Method for preparing polystyrolsulfon acid aqueous solution through sodium p-styrenesulfonate polymerization

A technology of sodium styrene sulfonate and polystyrene sulfonic acid is applied in the field of preparing polystyrene sulfonic acid aqueous solution from an aqueous solution of sodium polystyrene sulfonate, and can solve the problem of limited production area, many process control points and low product sulfonation degree. And other issues

Inactive Publication Date: 2014-07-09
唐山德方化学有限公司 +2
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0006] Sulfur trioxide sulfonation method (Guo Ge et al. "New process for the synthesis of polystyrene sulfonic acid by sulfur trioxide low-temperature sulfonation method" "Spectrum Laboratory" volume 28, No. 4, page 1849, July 2011) has solved the problem of side effects A large amount of waste acid is produced, but the conversion rate of sulfur trioxide is 89%, the sulfonation rate is 92%, and sulfur trioxide is not easy to transport, and the production area is limited
[0007] To sum up, due to the complexity of the polystyrene sulfonation reaction, especially the high molecular weight polystyrene sulfonation is more difficult, resulting in a low degree of sulfonation of the product; at the same time, the polystyrene sulfonation reaction involves many solvents, catalysts, sulfonating agents, etc. Such substances lead to many side reactions and by-products, resulting in difficulty in product separation and purification and unstable color; furthermore, due to many process control points, long process and difficult handling of by-products, the actual production has a great impact on the environment and high production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Preparation of initiator: Accurately weigh 5.7g of sodium persulfate and dissolve it in 100ml of deionized water, stir to fully dissolve it for use.

[0030] Feeding and polymerization: Add 20 L of deionized water into a 50 L reactor, then add 4.13 kg of sodium styrene sulfonate, and start the stirring speed at 85 rpm. Under the action of stirring, the temperature of the system was raised to 80° C., and the initiator was started to be added dropwise and completed within 1 hour. Keep the reaction temperature at 80±1°C, and the reaction time is 21 hours.

[0031] Discharging and acidification: After the reaction is completed, the system is cooled to room temperature 25°C under stirring, the discharge valve of the reactor is opened, and the material is discharged into the acidifier with a volume of 100L, and the stirring is started at a stirring speed of 40rpm, and the organic porous skeleton is added Solid acid 10kg, slowly stirred for 2 hours. Then use a 200-mesh polye...

Embodiment 2

[0034] Preparation of initiator: Accurately weigh 15g of sodium persulfate and dissolve it in 100ml of deionized water, stir to fully dissolve it for use.

[0035] Feeding and polymerization: Add 20 L of deionized water into a 50 L reactor, then add 4.13 kg of sodium styrene sulfonate, and start the stirring speed at 85 rpm. Under the action of stirring, the temperature of the system was raised to 80° C., and the initiator was started to be added dropwise and completed within 1 hour. Keep the reaction temperature at 80±1°C, and the reaction time is 8 hours.

[0036] Discharge and acidification: with embodiment 1.

[0037] The weight-average molecular weight of the product measured by polystyrene sulfonic acid standard sample viscosity comparison is 68,000.

Embodiment 3

[0039] Initiator preparation: accurately weigh 6g of azobisisopropylimidazoline and dissolve it in 100g of 1% polystyrene sulfonic acid aqueous solution, stir to fully dissolve it, and set aside.

[0040] Feeding and polymerization: Add 20 L of deionized water into a 50 L reactor, then add 4.13 kg of sodium styrene sulfonate, and start the stirring speed at 85 rpm. Under stirring, the temperature of the system was raised to 65° C., and the initiator was started to be added dropwise and completed within 1 hour. Keep the reaction temperature at 65±1°C, and the reaction time is 8 hours.

[0041] Discharge and acidification: with embodiment 1.

[0042] The weight-average molecular weight of the product measured by polystyrene sulfonic acid standard sample viscosity ratio is 200,000.

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Abstract

The invention provides a method for preparing a polystyrolsulfon acid aqueous solution through sodium p-styrenesulfonate polymerization, and relates to a method which is characterized in that sodium p-styrenesulfonate is used as a raw material for preparing a sodium polystyrenesulfonate aqueous solution, and then the sodium polystyrenesulfonate aqueous solution is used for preparing the polystyrolsulfon acid aqueous solution. The method comprises the following specific steps: preparing the sodium polystyrenesulfonate aqueous solution by using the sodium polystyrenesulfonate as the raw material and water as a reaction medium through polymerization under the effect of an initiating agent, acidizing the sodium polystyrenesulfonate aqueous solution by using organic porous skeleton solid acid, separating and refining, thus obtaining the polystyrolsulfon acid aqueous solution. Compared with a technology which uses sulfonating agents such as sulfuric acid, sulfur trioxide and chlorosulfonic acid for sulfonating polystyrene in organic solvents, the method has the advantages that raw material is single, the technological process is short, the organic solvent with relatively high toxicity is not adopted, lots of dilute acid is not generated, and no waste gases, industrial wastewater and waste resides are generated; and the sulfonation rate of the product is high, the molecular weight is easy to control, and the product purity is high.

Description

technical field [0001] The present invention relates to the preparation method of polystyrene sodium sulfonate and polystyrene sulfonic acid aqueous solution, specifically a kind of preparation method of polystyrene sodium sulfonate aqueous solution using sodium styrene sulfonate as raw material, and then by polystyrene sodium sulfonate aqueous solution Process for preparing an aqueous solution of polystyrene sulfonic acid. Background technique [0002] Polystyrene sulfonic acid (PSSA) is a very important water-soluble template polymer in functional polymer materials, and its aqueous solution is a common raw material in industrial production. PSSA has strong chemical reactivity, high electrical conductivity, and is easy to form a film. It is widely used in polymer luminous bodies, antistatic coatings, fuel cells, and water treatment ultrafiltration membranes. [0003] At present, the domestic PSSA market generally relies on imported solid products, which are configured into...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F112/14C08F8/36
Inventor 杨喜龙王淑莉杨伯涵
Owner 唐山德方化学有限公司
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