Preparation method of sodium polystyrene sulfonate ion exchange resin

A technology of sodium polystyrene sulfonate and ion exchange resin, which is used in cation exchange materials, medical preparations with non-active ingredients, pharmaceutical formulas, etc., can solve the problem of damage to resin structure, adverse preparation stability, environment and production and operator health. Threats and other issues, to achieve the effect of low reaction temperature, less impurities, and less health impact

Active Publication Date: 2010-10-20
SHANGHAI MODERN PHARMA ENG INVESTIGATION CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, at present, the production of sodium polystyrene sulfonate ion exchange resin both at home and abroad requires the use of dichloroethane as a swelling agent to swell polystyrene cross-linked copolymers, followed by sulfonation, and dichloroethane is a pharmaceutical The first class of solvents in the chemical industry poses a greater threat to the environment and

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0021] Example 1

[0022] Take 100g of styrene (99.4wt%) and 18g of divinylbenzene (80.2wt%) in a separatory funnel, extract 2 to 3 times with a 2% NaOH solution by weight, each time about 100g, wash with water until neutral, The refined styrene and divinylbenzene were obtained, and 1.2 g of BPO was added and stirred to dissolve.

[0023] Add 500g of water and 5g of PVA to a 1L three-necked reaction flask, start stirring, after the PVA swells, heat to 50±2°C to completely dissolve the PVA, and then add 5mg of methylene blue to completely dissolve. Then, the above-mentioned refined styrene and divinylbenzene dissolved in BPO are added, and the stirring speed is adjusted so that the particle size of the emulsion droplets is 100 μm. Heat to 80±2°C and keep it for 3 hours, then to 90±2°C and keep it for 2 hours, and then to 95°C and keep it for 2 hours. Stop heating and continue stirring until the temperature drops to about 40°C. The obtained resin was filtered with a Buchner funnel...

Example Embodiment

[0030] Example 2

[0031] Take 100g of styrene (99.4wt%) and 5.5g of divinylbenzene (80.2wt%) in a separatory funnel, and use the same method in Example 1 for purification to obtain refined styrene and divinylbenzene. 0.5g BPO is stirred and dissolved.

[0032] Add 300g of pure water and 3g of PVA to a 1L three-necked reaction flask, start stirring, after the PVA is swelled, heat to 50±2℃ to completely dissolve the PVA, and then add 5mg of methylene blue to completely dissolve. Then, the above-mentioned refined styrene and divinylbenzene were added, and the stirring speed was adjusted so that the average particle size of the emulsion droplets was 50 μm. Slowly heat the temperature to 80±2°C and keep it for 2 hours, then the temperature to 90±2°C and keep it for 3 hours, and then the temperature to 95°C and keep it for 2 hours. Stop heating and continue stirring until the temperature drops to about 40°C. The obtained resin is filtered with a Buchner funnel, rinsed with hot water ...

Example Embodiment

[0038] Example 3

[0039] Take 100g of styrene (99.4wt%) and 25g of divinylbenzene (80.2wt%) in a separatory funnel, and use the same method in Example 1 for purification to obtain refined styrene and divinylbenzene, add 2.5 g BPO is stirred and dissolved, and then set aside.

[0040] Add 500g of pure water and 5g of PVA to a 1L three-necked reaction flask, start stirring, after the PVA swells, heat to 50±2°C to completely dissolve the PVA, and then add 5mg of methylene blue to completely dissolve. Then, the above-mentioned refined styrene and divinylbenzene (with BPO dissolved) are added, and the stirring speed is adjusted so that the average particle size of the emulsion droplets is 120 μm. Heat to 80±2°C and keep it for 3 hours, then to 90±2°C and keep it for 2 hours, and then to 95°C and keep it for 2 hours. Stop heating and continue stirring until the temperature drops to about 40°C. The obtained resin is filtered with a Buchner funnel, rinsed with hot water at 85°C, filter...

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PUM

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Abstract

The invention provides a preparation method of a sodium polystyrene sulfonate ion exchange resin, which comprises the following steps: (1) taking styrene as a monomer, divinylbenzene as a cross-linking agent, benzoyl peroxide as an initiator, polyvinyl alcohol as a suspending agent, methylene blue as an aqueous phase polymerization inhibitor and water as a reaction medium, and carrying out suspension polymerization reaction at 78-97 DEG C; and (2) adding copolymer in the step (1) in chloroform for swelling, adding sulfuric acid at 60-95 DEG C for sulfonation reaction to obtain a sulfonate hydrogen type resin, reacting the sulfonated hydrogen type resin and NaOH to convert into sodium type, then purifying and drying to obtain the spherical sodium polystyrene sulfonate ion exchange resin. The invention adopts chloroform to replace the traditional dichloroethane as a sweller, and has less damage to human health and environment and obviously lowered temperature of sulfonation reaction, and the prepared pharmaceutical bead ion exchange resin has small grain diameter, light color, high purity and less impurities and conforms to the requirements of United States and European pharmacopeia.

Description

[0001] Technical field [0002] The invention relates to a preparation method of polystyrene sodium sulfonate ion exchange resin. technical background [0003] Sodium polystyrene sulfonate ion exchange resin has been widely used in various fields such as water purification, separation and purification of compounds, and pharmaceutical preparations. Among them, as an auxiliary material for oral sustained and controlled release suspensions, sodium polystyrene sulfonate ion exchange resin has been provided as an auxiliary material for pharmaceutical specifications abroad, such as Rohm & Haas and Dow Chemical. Both produce pharmaceutical grade resins. [0004] However, the current production of sodium polystyrene sulfonate ion exchange resin at home and abroad requires the use of ethylene dichloride as a swelling agent to swell polystyrene cross-linked copolymers, followed by sulfonation, and ethylene dichloride is a pharmaceutical The first class of solvents in the solvent poses...

Claims

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Application Information

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IPC IPC(8): C08F212/08C08F2/20C08F8/44C08F8/36B01J39/20A61K47/32
Inventor 侯惠民王健傅民邹凌燕陈芳夏怡然
Owner SHANGHAI MODERN PHARMA ENG INVESTIGATION CENT
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