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Synthesis process for 2-acrylamido-2-methyl propane sulfonic acid through continuous method

A technology based on methylpropanesulfonic acid and acrylamide, which is applied in the preparation of sulfonic acid, organic chemistry, etc., can solve the problems of insufficient yield and purity of synthetic products, cumbersome process operations, poor quality stability, etc., and improve product yield. The effect of high efficiency and quality stability, avoiding manual operation, and strong reaction stability

Inactive Publication Date: 2012-02-15
WEIFANG QUANXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this process is produced by batch method, and the reaction temperature and conditions of each step are different, which requires cumbersome process operations, high labor intensity, complicated control, low yield of products, and poor quality stability.
[0006] In recent years, the patent US6448347 (2002) of Robert E. Quinn et al., and the patent US6504050 (2003) of Barve et al. all mentioned the process of continuous synthesis of 2-acrylamido-2-methylpropanesulfonic acid, and Lunhong Kawakami The patent 03-077859 (1991) also proposed a similar process, but due to its limitations in the design of the process and the way of adding raw materials, the synthetic product did not achieve a relatively ideal yield and purity

Method used

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  • Synthesis process for 2-acrylamido-2-methyl propane sulfonic acid through continuous method
  • Synthesis process for 2-acrylamido-2-methyl propane sulfonic acid through continuous method

Examples

Experimental program
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Effect test

Embodiment 1

[0018] The acrylonitrile with water content of 0.2% is added into the four-mouth glass container with stirring device through the flow meter by the metering pump at a flow rate of 420g / h, and simultaneously oleum, wherein free SO 3 The content is 3%, and the metering pump is added to the same container through the flow meter at a flow rate of 76g / h for mixing. The temperature in the mixing container is controlled by an ice-water bath to be 11±1°C, and the mixed liquid flows into the belt through the overflow port in the middle of the mixer. In the primary reactor with stirring paddle, at the same time, isobutene with a purity of 99.76% was vaporized and added to the primary reactor at a flow rate of 32 g / h. The overflow port in the middle of the first-stage reactor flows into the second-stage reactor with stirring paddle, and at the same time, isobutene with a purity of 99.76% is vaporized and added to the second-stage reactor at a flow rate of 16 g / h, and the reactor is contro...

Embodiment 2

[0021] The acrylonitrile with water content of 0.2% is added into the four-mouth glass container with stirring device through the flow meter by the metering pump at a flow rate of 420g / h, and simultaneously oleum, wherein free SO 3 The content is 2.0%, and it is added to the same container by a metering pump at a flow rate of 76 g / h through a flowmeter for mixing, and the temperature in the mixing container is controlled by an ice-water bath to 11±1 °C. The mixed solution flows into the primary reactor with a stirring paddle through the overflow port in the middle of the mixer, and at the same time, isobutene with a purity of 99.8% is vaporized and added to the primary reactor at a flow rate of 32 g / h, and the reactor is controlled by a water bath The internal temperature is 39±1°C. The mixed liquid flows into the secondary reactor with a stirring paddle through the overflow port in the middle of the primary reactor, and at the same time, isobutene with a purity of 99.8% is va...

Embodiment 3

[0024] Add acrylonitrile with a water content of 0.2% into a four-port glass container with a stirring device through a flow meter at a flow rate of 378g / h by a metering pump, and simultaneously fuming sulfuric acid, wherein free SO 3 The content is 3%, and it is added to the same container by a metering pump at a flow rate of 68.4 g / h through a flowmeter for mixing, and the temperature in the mixing container is controlled by an ice-water bath to 11±1 °C. The mixed liquid flows into the primary reactor with stirring paddle through the overflow port in the middle of the mixer. At the same time, isobutene with a purity of 99.78% is vaporized and then added to the primary reactor at a flow rate of 28.8g / h. The reactor is controlled by a water bath The internal temperature is 39±1°C. The mixed liquid flows into the secondary reactor with a stirring paddle through the overflow port in the middle of the primary reactor, and at the same time, isobutene with a purity of 99.78% is vap...

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Abstract

The invention discloses a synthesis process for 2-acrylamido-2-methyl propane sulfonic acid through a continuous method. The synthesis process comprises the following steps of: continuously and uniformly mixing acrylonitrile and fuming sulfuric acid at the temperature of 10-12 DEG C; performing first order reaction and second order reaction at the temperature of 20-45 DEG C under a condition of introducing vaporized isobutene; and slaking, centrifuging and drying to continuously produce the 2-acrylamido-2-methyl propane sulfonic acid product. By designing unique first order reaction, second order reaction and slaking flow, completeness degree of reaction of the material is guaranteed, the product yield and the quality stability are improved, and the reaction period is greatly shortened. The synthesis process has the advantages of scientific and rational flow design, practicability, product yield of over 96 percent and liquid phase detection purity of over 96 percent.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis technology, in particular to the synthesis technology of 2-acrylamido-2-methylpropanesulfonic acid. Background technique [0002] 2-Acrylamido-2-Methyl Propane Sulfonic Acid (AMPS) is an acrylamide-based anionic monomer. It is a white crystalline solid with a melting point of 185°C (decomposition). Its structural formula is: [0003] [0004] It can be seen from its structure that it contains strong anionic, water-soluble sulfonic acid groups, shielded amide groups and unsaturated double bonds, which make it have excellent performance. The sulfonic acid group makes it have dyeing affinity, conductivity, ion exchange and good tolerance to divalent cations; the amide group makes it have good hydrolytic stability, acid resistance, alkali resistance and heat resistance Stability; and the active double bond makes it have addition and polymerization properties. Therefore, 2-acrylamido-2...

Claims

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Application Information

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IPC IPC(8): C07C309/15C07C303/02
Inventor 隋奎江李志军
Owner WEIFANG QUANXIN CHEM
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