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Preparation method of quaternary ammonium cationic starch flocculant prepared by dmso/h2o/naoh system

A technology of quaternary ammonium salt cation and flocculant is applied in the field of preparing quaternary ammonium salt cationic starch flocculant in DMSO/H2O/NaOH system, which can solve the problem of low substitution degree, poor hydrophilicity and poor flocculation effect of quaternary ammonium salt cationic starch flocculant. and other problems, to achieve the effect of shortening the total reaction time, improving the reaction efficiency, and strong plasticity

Inactive Publication Date: 2018-11-02
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, wet method and solvent method are the main methods of preparing quaternary ammonium salt cationic starch flocculants, wherein, wet method is to disperse starch in water to form a slurry, and solvent method is to disperse starch in organic solvents (such as ethanol, methanol, iso Propanol, etc.) to form a slurry, the common point is to react with the cationization agent in the heterogeneous system, and the cationization agent is only carried out on the surface of the starch granules, and the degree of substitution of the prepared quaternary ammonium cationic starch flocculant Low, poor hydrophilicity, cannot fully contact with wastewater, cannot form a strong bridging effect with particles, and the flocculation effect is poor

Method used

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  • Preparation method of quaternary ammonium cationic starch flocculant prepared by dmso/h2o/naoh system
  • Preparation method of quaternary ammonium cationic starch flocculant prepared by dmso/h2o/naoh system
  • Preparation method of quaternary ammonium cationic starch flocculant prepared by dmso/h2o/naoh system

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Experimental program
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Effect test

Embodiment 1

[0027] Dissolve 0.27g of sodium hydroxide in 13g of water. After the solid sodium hydroxide is completely dissolved, add 100g of dimethyl sulfoxide and 10g of absolute dry cornstarch, heat and stir at 85°C and react for 1h under reflux conditions to obtain starch activation solution. Get 9.2g of 3-chloro-2-hydroxypropyltrimethylammonium chloride solution (60%) and 4.87g of sodium hydroxide solution (40%) in the ice-water bath after activating for 5 minutes and immediately add to the starch cooled to 60°C In the activation solution, stirred at 500 rpm, reacted at 60°C for 1 hour, cooled to room temperature, extracted the crude product with ethanol, dried under reduced pressure, extracted twice with ethanol-glacial acetic acid mixed solution, dried to constant weight to obtain a white powder It is a quaternary ammonium salt cationic starch flocculant with a measured degree of substitution of 0.154, which can be well dissolved in cold water to form a transparent solution and has ...

Embodiment 2

[0029] Dissolve 0.20g of sodium hydroxide in 10g of water, add 100g of dimethyl sulfoxide and 10g of absolute dry cornstarch to it after the solid sodium hydroxide is completely dissolved, heat and stir at 105°C and condense and reflux for 1 hour, Obtain starch activation solution. Get 10.0g of 3-chloro-2-hydroxypropyltrimethylammonium chloride solution (60%) and 10.0g of sodium hydroxide solution (20%) in an ice-water bath for 3 minutes after activation and immediately add to cool to 70°C In the starch activation solution, stirred at 800 rpm, reacted at 70°C for 0.8h, cooled to room temperature, extracted the crude product with ethanol, dried under reduced pressure, extracted twice with ethanol-glacial acetic acid mixed solution, and dried to constant weight The quaternary ammonium salt cationic starch flocculant in the form of white powder was obtained, and its degree of substitution was measured to be 0.167, which can be dissolved in cold water to form a transparent solutio...

Embodiment 3

[0031] Dissolve 0.13g of sodium hydroxide in 6.5g of water. After the solid sodium hydroxide is completely dissolved, add 100g of dimethyl sulfoxide solution and 10g of dry cornstarch to it, heat and stir at 115°C and condense and reflux for 0.8 After h, the starch activation solution was obtained. Get 10.0g of 3-chloro-2-hydroxypropyltrimethylammonium chloride powder and 20.0g of sodium hydroxide solution (15%), activate it in an ice-water bath for 3 minutes, and immediately add it to the starch activation solution cooled to 75°C , stirred at 500 rpm, reacted at 75°C for 1 h, cooled to room temperature, extracted the crude product with ethanol, dried under reduced pressure and extracted 3 times with a mixed solution of ethanol-glacial acetic acid, dried to constant weight to obtain white powder The quaternary ammonium salt cationic starch flocculant has a degree of substitution of 0.254. It can be well dissolved in cold water to form a transparent solution and has a good floc...

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Abstract

The invention discloses a method for preparing a quaternary ammonium cationic starch flocculant in a DMSO / H2O / NaOH system. The method comprises following steps: 1), NaOH is dissolved in water, DMSO and starch are added, a mixture is heated, stirred and subjected to reflux condensation for a reaction, and a starch activation liquid is obtained; 2), the starch activation liquid obtained in the step 1) is cooled to 60-75 DEG C, then an etherifying agent activation liquid is added and stirred, and a reaction is performed for 0.5-1 h; 3), the white powdery quaternary ammonium cationic starch flocculant is obtained through cooling, purification and drying. According to the method, the starch is pre-activated in the DMSO / H2O / NaOH system, the reactions are performed in a homogeneous system, so that the starch has higher plasticity, active sites for combination of an etherifying agent and the starch are increased, the activated starch can react with the cationic etherifying agent rapidly, the quaternary ammonium cationic starch flocculant prepared with the method can be completely dissolved in water, colloid particles can be clustered through flocculation under the sufficient bridging and cross-linking actions, and the flocculation effect cannot be influenced by a settlement action of the flocculant.

Description

technical field [0001] The invention belongs to the technical field of new environmental protection materials, in particular to a DMSO / H 2 A method for preparing a quaternary ammonium salt cationic starch flocculant in an O / NaOH system. Background technique [0002] With industrial progress and social development, increasing water pollution has posed a major threat to human survival and safety, and has become a major obstacle to human health, economic and social sustainable development. The protection and sustainable use of water resources has drawn extensive attention from all over the world. [0003] Flocculant is currently the most widely used agent in sewage treatment. Flocculation and sedimentation method can quickly increase the sewage treatment rate and improve the wastewater treatment effect in wastewater treatment. It is an efficient and economical water treatment method. At present, flocculants are mainly divided into two categories: inorganic salt flocculants an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/12C02F1/56
CPCC02F1/56C08B31/125
Inventor 金士威肖磊邓克俭
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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