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A kind of preparation method of 2-acrylamido-2-methylpropanesulfonic acid

A technology of methylpropanesulfonic acid and acrylamide, which is applied in the field of preparation of 2-acrylamido-2-methylpropanesulfonic acid, which can solve the problems of large refining and purification losses, multiple by-product impurities, and poor product quality. , to achieve the effect of less solvent residue, high dissolution clarity and low product loss

Active Publication Date: 2022-06-03
WEIFANG QUANXIN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many by-products will be produced in the synthesis of 2-acrylamido-2-methylpropanesulfonic acid, and the purity is not high, so it can only be used in industries with low requirements such as water treatment agents
[0007] On the whole, the 2-acrylamido-2-methylpropanesulfonic acid prepared by the prior art has poor product quality and low purity. It not only contains more by-product impurities, but also has a large amount of black after dissolution. Or white small particle impurities, which cannot meet the requirements of special industries such as medicine and cosmetics
Second, the refining and purification loss is large, the yield is low, and it is uneconomical

Method used

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  • A kind of preparation method of 2-acrylamido-2-methylpropanesulfonic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of crude 2-acrylamido-2-methylpropanesulfonic acid:

[0032] The raw material acrylonitrile and nicotinic acid are mixed at low temperature, and then isobutylene is introduced to obtain a slurry, which is filtered and dried to obtain a crude 2-acrylamido-2-methylpropanesulfonic acid with a liquid phase purity of 97.1%.

[0033] (1) Add 200g of crude 2-acrylamido-2-methylpropanesulfonic acid and 0.0152g of p-hydroxyanisole to a mixed solution of 128g of purified water and 32g of ethanol at room temperature, and stir to dissolve;

[0034] (2) Add 3.6g of activated carbon. After stirring for 30 min, it was filtered.

[0035] (3) Control the temperature to 15°C, the stirring speed is 200 rpm, and add acetone dropwise to the filtrate. After a period of time, the solution becomes turbid, and the speed is adjusted to 180 rpm;

[0036] Continue to drip at a slow and uniform speed for 2h, and add 1800g of acetone dropwise;

[0037] After 1 h, the temperature was l...

Embodiment 2

[0039] Preparation of crude 2-acrylamido-2-methylpropanesulfonic acid:

[0040] The raw material acrylonitrile and nicotinic acid are mixed at low temperature, and then isobutylene is introduced to obtain a slurry, which is filtered and dried to obtain a crude 2-acrylamido-2-methylpropanesulfonic acid with a liquid phase purity of 97.1%.

[0041] (1) At room temperature, add 200g of crude 2-acrylamido-2-methylpropanesulfonic acid and 0.02g of p-hydroxyanisole to a mixed solution of 140g of purified water and 60g of ethanol, and stir to dissolve;

[0042] (2) Add 5g of activated carbon. After stirring for 30 min, it was filtered.

[0043] (3) Control the temperature to 18°C, the stirring speed is 200 rpm, and add acetone dropwise to the filtrate. After a period of time, the solution appears turbid, and the speed is adjusted to 180 rpm;

[0044] Continue to drip at a slow and uniform speed for 2.5h, and add 2000g of acetone dropwise;

[0045] After 1 h, the temperature was lo...

Embodiment 3

[0047] Preparation of crude 2-acrylamido-2-methylpropanesulfonic acid:

[0048] The raw material acrylonitrile and nicotinic acid are mixed at low temperature, and then isobutylene is introduced to obtain a slurry, which is filtered and dried to obtain a crude 2-acrylamido-2-methylpropanesulfonic acid with a liquid phase purity of 97.1%.

[0049] (1) At room temperature, add 200g of crude 2-acrylamido-2-methylpropanesulfonic acid and 0.012g of p-hydroxyanisole to a mixed solution of 135g of purified water and 45g of ethanol, and stir to dissolve;

[0050] (2) Add 4g of activated carbon. After stirring for 30 min, it was filtered.

[0051] (3) Control the temperature to 13°C, the stirring speed is 200 rpm, and add acetone dropwise to the filtrate. After a period of time, the solution becomes turbid, and the speed is adjusted to 180 rpm;

[0052] Continue to drip at a slow and uniform speed for 2.5h, and add 2280g of acetone dropwise;

[0053] After 1 h, the temperature was l...

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Abstract

The invention discloses a preparation method of 2-acrylamido-2-methylpropanesulfonic acid, comprising the following steps: (1) synthesizing a crude product of 2-acrylamido-2-methylpropanesulfonic acid, at normal temperature, Dissolved in a water-based mixed solvent, the weight of the 2-acrylamido-2-methylpropanesulfonic acid crude product and the mixed solvent is 1:0.8-1; (2) Add the total amount of 1‑2% activated carbon, stirred for 30min, and filtered. (3) Add the dissolving agent dropwise to the above filtrate, and control the temperature at 0-50°C. When the solution becomes turbid and crystals are precipitated, reduce the stirring frequency and continue to drop the dissolving agent slowly and uniformly for 2-3 hours. After the dropwise addition is completed, keep warm for 1 hour, cool down to below 10°C, centrifuge, wash, and dry to obtain 2‑acrylamido‑2‑methylpropanesulfonic acid product. The product loss of the invention is small, the yield is high, and the obtained product has high quality. The application range is wider and can meet the needs of some special industries.

Description

technical field [0001] The invention relates to the technical field of production of chemical products, in particular to a preparation method of 2-acrylamido-2-methylpropanesulfonic acid. Background technique [0002] 2-Acrylamido-2-methylpropanesulfonic acid (AMPS) molecule has carbon-carbon double bond, carboxyl group and sulfonic acid group, which endow it with excellent and unique properties. The carbon-carbon double bond can homopolymerize and copolymerize the molecule itself or with other molecules to form a high polymer; the carboxyl group makes the molecule have excellent adsorption and complexation; the sulfonic acid group makes the molecule have excellent water solubility and salt resistance, And it has excellent stability; its application in some fields has become an irreplaceable monomer and polymer. Widely used in oil field chemistry, water treatment agent, chemical fiber, plastic, printing and dyeing, coating, surfactant, antistatic agent, ceramics and other f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/44C07C309/15
CPCC07C303/44C07C309/15Y02P20/10
Inventor 张坤树林普文李志军蒋华锋
Owner WEIFANG QUANXIN CHEM