide free radical, the content (GC) 88.35%, the yield is about 82%.

Embodiment 3

[0035] Put 100g of bis(2,2,6,6-tetramethyl-4-hydroxypiperidinyl) sebacic acid nitroxide free radical into the electrolytic reaction bottle, then drop into 45g of water, 50g of methanol, and 6g of hydroxide Potassium, 50g formic acid, at 600A / m 3 Electrolytic catalytic oxidation under current density, the anode material is BDD electrode, and the cathode material is titanium plate. After 24 hours of electrolysis, the electrolyte solution is filtered to obtain 93g of alkoxylated intermediate product of sebacic acid diester nitroxide free radical, the content (GC) 93.25%, the yield is about 85%.

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Abstract

The invention relates to the technical field of preparation of light stabilizers and particularly relates to a preparation method of alkoxylation intermediates on the basis of diester-sebacate nitroxyl radicals. The preparation method comprises the following steps: carrying out electrolytic catalytic oxidation on bis(2,2,6,6-tetramethyl-4-hydroxypiperidine) sebacate nitroxyl radicals under the existence of water, alcohol, alkali and HCOOH to prepare the alkoxylation intermediates. The preparation method involved in the invention has the following beneficial effects that a reaction is low in temperature compared with a conventional reaction, catalysts are not needed and the reaction is rapid; raw materials are wide in source and low in cost; the final yield of a product is high, so that thepreparation method has more economic value.

Description

technical field [0001] The invention relates to the technical field of light stabilizer preparation, in particular to a method for preparing an alkoxylation intermediate based on sebacic acid diester nitroxide free radical. Background technique [0002] In order to improve the weather resistance of plastic products, light stabilizers are often added in the production process. Most of the existing light stabilizers are hindered amine light stabilizers, such as bis(1-octyloxy-2,2,6,6-tetramethyl-4-piperidinyl) sebacate is a Hindered amine light stabilizer. For example, the Chinese patent with publication number CN106699639A discloses a synthesis method of light stabilizer HS-112. It should be noted that the light stabilizer HS-112 is the trade name of bis(1-octyloxy-2,2,6,6-tetramethyl-4-piperidinyl) sebacate. The patent mentions that by reacting molybdenum trioxide as a catalyst, n-octane as a raw material and a solvent with bis(2,2,6,6-tetramethylpiperidinyl) sebacate nit...

Claims

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Application Information

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IPC IPC(8): C25B3/02C25B11/04C25B3/23
CPCC25B11/04C25B3/23
Inventor 韩炎胡新利王晶赵飞邓啸韬
Owner 宿迁联盛科技股份有限公司
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