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Preparation method of quaternary phosphonium cation starch microspheres

A cationic starch and quaternary phosphonium-type technology, which is applied in the field of preparation of quaternary phosphonium-type cationic starch microspheres, can solve the problems of few reports on the preparation and research of cationic starch microspheres, achieve reduced material costs, strong binding ability, Ease of industrial production

Inactive Publication Date: 2012-07-25
HENAN UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] There are few reports on the preparation and research of cationic starch microspheres

Method used

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  • Preparation method of quaternary phosphonium cation starch microspheres
  • Preparation method of quaternary phosphonium cation starch microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Measure 100 ml of toluene and 40 ml of castor oil, put them in a 250 ml three-necked bottle, add 0.8 g of Span80, heat to 50°C, stir evenly, and form an oil phase. Take another 6 grams of cornstarch, gelatinize with 50 ml of distilled water at 85°C for 30 minutes, and cool to room temperature. Add 1 gram of N,N'-methylenebisacrylamide, 2 grams of acrylamide, 3 grams of allyltrimethylammonium chloride, 1 gram of allyltriphenylphosphonium bromide and 0.1 gram of ammonium persulfate, stirred evenly to obtain the aqueous phase. Slowly add the water phase to the oil phase, control the stirring speed at 600 rpm, take samples every 2 minutes and observe under the microscope. After the liquid beads are evenly dispersed, slowly add a small amount of aqueous solution with 0.02 g of sodium bisulfite dissolved in advance. React for 3 hours. Then, filter, wash with ethyl acetate, and then wash repeatedly with acetone and ethanol. Vacuum drying at 50°C to obtain white powdery star...

Embodiment 2

[0031] Measure 120 ml of cyclohexane, place it in a 250 ml three-necked bottle, add 0.6 g of Span80 and 0.4 g of Tween60, heat to 50° C., stir evenly, and form an oil phase. Another 2.0 g of soluble corn starch was taken, gelatinized with 20 ml of distilled water at 80° C. for 30 minutes, and cooled to room temperature. Add 0.3 g of N,N'-methylenebisacrylamide, 2.0 g of acrylamide, 0.5 g of vinylbenzyltributylphosphonium chloride and 0.03 g of cerium ammonium nitrate to the starch paste under stirring, stir well, and wash with nitric acid Adjust to slightly acidic to obtain an aqueous phase. Slowly add the water phase to the oil phase, take samples every 2 minutes and observe under the microscope. After the liquid droplets are evenly dispersed, raise the temperature to 40°C and react for 4 hours. Then, let it stand, high-speed centrifugation, and separate the upper oil phase. The polymer phase in the lower layer was first cleaned with ethyl acetate, then washed repeatedly wi...

Embodiment 3

[0033]Measure 80 ml of cyclohexane and 20 ml of chloroform, put them in a 250 ml three-necked bottle, add 0.9 g of Span60 and 0.1 g of Tween60, heat to 50 ° C, stir evenly, and form an oil phase. Take another 2 grams of tapioca starch, gelatinize with 30 ml of distilled water at 85°C for 30 minutes, cool to room temperature, continue to add 0.4 g of N,N'-methylenebisacrylamide, 0.6 g of acrylamide, 0.5 g of vinylbenzyl Tributylammonium chloride, 1.5 g of vinylbenzyltributylphosphonium chloride and 0.2 g of sodium persulfate were stirred evenly to obtain an aqueous phase. Slowly add the water phase to the oil phase, control the stirring speed at 1500 rpm, take samples every 2 minutes and observe under the microscope until the liquid droplets are evenly dispersed, and then fill with nitrogen and deoxygenate for 15 minutes. Then the temperature was raised to 65° C., an aqueous solution in which 0.15 g of sodium bisulfite was dissolved in advance was added, and the mixture was rea...

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Abstract

The invention discloses a preparation method of quaternary phosphonium cation starch microspheres. The method comprises the steps that: (1) starch, cation monomers, and acrylamide are weighed; (2) the starch is prepared into a paste by using water; the cation monomers and acrylamide are delivered into the paste; N,N'-methylenebisacrylamide is added to the mixture; an oxidizing agent is added to the mixture; the mixture is uniformly mixed, such that a dispersed phase is formed; (3) a disperse medium is adopted; an inverse suspending dispersing agent is added to the disperse medium; the mixtureis heated, such that the dispersing agent is dissolved; (4) the dispersed phase is added to the disperse medium, and the mixture is uniformly mixed by stirring, such that a water-in-oil suspension liquid is formed; nitrogen is delivered in for removing oxygen; or a reducing agent can be added, and a reaction is carried out for 0.5-5h under a temperature of 0-60 DEG C; (5) when the reaction is finished, the temperature is reduced, oil and water phases are separated; and the material is washed, such that the cation starch microspheres are obtained. The technology provided by the invention is simple, and is suitable for industrial productions. The cation starch microspheres provided by the invention is advantaged in high absorbency and good thermal stability.

Description

[0001] technical field [0002] The invention relates to the preparation of starch microspheres, in particular to a method for preparing quaternary phosphonium cationic starch microspheres. The cationic starch microspheres produced by this technology can be used in industries and fields such as chemical industry, pharmacy, petroleum, environmental protection, agriculture and mining. Adsorption and / or controlled release of anionic compounds. Background technique [0003] Cross-linked starch microspheres use natural polymers as carriers, which have the advantages of degradability, controlled release, biocompatibility, adsorption and embedding, and rich sources of raw materials. They are used as carriers, adsorbents, embedding agents, etc. It has broad application prospects in industries and fields such as medicine, petroleum, environmental protection, agriculture and mining, especially in the fields of drug loading and separation and purification. [0004] There are three typ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/00C08F220/56C08F226/02C08F230/02C08F2/32C08F4/40C08J3/16C08L51/02B01J20/26B01J20/30
Inventor 宋伟强魏凤春程文喜夏绍灵张琳琪彭进
Owner HENAN UNIVERSITY OF TECHNOLOGY
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