Catalyst, preparation method thereof and use thereof in production of nitroxide radical piperidinols

A nitroxide radical piperidinol and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of difficult wastewater treatment, low conversion rate of raw materials, and low catalytic activity.

Active Publication Date: 2021-04-06
SHANGHAI HUAYI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the prior art proposes using magnesium hydroxide as a catalyst, or using a sodium tungstate-ethylenediaminetetraacetic acid disodium catalyst system to oxidize 2,2,6,6-tetramethyl-4-hydroxypiperone with hydrogen peroxide in aqueous solution Pyridine synthesizes 2,2,6,6-tetramethyl-4-hydroxypiperidine nitroxide radical, but when magnesium hydroxide is used as a catalyst, because the catalytic activity is low, the amount of catalyst required is large, and the conversion rate of raw materials is low ; When sodium tungstate-edetate disodium is used as a catalyst, the catalyst is completely dissolved in the reaction system. Although the catalyst performance is good, it is difficult to recover the catalyst after the reaction, and the wastewater after the reaction contains a large amount of tungsten metal ions , wastewater treatment is difficult, environmental protection pressure is high
In addition, when magnesium hydroxide or sodium tungstate-ethylenediaminetetraacetic acid disodium is used as a catalyst, the raw hydrogen peroxide itself will decompose in large quantities to generate oxygen and water, resulting in a low effective utilization rate of hydrogen peroxide and an increase in production costs

Method used

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  • Catalyst, preparation method thereof and use thereof in production of nitroxide radical piperidinols

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preparation example Construction

[0023] The preparation method of catalyst of the present invention comprises the following steps:

[0024] 1. Provide a mixed solution of tetraethyl silicate and water

[0025] The mass ratio of tetraethyl silicate and water in the mixed solution of tetraethyl silicate and water of the present invention is between 0.05~0.5, preferably between 0.08~0.46, more preferably between 0.12~0.42, preferably between Between 0.16 and 0.38, preferably between 0.20 and 0.32, preferably between 0.25 and 0.28.

[0026] The method of the present invention includes the step of adjusting the pH value of the mixed solution of tetraethyl silicate and water to 10.0-12.0, preferably to 10.5-11.5. The base used to adjust the pH is not particularly limited, and may be a conventional base known in the art, such as alkali metal hydroxide, ammonia water, organic base and the like. Ammonia is preferably used.

[0027] The method of the present invention also includes the step of stirring the mixed sol...

Embodiment 1

[0047] 1. Synthesis of catalyst:

[0048] Dissolve 20.833 grams of tetraethyl silicate in 100 grams of water at 25°C, then add dropwise 25% ammonia water to a pH value of 11.0, then stir at room temperature for 4 hours, tetraethyl silicate slowly hydrolyzes, and the solution Gradually turns milky white. Mix 0.534 grams of tetraethyl titanate and 5.34 grams of absolute ethanol evenly, and then slowly add it dropwise into the solution containing silicon dioxide, control the temperature during the dropwise addition at 20-30°C, and continue stirring for 4 hours after the dropwise addition is completed , and then the slurry was filtered, washed three times with 100ml of distilled water, dried at 120°C for 12 hours, and then calcined at 500°C for 4 hours to obtain a titanium-containing solid catalyst. The element composition of the solid catalyst was analyzed by an inductively coupled atomic emission spectrometer (ICP-AES). The content of titanium in the solid catalyst was 2% by we...

Embodiment 2

[0056] Add 157 grams of 2,2,6,6-tetramethyl-4-hydroxypiperidine, 121.5 grams of 28% hydrogen peroxide in a 2L three-necked flask as raw material, 1.57 grams of titanium-containing solid catalyst (same as Example 1), to 786 grams of water was used as a solvent, the reaction temperature was 80° C., and the reaction time was 3 hours. After the reaction, the catalyst was filtered out, all the solvent was evaporated, and the remaining organic phase was cooled, crystallized, and filtered to obtain 2,2,6,6-tetramethyl-4-hydroxypiperidine nitroxide free radical, which was obtained by Gas chromatography quantitative analysis showed that the product weight was 132.6 grams, the product yield was 84.3%, and the hydrogen peroxide effective utilization rate was 84.3%.

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Abstract

The invention discloses a catalyst, a preparation method thereof and use thereof in production of nitroxide radical piperidinols The catalyst for synthesizing nitroxide free radical piperidinol comprises, by total weight of the catalyst, 0.1-5.0% of a titanium element, 30-48% of a silicon element and the balance of an oxygen element. The catalyst is prepared by the following method: providing a mixed solution of tetraethyl silicate and water, wherein the mass ratio of tetraethyl silicate to water being 0.05-0.5; adjusting the pH value of the solution to 10.0-12.0, and stirring the solution; providing a mixed solution of tetraethyl titanate and absolute ethyl alcohol, wherein the mass ratio of tetraethyl titanate to absolute ethyl alcohol is 0.02-0.5; and mixing the two mixed solutions, and carrying out stirring and roasting to obtain a catalyst product.

Description

technical field [0001] The invention relates to a titanium-containing solid catalyst, a preparation method of the catalyst and its use in the preparation of nitroxide radical piperidinol (that is, 2,2,6,6-tetramethyl-4-hydroxypiperidine nitroxide radical) use in . Background technique [0002] 2,2,6,6-Tetramethyl-4-hydroxypiperidine nitroxide radical (also known as nitroxide radical piperidinol or inhibitor 701) is a new type of polymerization inhibitor, which is a stable It is extremely stable to light and heat, can terminate the oxidation chain, and can be used as a polymerization inhibitor for polymer monomers, an anti-aging agent for polymer materials, a high-efficiency ultraviolet light absorber, and thermal degradation of polyformyl and polyvinylamine Inhibitors. Due to the excellent polymerization inhibition performance of 2,2,6,6-tetramethyl-4-hydroxypiperidine nitroxide free radicals on unsaturated compounds, it can be applied to prevent polymerization fouling of ...

Claims

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Application Information

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IPC IPC(8): B01J21/06B01J21/08C07D211/94
CPCB01J21/063B01J21/08C07D211/94
Inventor 熊德胜罗从光庄岩崔曜褚小东
Owner SHANGHAI HUAYI NEW MATERIAL
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