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A kind of preparation method of p-chlorobenzaldehyde

A technology of p-chlorobenzaldehyde and p-chlorotoluene, which is applied in the preparation of hydrocarbon ammoxidation, nitrile reduction and hydrolysis preparation, organic chemistry, etc., can solve the problems of complicated operation, high cost, and high cost, and achieve simple process operation and equipment The effect of low requirements and low comprehensive investment

Active Publication Date: 2022-04-26
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrolysis process will also use metal salt catalysts, which will generate a large amount of waste water, etc., and metal salt catalysts are difficult to recycle, so the cost is high and the environment is polluted.
[0006] The above-mentioned preparation method is not suitable for large-scale application and production, and has problems such as complicated operation, high cost, and poor safety and sanitation conditions, which affect economic benefits and need further improvement

Method used

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  • A kind of preparation method of p-chlorobenzaldehyde
  • A kind of preparation method of p-chlorobenzaldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Oxidation reaction: Take a fixed bed reactor and fill it with an ammonia oxidation catalyst V 2 o 5 After the volume is 25ml, heat up to 350°C, use nitrogen gas to purge at a gas velocity of 200sccm for 1h, then pass in hydrogen gas to purge at a gas velocity of 100sccm for 1h, and then pass in ammonia gas to purge at a gas velocity of 50sccm for 0.5h to activate the ammonia oxidation catalyst V 2 o 5 , after the temperature is stabilized, feed the mixed gas of ammonia gas and oxygen molar ratio 1:1.6, ammonia gas and p-chlorotoluene molar ratio 1:1.2 to the fixed bed reactor for 10min, take 20g p-chlorotoluene and use the feed pump to Airspeed 1.2h -1 0.5 g / min of p-chlorotoluene was passed into the reactor, and p-chlorobenzonitrile was collected at the lower end, and the obtained p-chlorobenzonitrile crude product was 21.77 g, and the measured p-chlorobenzonitrile content was 96%. The reaction equation is as follows:

[0018]

[0019] (2) Hydrolysis reactio...

Embodiment 2

[0022] The difference between this implementation method and Example 1 is that the molar ratio of ammonia to oxygen is 1:1.7, the other steps are the same, and a total of 20.68g of p-chlorobenzaldehyde is obtained, and the molar yield is 93.12%.

Embodiment 3

[0024] The difference between this implementation method and Example 1 is that the molar ratio of ammonia to oxygen is 1:1.8, the other steps are the same, and a total of 20.28g is obtained, and the molar yield is 91.3%.

[0025] Known from above embodiment 1 / 2 / 3, when the mol ratio of ammonia and oxygen is 1:1.7, the molar yield of p-chlorobenzaldehyde is the highest, so the mol ratio of ammonia and oxygen is preferably 1:1.7.

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Abstract

The invention provides a kind of preparation method of p-chlorobenzaldehyde, fills in the fixed-bed reactor the ammoxidation catalyst V 2 o 5 , after heating up, feed nitrogen and hydrogen to the ammonia oxidation catalyst V 2 o 5 For activation, the ammonia oxidation catalyst V 2 o 5 After the activation is completed, continue to pass in nitrogen for purging, and pass in the mixed gas of ammonia and oxygen, ammonia and p-chlorotoluene in advance. For benzonitrile, add p-chlorobenzonitrile to a high-pressure reaction kettle, add reduction catalyst Raney nickel and formic acid solution, replace the air in the kettle with nitrogen, fill in hydrogen to heat up, and then react with heat preservation and pressure, then cool and filter to obtain the filtrate, which is used toluene After extraction, toluene is recovered under reduced pressure to obtain p-chlorobenzaldehyde. The method has simple process operation, avoids the use of chlorine gas, and does not generate a large amount of hydrogen chloride tail gas, waste water, waste acid and the like. It has low requirements on equipment, small comprehensive investment and fast return, and high conversion rate, which belongs to the field of organic chemical technology.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry and relates to a preparation method of p-chlorobenzaldehyde. Background technique [0002] p-Chlorobenzaldehyde is an important intermediate of new pesticides, medicines and dyes. In medicine, p-chlorobenzaldehyde can be condensed and cyclized with mercaptopropionic acid to prepare fenalu. In terms of pesticides, p-chlorobenzaldehyde is used to synthesize the herbicide Maidi San, the plant growth regulator paclobutrazol and uniconazole, etc. In terms of dyes, p-chlorobenzaldehyde is used to synthesize acid blue 7BF, acid brilliant blue 6B, etc. [0003] At present, the preparation method of p-chlorobenzaldehyde usually adopts the following modes: [0004] Patent CN104557492A introduces that p-chlorotoluene is irradiated with chlorine gas in the presence of an initiator and reacted with chlorine gas. The chlorination temperature is 90-140° C. to obtain a mixture of p-chlorobenz...

Claims

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Application Information

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IPC IPC(8): C07C45/44C07C47/55
CPCC07C45/44C07C253/28C07C47/55C07C255/50
Inventor 程贺于童黄秀泉吴斌赵建伟
Owner SHANDONG GUOBANG PHARMA