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Preparation method of starch grafted acrylamide flocculating agent

A technology of acrylamide and starch grafting, which is applied in the direction of flocculation/sedimentation water/sewage treatment, etc., can solve the problems of many by-products, mild reaction conditions, implosion polymerization, etc., to improve the reaction rate and conversion rate, mild reaction conditions, The effect of good flocculation performance

Inactive Publication Date: 2010-05-12
GUANGZHOU UNIVERSITY
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  • Abstract
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  • Application Information

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Problems solved by technology

However, the aqueous solution polymerization method is difficult to control the production process due to the difficulty of heat dissipation during the polymerization process, and the production process is difficult to control, and there are many by-products, and the resulting product has poor stability.
[0004] The inverse emulsion polymerization method is a new polymerization method that has attracted much attention in recent years. It is characterized in that the water-soluble monomer is dispersed in a non-polar liquid with the help of an emulsifier, and then polymerized after forming a water-in-oil state. This This method has the advantages of high polymerization rate, high product solid content, large molecular weight and narrow distribution, and mild reaction conditions. The method of amide graft copolymer, this method is: will be based on Span80 composite emulsifier and liquid paraffin mix, add the mixture of 30% starch milk and 40% monomer acrylamide under stirring to form inverse emulsion, generally Inject high-purity nitrogen for 30 minutes, raise the temperature to 35-55°C, slowly add the initiator ammonium persulfate dropwise and react for 4 hours. The oil-water ratio of the emulsion is 0.8-1.6, the concentration of the emulsifier is 2-10%, the concentration of the initiator is 1-7mmol / L, and the ratio of monomer to starch is 0.8-1.8. The stability of the inverse emulsion system is inverse The key to the success or failure of emulsion polymerization, and the determinant of the stability of the emulsion system is the emulsification system. Although the article claims that the emulsification system in its method is a compound emulsifier, it only discloses one of the components of the compound emulsifier— —Span80, those skilled in the art can't repeat the method and reach the effect claimed by the paper without knowing the remaining components of the emulsifier. In addition, the method of the paper adopts ammonium persulfate as the initiator of polymerization, although ammonium persulfate can The graft copolymerization reaction of starch acrylamide is effectively initiated, but the efficiency of the initiation reaction is low, resulting in a relatively low grafting rate (up to about 85%) and grafting efficiency (less than 60%) of the copolymer.

Method used

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  • Preparation method of starch grafted acrylamide flocculating agent
  • Preparation method of starch grafted acrylamide flocculating agent

Examples

Experimental program
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Effect test

example 1

[0023] Take 40g of liquid paraffin, 2.24g of Span80, 0.16g of Tween 80 and 0.80g of OP-4 in a three-necked flask, stir to dissolve, add water 30mL and starch 6.7g, and stir until an inverse emulsion is formed. The conductivity is close to 0, and the stability of the emulsion is close to 1.

[0024] Pass nitrogen into the above-mentioned emulsion until the oxygen in the three-necked flask is completely removed, heat to 50°C, continue to pass nitrogen and stir, add dropwise 1mL of potassium permanganate solution with a mass concentration of 1%, stir for 20min, add 50% potassium permanganate solution Acrylamide solution 18.8g, react for 3h, stop stirring; transfer the mixture in the beaker to a 1000mL beaker, add ethanol after cooling to room temperature, stir until no solid product is formed, filter and separate the solid in the beaker, and use ethanol and acetone Wash and filter repeatedly until the filter cake is loose and small particles, and finally dry to the moisture conte...

example 2

[0026] Take 46g of liquid paraffin, 3.6g of Span80, 0.1g of Tween 80 and 0.3g of OP-4 in a three-necked flask, stir for 4 to dissolve, add 29.2g of water and 6.7g of starch, and stir until an inverse emulsion is formed. The conductivity is close to 0, and the stability of the emulsion is close to 1.

[0027] Introduce nitrogen into the above-mentioned emulsion until the oxygen in the three-necked flask is completely removed, continue nitrogen and stirring, add 10.8g of 50% acrylamide solution, heat to 40°C, add dropwise 0.6mL of 1% potassium permanganate solution, and react 7h, stop stirring, transfer the mixture in the beaker to a 1000mL beaker, add ethanol after cooling to normal temperature, stir until a solid product is obtained, filter to separate the solid in the beaker from the mixture, and wash the filter cake repeatedly with ethanol and acetone to the filter cake It is loose and small particles, and finally vacuum-dried to the moisture content required by the product....

example 3

[0028] Example 3 Take 27g of liquid paraffin, 0.7g of Span80, 0.05g of Tween 80, and 0.25g of OP-4 in a three-necked flask, stir to dissolve, add 27.6g of water, 6.7g of starch, stir until an inverse emulsion is formed, and measure its conductivity The ratio is close to 0, and the emulsion stability is close to 1.

[0029] Pass nitrogen into the above emulsion until the oxygen in the three-necked flask is completely removed, continue to pass nitrogen and stir, add dropwise 3mL of 1% potassium permanganate solution, stir for 20min, add 26.8g of 50% acrylamide solution, and heat to 60°C , react for 1h, stop stirring, transfer the mixture in the beaker to a 1000mL beaker, add ethanol after cooling to normal temperature, stir until a solid product is obtained, filter and separate the solid in the beaker from the mixture, and wash the filter cake repeatedly with ethanol and acetone until The filter cake is loose and small particles, and finally vacuum-dried to the moisture content ...

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Abstract

The invention provides a preparation method of a starch grafted acrylamide flocculating agent, which comprises the following concrete step of polymerizing starch and acrylamide in a reversed emulsion formed by liquid paraffin, water and a compounded emulsifying agent to form a graft copolymer of the starch and the acrylamide, wherein potassium permanganate is used as an initiator, and the compounded emulsifying agent comprises span 80, Tween 80 and alkylphenol polyoxyethylene (4) in a mass ratio of 7-9:0.1-0.5:0.9-2.5. The method adopts the compounded emulsifying agent comprising the span 80, the Tween 80 and the alkylphenol polyoxyethylene (4) for preparing the reversed emulsion, thereby stabilizing the system of the reversed emulsion, providing a stable reaction environment for polyreaction, and being helpful for improving the stability of products. In addition, in the method, the potassium permanganate is also selected as the initiator, thereby effectively improving the efficiency of initiating the polyreaction.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a polymer compound obtained by reacting only carbon-carbon unsaturated bonds. Background technique [0002] Organic flocculants refer to natural or synthetic organic molecular substances that can produce flocculation. Natural organic flocculants are protein or polysaccharide compounds, such as starch, protein, animal glue, sodium alginate, sodium carboxymethylcellulose, etc.; synthetic organic flocculants include polyacrylamide, sodium polyacrylate, polyethylene Pyridinium salt, polyethyleneimine, etc. These flocculants are all water-soluble linear polymer substances, most of which can be ionized in water, and are polymer electrolytes. According to the characteristics of their dissociated groups, they can be divided into anion, cation and amphoteric types. After the flocculant is ionized in water, its chain molecules can produce bonding and bridging effects, and the charged gro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F251/00C08F220/56C08F2/32C08F4/26C02F1/56
Inventor 尚小琴王东耀刘汝锋
Owner GUANGZHOU UNIVERSITY
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