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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 the health of production operators
Secondly, the particle size of the currently produced resin is mostly in the range of 400-2000 μm, and it needs to be pulverized to reach the particle size required by the preparation carrier, and the pulverization will partially destroy the structure of the resin and produce a new surface, which is not conducive to the stability of the preparation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 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 weight concentration of 2% NaOH solution, about 100g each time, wash with water until neutral, To obtain refined styrene and divinylbenzene, add 1.2g of BPO and stir to dissolve.

[0023] Add 500g of water and 5g of PVA into a 1L three-necked reaction flask, start stirring, and after the PVA swells, heat to 50±2°C to completely dissolve the PVA, then add 5mg of methylene blue to completely dissolve it. Then add the above-mentioned refined styrene and divinylbenzene dissolved in BPO, and adjust the stirring speed so that the emulsion droplet size is 100 μm. Heat up to 80±2°C and keep for 3 hours, then raise to 90±2°C and keep for 2 hours, then raise to 95°C and keep 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. to remove th...

Embodiment 2

[0031] Get 100g styrene (99.4wt%) and 5.5g divinylbenzene (80.2wt%) and put in the separating funnel, refine with the same method in Example 1, get refined styrene and divinylbenzene, add 0.5g of BPO was stirred to dissolve.

[0032] Add 300g of pure water and 3g of PVA into a 1L three-necked reaction flask, and 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 it. Then add the above-mentioned refined styrene and divinylbenzene, and adjust the stirring speed so that the average particle size of the milk droplets is 50 μm. Slowly heat up to 80±2°C and keep for 2 hours, then raise the temperature to 90±2°C and keep for 3 hours, then raise the temperature to 95°C and keep 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., and filtered with a Buchner funnel to co...

Embodiment 3

[0039] Get 100g styrene (99.4wt%) and 25g divinylbenzene (80.2wt%) and put in the separating funnel, refine with the same method in Example 1, get refined styrene and divinylbenzene, add 2.5 After stirring and dissolving g BPO, set aside.

[0040] Add 500g of pure water and 5g of PVA into a 1L three-necked reaction flask, start stirring, and after the PVA swells, heat to 50±2°C to completely dissolve the PVA, then add 5mg of methylene blue to completely dissolve it. Then add the above-mentioned refined styrene and divinylbenzene (dissolved with BPO), and adjust the stirring speed so that the average particle size of the milk droplets is 120 μm. Heat up to 80±2°C and keep for 3 hours, then raise to 90±2°C and keep for 2 hours, then raise to 95°C and keep 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, rinsed with hot water at 85° C., and filtered through a Buchner funnel to contr...

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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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