Method for preparing quaternary ammonium cationic starch flocculant in 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 positive electricity.

Inactive Publication Date: 2016-09-21
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • 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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  • Method for preparing quaternary ammonium cationic starch flocculant in DMSO/H2O/NaOH system
  • Method for preparing quaternary ammonium cationic starch flocculant in DMSO/H2O/NaOH system
  • Method for preparing quaternary ammonium cationic starch flocculant in DMSO/H2O/NaOH system

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Embodiment 1

[0027] Dissolve 0.27g of sodium hydroxide in 13g of water, after the sodium hydroxide solid is completely dissolved, add 100g of dimethyl sulfoxide and 10g of absolutely dry corn starch, heat and stir at 85℃ and condense and reflux for 1 hour to obtain starch Activation solution. Take 9.2g of 3-chloro-2-hydroxypropyltrimethylammonium chloride solution (60%) and 4.87g of sodium hydroxide solution (40%) in an ice-water bath for 5 minutes, and immediately add them to the starch cooled to 60℃ In the activation solution, stir at 500 rpm and react at 60°C for 1 hour, then cool to room temperature, extract the crude product with ethanol, dry under reduced pressure, extract twice with ethanol-glacial acetic acid mixed solution, and dry to constant weight to obtain a white powder The quaternary ammonium salt cationic starch flocculant has a degree of substitution of 0.154. It can be dissolved in cold water to form a transparent solution and has a good flocculation effect.

Embodiment 2

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

Embodiment 3

[0031] Dissolve 0.13g of sodium hydroxide in 6.5g of water, add 100g of dimethyl sulfoxide solution and 10g of absolutely dry corn starch to the sodium hydroxide solid after the solid is completely dissolved, heat at 115℃, stir and condense and reflux for 0.8 After h, the starch activation solution was obtained. Take 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℃ After stirring at 500 rpm and reacting at 75°C for 1 hour, it was cooled to room temperature, the crude product was extracted with ethanol, dried under reduced pressure, and then extracted with ethanol-glacial acetic acid mixed solution for 3 times, and dried to constant weight to obtain a white powder The quaternary ammonium salt cationic starch flocculant has a degree of substitution of 0.254. It can be dissolved in cold water to form ...

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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 environmental protection new materials, and specifically relates to a DMSO / H 2 Method for preparing quaternary ammonium salt cationic starch flocculant in 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 have received extensive attention from the world. [0003] Flocculant is currently the most widely used agent in sewage treatment. The flocculation 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 and organic...

Claims

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Application Information

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Patent Type & Authority Applications(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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