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Method for synthesizing allylamine using transfer line reactor

A pipeline reactor and allylamine technology, which is applied in the preparation of amino-substituted functional groups, organic chemistry, etc., can solve the problems of high raw material costs, serious pollution emissions, etc., and achieve good safety effects

Inactive Publication Date: 2007-05-16
杭州新成化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are also reports in the literature that it is produced through the hydrolysis reaction of diallylamine and sulfuric acid. This method has a high yield and can reach 88%, but the cost of raw materials is high and the pollution discharge is serious.

Method used

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  • Method for synthesizing allylamine using transfer line reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: A kind of method utilizing pipeline reactor to prepare allylamines, reaction process is as follows:

[0028]Take allyl chloride 1000g (13.1mol), catalyst 25g, solvent methanol 2000g, liquid ammonia 4454g (262mol). The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the temperature of the reactor jacket at 90°C, adjust the flow rate, divide the above raw materials into two groups and pour them into the pipeline reactor at the same time, the system pressure is 1.2Mpa, and the reaction residence time is 12 minutes. Sampling and analysis showed that the conversion rate of raw material allyl chloride was 99.9%. Rectify the synthetic liquid, extract 433g of allylamine from the fraction at 52-55°C, extract 241.4g of diallylamine from the fraction at 107-111°C, and obtain 23.9g of triallylamine as a by-product, accounting for 3.4% of the product %.

Embodiment 2

[0029] Embodiment 2: a kind of method utilizing pipeline reactor to prepare allylamines, reaction process is as follows:

[0030] Take 1000g (13.1mol) of allyl chloride, 33g of catalyst, 200g of solvent ethanol, and 3340.5g (196.5mol) of liquid ammonia. The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the reactor jacket temperature at 80°C, adjust the flow rate, divide the above raw materials into two groups and pour them into the pipeline reactor at the same time, the system pressure is 1.0Mpa, and the reaction residence time is 9 minutes. Sampling and analysis showed that the conversion rate of raw material allyl chloride was 99.85%. The synthetic liquid was rectified, and 395.8g of allylamine was obtained by extracting the fraction at 52-55°C, 260.5g of diallylamine was obtained at the fraction of 107-111°C, and 35.9g of triallylamine as a by-product, accounting for 4% of the product 5.1%.

Embodiment 3

[0031] Embodiment 3: a kind of method utilizing pipeline reactor to prepare allylamines, reaction process is as follows:

[0032] Take allyl chloride 1000g (13.1mol), catalyst 45g, solvent 2000g, liquid ammonia 2227g (131mol). The reactor adopts a pipeline reactor, and the feed adopts a metering pump. Keep the temperature of the reactor jacket at 75°C, adjust the flow rate, divide the above raw materials into two groups and pour them into the pipeline reactor at the same time, the system pressure is 0.95Mpa, and the reaction residence time is 10 minutes. Sampling and analysis showed that the conversion rate of raw material allyl chloride was 99.79%. The synthetic liquid was rectified, and 365.8g of allylamine was obtained by mining the fraction at 52-55°C, 273.2g of diallylamine was obtained at the fraction of 107-111°C, and 47.8g of triallylamine as a by-product, accounting for 10% of the product 6.9%.

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Abstract

The invention discloses a preparing method of alkylamine through pipe reactor, which comprises the following steps: adopting allyl chloride as raw material; blending catalyst, solvent and ammonia phase evenly; pumping in the pipe reactor through metering pump according to the rate of materials; ammonifying to produce acrylamide, diallylamine and triallylamine; adding sodium hydroxide solution to remove amino to obtain the product; setting the normal pressure in the reactor system at 3.0Mpa under 40-80Deg C for 5-20min; rectifying the product; evaporating the solvent and surplus ammonia; gathering 52-55Deg C fraction as acrylamide; boiling to remove water; gathering 107-111Deg C fraction as diallylamine.

Description

technical field [0001] The invention relates to a chemical synthesis method, in particular to a method for preparing allylamines using a pipeline reactor. Background technique [0002] Allylamine (alias: 3-aminopropene), used in pharmaceutical intermediates, household chemicals, emulsion modifiers, organic synthesis and resin modifiers, silicon products, etc. It has been reported that polymers that can be polymerized with plasma to generate reverse osmosis wax are used in airtight manned spacecraft; they can also be used as corrosion inhibitors, catalysts and solvents. [0003] Diallylamine (alias: two-2-propenylamine), is a widely used organic synthesis intermediate, organic synthesis raw material, ionic water purifier, polymer monomer, pharmaceutical intermediate and synthetic resin modified body. [0004] Such substances have been reported in the literature, such as Duan Changqiang, Meng Zhuangfang, Zhang Tai, etc. The first volume of mod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/22C07C209/08
Inventor 陈国建南巍冈
Owner 杭州新成化学有限公司
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