Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

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
View PDF15 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the reaction temperature is higher, and other by-products will be formed

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Catalyst preparation: Add 100mL of 20% nitric acid to 5g of coconut shell activated carbon, stir with a magnetic stirrer at a temperature of 80°C for 8h, wash with distilled water to reach neutrality, filter and dry. Add 100mL of 30% sulfuric acid, stir at 60°C for 6h, soak for 0.5h, wash until neutral, dry at 120°C, and roast 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 30 g of p-dichlorobenzene into the reactor, heat to 60°C until p-dichlorobenzene completely melts, add 5 g of the above catalyst, and slowly add it dropwise to p-dichlorobenzene Nitric acid, the stirring rate is 600r / min, the reaction temperature is 60°C, and the constant temperature reaction is 0.5h. After the reaction, the yield of 2,5-dichloronitrobenzene is 95%. Basically no waste acid is generated.

Embodiment 2

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

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

Embodiment 3

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

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

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.

Description

technical field [0001] The present invention relates to a method for preparing a catalyst used in the nitration process of organic compounds and a method for synthesizing corresponding nitrated compounds, in particular to the preparation and preparation of a catalyst capable of converting p-dichlorobenzene into 2,5-dichloronitrobenzene resolve resolution. Background technique [0002] 2,5-Dichloronitrobenzene is an important chemical intermediate, mainly used in the production of ice dyes, and also used as a nitrogen fertilizer synergist to increase rice yield. It is one of the species with the lowest toxicity of known nitrogen fertilizer synergists One, 2,5-dichloronitrobenzene is the raw material for the preparation of trichloronew (2,4,4-trichloro-2-hydroxydiphenyl ether). [0003] At present, the domestic production of 2,5-dichloronitrobenzene mainly adopts a batch production process, that is, sulfuric acid is used as the base acid, p-dichlorobenzene is added, the tempe...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): B01J27/02B01J27/24B01J29/08B01J31/02B01J37/02C07C201/08C07C205/12
CPCB01J27/02B01J27/24B01J29/084B01J31/0225B01J37/0207C07C201/08C07C205/12
Inventor 刘卓王晓宁陈永乐张伟黄伟金汉强吴其建陈永平
Owner CHINA PETROLEUM & CHEM CORP
Features
  • Generate Ideas
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com