Preparation method of nitration catalyst and application

A nitration catalyst and catalyst technology, which can be used in catalyst activation/preparation, nitro compound preparation, physical/chemical process catalysts, etc., can solve the problem of high reaction temperature, achieve low impurity content, reduce the generation of waste acid, and be easy to separate. Effect

Inactive Publication Date: 2019-12-13

CHINA PETROLEUM & CHEM CORP +1

15 Cites 0 Cited by

AI-Extracted Technical Summary

Problems solved by technology

But the reaction temperature is higher...

Abstract

The invention provides a preparation method of a nitration catalyst. The preparation method comprises the following steps: performing acid pickling on a catalyst carrier, wherein the mass ratio of thecarrier to an acid is (1:0.5)-(1:5), the washing temperature is 20-80 DEG C, and the time is 1-6 hours; performing modification treatment on the pretreated catalyst carrier, wherein the treatment temperature is 20-80 DEG C, the treatment time is 1-6 hours, and the soaking time is 0.5-24 hours; and after modification, performing washing till neutral, performing filtering, and performing drying androasting, wherein the roasting temperature is 200-600 DEGC. By adopting the preparation method provided by the invention, after acid pickling with the catalyst carrier, the impurity content is low; as the catalyst is modified by using a modifier, the content of waste acids can be reduced, thus being environment-friendly; and a reaction product is easy to separate from the catalyst.

Application Domain

Molecular sieve catalystsOrganic-compounds/hydrides/coordination-complexes catalysts +2

Technology Topic

Spent acidTreatment time +4

Examples

Experimental program(7)
Comparison scheme(1)

Example Embodiment

[0019] Example 1

[0020] Catalyst preparation: Add 5g of coconut shell activated carbon to 100mL of 20% nitric acid, stir for 8h with a magnetic stirrer at a temperature of 80℃, wash with distilled water to reach neutrality, filter and dry. After adding 100mL 30% sulfuric acid and stirring at 60°C for 6h, immersing for 0.5h, washing to neutrality, drying at 120°C, and calcining at 500°C for 2h to obtain sulfuric acid-activated carbon 1 catalyst. (20% nitric acid used for washing can be recycled)

[0021] Synthesis of 2,5-dichloronitrobenzene: Add 30g of p-dichlorobenzene into the reactor, heat to 60℃ until p-dichlorobenzene is completely melted, add 5g of the above catalyst, and slowly add dropwise to p-dichlorobenzene Nitric acid, stirring rate 600r/min, reaction temperature 60℃, constant temperature reaction for 0.5h, after reaction, the yield of 2,5-dichloronitrobenzene is 95%. Basically no waste acid is produced.

Example Embodiment

[0022] Example 2

[0023] Catalyst preparation: Add 10g of nutshell activated carbon to 200mL of 25% nitric acid, stir for 0.5h with a magnetic stirrer at a temperature of 30°C, wash with distilled water to reach neutrality, filter and dry. Add 20 g of 20% sulfuric acid solution, stir at 40°C for 6 hours, immerse for 12 hours, wash to neutrality, dry at 120°C, and calcinate at 600°C for 2 hours to obtain p-toluene sulfuric acid-activated carbon 2 catalyst.

[0024] Synthesis of 2,5-dichloronitrobenzene: Add 30g of p-dichlorobenzene into the reactor, heat to 60℃ until p-dichlorobenzene is completely melted, add 5g of the above catalyst, and slowly add dropwise to p-dichlorobenzene Nitric acid, stirring rate 1500r/min, reaction temperature 75℃, constant temperature reaction for 2h, after reaction, the yield of 2,5-dichloronitrobenzene is 91%. Basically no waste acid is produced.

Example Embodiment

[0025] Example 3

[0026] Add 5g of HY molecular sieve to 200mL of 10% hydrochloric acid, stir for 4h with a magnetic stirrer at a temperature of 30℃, wash with distilled water to reach neutrality, filter and dry. Add 20g of 10% hydrochloric acid solution, stir at 10°C for 6h, immerse for 24h, wash to neutrality, dry at 120°C, and calcinate at 400°C for 2h to obtain salt-HY catalyst.

[0027] Synthesis of 2,5-dichloronitrobenzene: Add 30g of p-dichlorobenzene into the reactor, heat to 60℃ until p-dichlorobenzene is completely melted, add 5g of the above catalyst, and slowly add dropwise to p-dichlorobenzene Nitric acid, stirring rate 1200r/min, reaction temperature 80℃, constant temperature reaction for 1h, after reaction, the yield of 2,5-dichloronitrobenzene is 80.5%. Basically no waste acid is produced.

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.

Classification and recommendation of technical efficacy words

low impurity content

Preparation method of nitration catalyst and application

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

Similar technology patents

Method for extracting and purifying beet red pigment from garden beet concentrated juice

Polyvinyl acetate mixed suspended liquid and preparation method and application thereof

Flaxseed oil production technology

High-oxidation-resistance lanthanide nickel base superalloy and preparation method and application thereof

Waste plastic single-screw extrusion granulation equipment and process

Classification and recommendation of technical efficacy words

Method of forming a dielectric layer and method of manufacturing a semiconductor device using the same

Method for preparing gasoline and diesel by oil washing hydrogenation

Stable lenalidomide oral solid preparation

Preparing method for ball-like metal magnetically soft alloy powder

40-thousand-ton hard carbon black reaction furnace and production process of carbon black