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Oxidative carbonylation synthesis process, catalyst for treating oxidative carbonylation synthesis waste liquid, and preparation method of catalyst

A synthesis process and waste liquid treatment technology, applied in the preparation of carbon monoxide or formate reaction, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve problems such as loss of N element, and achieve improved treatment efficiency and low-cost treatment. Effect

Active Publication Date: 2017-07-28
武汉聚川科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In view of the above defects or improvement needs of the prior art, the present invention provides a synthesis process of oxidative carbonylation method, its waste liquid treatment catalyst and its preparation method, the purpose of which is to reduce nitric acid produced by the synthesis reaction to finally generate nitrogen Nitrate esters are used as raw materials for the synthesis of oxidative carbonylation to form a non-destructive cycle of N elements, thus solving the technical problem of the loss of N elements in the existing oxidative carbonylation method

Method used

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  • Oxidative carbonylation synthesis process, catalyst for treating oxidative carbonylation synthesis waste liquid, and preparation method of catalyst
  • Oxidative carbonylation synthesis process, catalyst for treating oxidative carbonylation synthesis waste liquid, and preparation method of catalyst
  • Oxidative carbonylation synthesis process, catalyst for treating oxidative carbonylation synthesis waste liquid, and preparation method of catalyst

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Embodiment 1

[0066] Embodiment 1 oxidative carbonylation method synthetic oxalate

[0067] The catalyst used in this example is activated carbon modified by B. The specific method is to add the activated carbon to the mass ratio of B:AC=1:20 to add boric acid aqueous solution and impregnate it in an equal volume, dry it at 120°C for 2 hours, and then dry it at 500-600°C Roasting in air isolation for 2 hours, cooling in air isolation, immersion and washing with nitric acid aqueous solution etc. for 3 times can obtain the catalyst used in this example.

[0068] The technological process that present embodiment adopts, waste liquid nitric acid treatment is attached figure 2 , the mixed tower is used as the reactor, the upper section of the tower is used as a packing device, and the filler is catalyst particles, which are packed in two sections; the lower section is a tray tower.

[0069] For the process of this embodiment, see figure 2 :

[0070] Synthesis by oxidative carbonylation:

...

Embodiment 2

[0083] Embodiment 2 oxidative carbonylation method synthetic oxalate

[0084] The carbon-based catalyst used in this embodiment is a carbon-adhered material; the carbon-adhered material includes a substrate and a carbon material layer covering the surface of the substrate. The carbon material layer has a porous structure, including 90%-95% carbon powder and 5%-10% tar by mass fraction.

[0085] The matrix is ​​a ceramic filler treated with 5% potassium hydroxide at 100°C for 3-5 hours.

[0086] The carbon-based catalyst is prepared as follows:

[0087] A. Heat the mixture of carbon powder and tar in the formula ratio to 120°C, and stir evenly to form a carbon material dispersion;

[0088] B. Immerse the ceramic filler treated with 5% potassium hydroxide at 100°C for 3 to 5 hours into the above dispersion liquid, take it out after immersion for 0.5 hour and drain it for 2 hours, so that the carbon material is dispersed and evenly attached to the surface of the ceramic filler ...

Embodiment 3

[0105] Embodiment 3 oxidative carbonylation method synthetic oxalate

[0106] The carbon-based catalyst used in this embodiment is a carbon-adhered material, specifically carbon-coated stainless steel wire mesh filler; the carbon-adhered material includes a substrate and a carbon material layer covering the surface of the substrate. The carbon material layer has a porous structure, including 85%-90% carbon powder, 10%-15% tar, and 0.1%-0.3% platinum as an auxiliary agent.

[0107] The matrix is ​​stainless steel wire mesh packing.

[0108] The carbon-based catalyst is prepared as follows:

[0109] A. Heat the mixture of carbon powder and tar in the proportion of the formula to 150°C, and stir evenly to form a carbon material dispersion;

[0110] B. Treat the stainless steel wire mesh with 20% nitric acid solution at 100°C for 1 to 3 minutes, rinse until neutral, then treat it with 3% potassium hydroxide solution at 80°C for 15 minutes, and immerse the treated stainless steel...

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Abstract

The present invention discloses an oxidative carbonylation synthesis process, a catalyst for treating an oxidative carbonylation synthesis process waste liquid, and a preparation method of the catalyst. According to the oxidative carbonylation synthesis process, nitric acid generated in an oxidative carbonylation synthesis reaction is reduced by using nitric oxide as a reducing agent to generate nitrite, and the generated nitrite is re-poured into oxidative carbonylation synthesis so as to form nitrogen lossless cycle. The catalyst is a carbon attaching material, and comprises a matrix and a carbon material layer covering the surface of the matrix, wherein the carbon material layer has a porous structure and comprises 85-95% by mass of a carbon material and 5-15% by mass of a binder, and the matrix is a tower regular filler or random filler. The catalyst of the present invention can greatly improve the nitric acid conversion efficiency.

Description

technical field [0001] The invention belongs to the field of chemistry and chemical engineering, and more specifically relates to an oxidative carbonylation synthesis process, a waste liquid treatment catalyst and a preparation method thereof. Background technique [0002] The chemical waste liquid containing dilute nitric acid and nitrogen monoxide waste gas will be produced in the ester synthesis process of oxidative carbonylation method. Take the industrial synthesis of oxalate ester and carbonate ester as an example: the following reactions occur during the synthesis process: [0003] (1) 2RONO+2CO=ROOCCOOR+2NO [0004] (2) 2RONO+CO=ROOCOR+2NO [0005] Reaction 1 and 2 are the reaction formulas of oxalate and carbonate respectively. The nitric oxide (NO) formed in the reaction must be converted into nitrite to maintain the continuous reaction. During the conversion of NO into nitrite, there are The following reaction occurs: [0006] (3) 4ROH+4NO+O 2 =4RONO+2H 2 o ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J21/18C07C69/36C07C67/36C07C69/96C07C68/00
CPCB01J21/18C07C67/36C07C68/00C07C69/36C07C69/96
Inventor 陶凌云徐艳群
Owner 武汉聚川科技有限公司
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