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Nitrogen-doped porous carbon catalyst, preparation method of catalyst and preparation method of beta-isophorone

A nitrogen-doped porous carbon and isophorone technology is applied in the preparation of carbon-based compounds, the preparation of organic compounds, organic chemical methods, etc. Realize the effect of circular application, high value-added utilization, and reduction of three wastes

Active Publication Date: 2018-09-28
WANHUA CHEM GRP CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method also faces problems such as many by-products, low space-time yield, and serious equipment corrosion.

Method used

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  • Nitrogen-doped porous carbon catalyst, preparation method of catalyst and preparation method of beta-isophorone
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  • Nitrogen-doped porous carbon catalyst, preparation method of catalyst and preparation method of beta-isophorone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Take 0.50g of coal tar pitch (Shanxi Zhongqiang Coal Chemical Co., Ltd.) to grind and sieve to obtain 150 mesh powder, then mix it with 15.0g of isoquinoline and 20.0g of p-phenylenediamine for ultrasonic treatment, then cool and reflux at 350°C, and air atmosphere ( Under the condition of flow rate of 150mL / g coal tar pitch powder / min), the oxidative crosslinking reaction was carried out, and the reaction time was 3h. After the reaction system dropped to room temperature, the reaction solution was filtered and dried to obtain nitrogen-rich heavy organic matter.

[0062] The resulting nitrogen-rich heavy organic matter was placed in a quartz boat and placed in a tube furnace in a nitrogen atmosphere (flow rate of 250mL / g nitrogen-rich heavy organic matter / min) from room temperature at a rate of 1°C / min. Pre-carbonize at 250°C for 2h; then in a carbon dioxide atmosphere (flow rate of 200mL g nitrogen-rich heavy organic matter / min), continue to heat up to 700°C for 2h at ...

Embodiment 2

[0064] Relevant process parameters are shown in Table 1, the air flow rate is 200mL / g coal tar pitch powder / min, the flow rate of nitrogen, carbon dioxide, and ammonia are respectively 200mL / g nitrogen-rich heavy organic matter / min, and the remaining process parameters refer to Example 1 to prepare nitrogen Doped porous carbon catalysts B, C, D, E, the result analysis is shown in Table 2.

[0065] Table 1 Preparation process parameters of nitrogen-doped porous carbon catalyst

[0066]

[0067] Table 2 Comparison table of structures and properties of nitrogen-doped porous carbon catalysts

[0068]

Embodiment 3

[0086] Add α-isophorone containing 0.5wt% nitrogen-doped porous carbon catalyst A to the still of a plate tower reactor with 30 plates, at 220°C, absolute pressure 0.1MPa, reflux ratio 10:1 The rectification reaction is carried out under certain conditions, and the α-IP isomerization reaction occurs. The reaction results are shown in Table 4.

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Abstract

The invention discloses a nitrogen-doped porous carbon catalyst, a preparation method of the catalyst and a preparation method of beta-isophorone. With coal-tar pitch as a raw material, the novel nitrogen-doped porous carbon catalyst containing L base and B base is prepared through the processes of oxidative crosslinking, pre-carbonization, activation and reactivation. The catalyst is used for preparing 3,5,5-trimethylcyclohex-3-alkene-1-ketone through an isomerization reaction of 3,5,5-trimethylcyclohex-3-alkene-2-ketone. The selectivity of the isomerization reaction reaches 99.6-99.9%. The preparation method has the advantages that the catalyst is easy to recycle, high in conversion rate and selectivity, environmentally friendly, high in space-time yield, capable of causing no corrosionto equipment and the like, and the high-additional-value utilization of coal resources is achieved.

Description

technical field [0001] The present invention relates to an isomerization catalyst, in particular to a nitrogen-doped porous carbon catalyst for preparing β-isophorone from α-isophorone and a preparation method thereof, and using the catalyst to prepare β-isophorone method of preparation. Background technique [0002] 3,5,5-Trimethylcyclohex-3-en-1-one (β-isophorone) is an important intermediate in the synthesis of vitamin E, carotenoids, astaxanthin and various spices, and is The main raw material for the synthesis of 2,6,6-trimethyl-2-cyclohexene-1,4-dione (tea ketone, KIP). [0003] The preparation of β-isophorone mostly uses 3,5,5-trimethylcyclohex-2-en-1-one (α-isophorone) as raw material, and carries out isomerization reaction under the action of catalyst get. α-isophorone and β-isophorone are a pair of isomers, and the formation of β-isophorone involves an equilibrium reaction of deconjugation, so its equilibrium concentration is relatively low, and it is necessary ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/10C07C45/67C07C49/603
CPCC07C45/67B01J27/24C07C2601/16C07B2200/09B01J35/618B01J35/643C07C49/603Y02P20/584
Inventor 宋军伟张涛吕英东郭劲资张旭程晓波王延斌朱龙龙林龙刘英瑞李莉黎源
Owner WANHUA CHEM GRP CO LTD
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