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Preparation method of catalysts for dichloro-pyridine oxynitride

A technology of dichloropyridine nitrogen oxide and catalyst is applied in the field of preparation of dichloropyridine nitrogen oxide catalyst, and achieves the effects of good selectivity and high catalytic activity

Active Publication Date: 2014-09-10
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For the catalytic oxidation catalyst of 2-chloropyridine nitrogen oxide, the use of titanium silicon as a catalyst is currently limited to micron or nanometer powder catalysts. For the shaped catalyst of 2-chloropyridine nitrogen oxide, it is used in fixed-bed reactors. , there is no report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 80kg of pure water and pour it into a 200L autoclave, add 25.3kg of tetrapropylammonium bromide under stirring, after mixing for 10 minutes, add 40.8kg of n-butylamine, 1.2kg of sodium hydroxide, stir and mix, and cool down at the same time. When the temperature is below 40°C, add 3.1kg of tetrabutyl titanate, stir to dissolve evenly, then add 73.5kg of silica sol, stir for another 30min, and heat up to 140-200°C for crystallization for 3-50h. The synthesized titanium-silicon molecular sieve is exchanged, washed, dried, and finally calcined at 400-1000° C. for 3-20 hours. About 20kg of titanium-silicon molecular sieve raw powder was obtained, the relative crystallinity was 96%, the silicon-aluminum ratio was 36, and the residual sodium was 0.05%.

[0021] Weigh 10kg of titanium-silicon molecular sieve raw powder, 0.3kg of squash powder, add 0.5kg of o-toluidine, add 2.3kg of pure water, knead in a small kneader at room temperature, knead evenly and extrude the dia...

Embodiment 2

[0023] Weigh 80kg of pure water and pour it into a 200L autoclave, add 25.3kg of tetrapropylammonium bromide under stirring, and after mixing for 10 minutes, add 40.8kg of n-butylamine and 1.2kg of sodium hydroxide, stir and mix, and cool down at the same time. When the temperature is below 35°C, add 3.1kg of tetraisopropyl titanate, stir to dissolve evenly, then add 73.5kg of silica sol, stir for 30min, and heat up to 140-200°C for 3-50h of crystallization. The synthesized titanium-silicon molecular sieve is exchanged, washed, dried, and finally calcined at 400-1000° C. for 3-20 hours. About 20kg of titanium-silicon molecular sieve raw powder was obtained, the relative crystallinity was 97%, the silicon-aluminum ratio was 32, and the residual sodium was 0.03%.

[0024] Weigh 10kg of titanium-silicon molecular sieve raw powder, 0.3kg of squash powder, add 0.5kg of o-toluidine, add 2.3kg of pure water, knead in a small kneader at room temperature, knead evenly and extrude the d...

Embodiment 3

[0026]Weigh 80kg of pure water and pour it into a 200L autoclave, add 25.3kg of tetrapropylammonium bromide under stirring, and after mixing for 10 minutes, add 40.8kg of n-butylamine and 1.2kg of sodium hydroxide, stir and mix, and cool down at the same time. When the temperature is below 35°C, add 3.1kg of tetraisobutyl titanate, stir to dissolve evenly, then add 73.5kg of silica sol, stir for another 30min, and heat up to 140-200°C for 3-50h of crystallization. The synthesized titanium-silicon molecular sieve is exchanged, washed, dried, and finally calcined at 400-1000° C. for 3-20 hours. About 20.5kg of titanium-silicon molecular sieve raw powder was obtained, the relative crystallinity was 94%, the silicon-aluminum ratio was 35, and the residual sodium was 0.06%.

[0027] Weigh 10kg of titanium-silicon molecular sieve raw powder, 0.3kg of squash powder, add 0.5kg of o-toluidine, add 2.3kg of pure water, knead in a small kneader at room temperature, knead evenly and extru...

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Abstract

The invention discloses a preparation method of catalysts for dichloro-pyridine oxynitride. The method comprises the steps that silicon sol is taken as a silicon source; alkyl titanium is taken as a titanium source; raw titanium silicon molecular sieve powder is synthesized under the condition of a tetrapropylammonium bromide template agent and mixed alkalis; the raw powder is taken as a raw material; sesbania powder is used as a bonding agent; amine and amine salt are taken as a pore-enlarging agent; the striped, spherical and sheeted catalysts are formed by kneading at the room temperature; and catalyst products are obtained by high-temperature roasting, and can be used for fixed-bed reactors directly. The catalysts are evaluated by small-size fixed-bed reactors; a transformation rate of dichloro-pyridine reaches above 90%; and the product selectivity reaches 88.3%.

Description

technical field [0001] The invention relates to a preparation method of a catalyst in the chemical industry field, in particular to a preparation method of a dichloropyridine nitrogen oxide catalyst, and the catalyst is suitable for catalytic oxidation reaction technology of a hydrocarbon compound fixed-bed reactor. Background technique [0002] Titanium silicon (TS-1) molecular sieve is an effective catalyst for some catalytic oxidation reactions, especially in the oxidation reactions of aromatic hydrocarbons, alcohols and olefins. In general, the smaller the particle size of the molecular sieve, the higher the catalyst activity and the better the selectivity. At present, the catalyst used for 2-chloropyridine nitrogen oxide is nano TS-1 catalyst, and the maximum particle size is less than 0.5 μm. Due to the small particle size of the nanometer TS-1 catalyst, there are problems such as the difficulty of separating the product from the catalyst during production, such as hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C07D213/89
Inventor 张庆怀邵军文怀有俞伟明谈赟
Owner SHANGHAI NOVEL CHEM TECH
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