A kind of preparation method of water-in-water emulsion type cationic polysaccharide biological flocculant

Abstract

The invention relates to a preparation method of a water-in-water emulsion-type cation polysaccharide biological flocculant. The preparation method is characterized in that: an auto-polymer or a copolymer of several types of unsaturated cation monomers is used as a stabilizer, a non-ionic polysaccharide biological flocculant is used as an auxiliary stabilizer, an aqueous solution of inorganic salts is used as a continuous phase, and by virtue of certain technological control, free radical polymerization is performed in an internal phase aqueous solution to form stable and dispersed cation polysaccharide biological flocculant emulsion containing micro polymer particles, wherein the solid content is more than or equal to 30 percent, the appearance viscosity is 300 to 10000 mPa.s, the average particle size is less than or equal to 10 micrometers, and the stability is more than or equal to 6 months. The product is simple in synthetic process, high in solubility, degradable, good in flocculation effect and free from secondary pollution, can be used for treating urban sewage and industrial waste water and dehydrating sludge, can be used as a filter aid and a retention aid in the papermaking industry, can be used for plugging adjustment and sewage treatment in oil fields and the like and is wide in application prospect and high in environmental protection value.

Description

technical field

[0001] The invention belongs to the technical field of polysaccharide biological flocculant modification technology, in particular to a preparation method of a water-in-water emulsion type cationic polysaccharide biological flocculant. Background technique

[0002] If the traditional aqueous solution polymerization method is not properly controlled, due to the uneven heat transfer and local exotherm during the polymerization process, it will lead to uneven polymerization and even gel formation. The apparent viscosity of the solid content product is very high, which affects the flocculation effect and brings a lot of inconvenience to the later treatment or use. The inverse emulsion polymerization method that appeared later, due to the mild reaction conditions, uniform and easy-to-control system temperature, less side reactions, and the obtained product has a relatively high molecular weight and a narrow distribution, high solid content and low apparent viscosi...

Examples

Embodiment 1

[0027] Preparation of stabilizer-polymethacryloyloxyethyltrimethylammonium chloride aqueous solution: Dilute methacryloyloxyethyltrimethylammonium chloride with a mass fraction of 80% by adding deionized water to a concentration of 40 %, into a three-necked flask, feed nitrogen, slowly heat up to 40°C, then add 0.2wt‰ (accounting for monomer mass) ammonium persulfate and sodium bisulfite with a mass ratio of 1:1, and control the stirring speed to 200r / min , after stirring for 20 minutes, keep warm for 5 hours, take it out and then purify, dry and grind.

[0028] Add water to the stabilizer to make a concentration of 21% aqueous solution, take 32g of this solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 25g of dimethyl diene with a mass concentration of 60%. Propylammonium chloride solution, 3g acrylamide, 40g ammonium sulfate, 0.02g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas...

Embodiment 2

[0031]Preparation of stabilizer-polydimethyldiallyl ammonium chloride aqueous solution: Dimethyldiallyl ammonium chloride with a mass fraction of 60% is diluted with deionized water to a concentration of 30%, and mixed with a three-necked flask , feed nitrogen, slowly raise the temperature to 50°C, then add 0.2wt‰ (accounting for monomer mass) of ammonium persulfate, control the stirring speed at 200r / min, stir for 10min, keep warm for 10h, take it out, purify, dry and grind.

[0032] Add water to the stabilizer to make a concentration of 15.6% aqueous solution, take 42.65g of this solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 18.75g of methacrylic acid with a mass concentration of 80%. Acyloxyethyltrimethylammonium chloride solution, 3.25g methacrylamide, 35g ammonium sulfate, 0.1g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas to remove oxygen, slowly heat up to 50°C, add 6...

Embodiment 3

[0035] Preparation of stabilizer-polymethacryloyloxyethyl dimethyl benzyl ammonium chloride aqueous solution: the mass fraction of methacryloyloxyethyl dimethyl benzyl ammonium chloride is 60%, add deionized water to dilute The concentration is 30%, and in the three-necked flask, feed nitrogen, slowly heat up to 50°C, then add 0.5wt‰ (accounting for monomer mass) of ammonium persulfate, control the stirring speed at 200r / min, stir for 20min, keep warm, 5h, after taking out, purify, dry and grind.

[0036] Add water to the stabilizer to prepare an aqueous solution with a concentration of 5%, take 44.7g of the solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 15g of methacrylamide with a mass concentration of 50%. Propyltrimethylammonium chloride solution, 0.25g acrylamide, 40g ammonium chloride, 0.02g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas to remove oxygen, slowly heat up ...

technical field

[0001] The invention belongs to the technical field of polysaccharide biological flocculant modification technology, in particular to a preparation method of a water-in-water emulsion type cationic polysaccharide biological flocculant. Background technique

[0002] If the traditional aqueous solution polymerization method is not properly controlled, due to the uneven heat transfer and local exotherm during the polymerization process, it will lead to uneven polymerization and even gel formation. The apparent viscosity of the solid content product is very high, which affects the flocculation effect and brings a lot of inconvenience to the later treatment or use. The inverse emulsion polymerization method that appeared later, due to the mild reaction conditions, uniform and easy-to-control system temperature, less side reactions, and the obtained product has a relatively high molecular weight and a narrow distribution, high solid content and low apparent viscosi...

Examples

Embodiment 1

[0027] Preparation of stabilizer-polymethacryloyloxyethyltrimethylammonium chloride aqueous solution: Dilute methacryloyloxyethyltrimethylammonium chloride with a mass fraction of 80% by adding deionized water to a concentration of 40 %, into a three-necked flask, feed nitrogen, slowly heat up to 40°C, then add 0.2wt‰ (accounting for monomer mass) ammonium persulfate and sodium bisulfite with a mass ratio of 1:1, and control the stirring speed to 200r / min , after stirring for 20 minutes, keep warm for 5 hours, take it out and then purify, dry and grind.

[0028] Add water to the stabilizer to make a concentration of 21% aqueous solution, take 32g of this solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 25g of dimethyl diene with a mass concentration of 60%. Propylammonium chloride solution, 3g acrylamide, 40g ammonium sulfate, 0.02g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas...

Embodiment 2

[0031]Preparation of stabilizer-polydimethyldiallyl ammonium chloride aqueous solution: Dimethyldiallyl ammonium chloride with a mass fraction of 60% is diluted with deionized water to a concentration of 30%, and mixed with a three-necked flask , feed nitrogen, slowly raise the temperature to 50°C, then add 0.2wt‰ (accounting for monomer mass) of ammonium persulfate, control the stirring speed at 200r / min, stir for 10min, keep warm for 10h, take it out, purify, dry and grind.

[0032] Add water to the stabilizer to make a concentration of 15.6% aqueous solution, take 42.65g of this solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 18.75g of methacrylic acid with a mass concentration of 80%. Acyloxyethyltrimethylammonium chloride solution, 3.25g methacrylamide, 35g ammonium sulfate, 0.1g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas to remove oxygen, slowly heat up to 50°C, add 6...

Embodiment 3

[0035] Preparation of stabilizer-polymethacryloyloxyethyl dimethyl benzyl ammonium chloride aqueous solution: the mass fraction of methacryloyloxyethyl dimethyl benzyl ammonium chloride is 60%, add deionized water to dilute The concentration is 30%, and in the three-necked flask, feed nitrogen, slowly heat up to 50°C, then add 0.5wt‰ (accounting for monomer mass) of ammonium persulfate, control the stirring speed at 200r / min, stir for 20min, keep warm, 5h, after taking out, purify, dry and grind.

[0036] Add water to the stabilizer to prepare an aqueous solution with a concentration of 5%, take 44.7g of the solution in a 500ml three-necked flask, then add 100g of polysaccharide bioflocculant with a mass concentration of 15%, and 15g of methacrylamide with a mass concentration of 50%. Propyltrimethylammonium chloride solution, 0.25g acrylamide, 40g ammonium chloride, 0.02g disodium ethylenediaminetetraacetate, start stirring, pass nitrogen gas to remove oxygen, slowly heat up ...