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CN-121609418-B - Aluminum ferric sulfate flocculating agent and preparation method thereof

CN121609418BCN 121609418 BCN121609418 BCN 121609418BCN-121609418-B

Abstract

The invention relates to the technical field of water treatment flocculating agent, and discloses an aluminum ferric sulfate salt flocculating agent and a preparation method thereof, wherein the method comprises the steps of firstly carrying out acid activation, silanization, starch etherification grafting and free radical copolymerization modification on attapulgite to prepare a modified attapulgite functional carrier with a nano adsorption framework, an organic long chain and strong electropositivity; then taking the carrier as a core, carrying out hydrolysis-loading reaction with ferric sulfate, aluminum sulfate and carbide slag under the control of pH, finally introducing sodium silicate to construct an inorganic gel network, curing and drying to obtain the aluminum ferric sulfate salt flocculating agent. The invention realizes multiple synergies of electric neutralization, adsorption bridging and net capturing rolling and sweeping by constructing an organic-inorganic hybrid structure, and the product has high-efficiency removal capability for colloid particles and soluble organic matters, compact flocs, rapid sedimentation and low-cost raw materials, stable process and environment-friendly comprehensive advantages.

Inventors

  • YANG JIANJUN
  • BAI YEWEI
  • ZHANG LIPING

Assignees

  • 陕西卓越材料科技有限公司

Dates

Publication Date
20260512
Application Date
20260202

Claims (8)

  1. 1. The aluminum ferric sulfate salt flocculating agent is characterized by comprising 8-15 parts by weight of aluminum sulfate, 15-30 parts by weight of ferric sulfate, 10-25 parts by weight of modified attapulgite, 1-5 parts by weight of carbide slag and 3-10 parts by weight of sodium silicate; the preparation method of the modified attapulgite comprises the following steps: Step (1), adding attapulgite and hydrochloric acid solution into a beaker, stirring and reacting for 2-3 hours, filtering, washing with water, drying a filter cake, and grinding to obtain acidified attapulgite; Adding an ethanol aqueous solution and 3-aminopropyl triethoxysilane into a flask provided with a condensation reflux device, uniformly mixing, adding a hydrochloric acid solution to adjust the pH to 4-5, stirring at room temperature for reacting for 20-30min, adding acidified attapulgite, heating to 75-80 ℃, stirring for reacting for 2-3h, centrifuging, washing with absolute ethanol, centrifuging for 3 times, and drying to obtain the aminated attapulgite; Adding the aminated attapulgite and deionized water into a beaker, carrying out ultrasonic treatment for 20-30min, adding corn starch, heating to 80-90 ℃, stirring and reacting for 20-30min, cooling to 40-50 ℃, adding sodium hydroxide solution to adjust the pH value to 10-11, dropwise adding epichlorohydrin, stirring and reacting for 2-3h, finally dropwise adding hydrochloric acid solution to neutralize the pH value of the system to 6-7, pouring the product into absolute ethyl alcohol for precipitation, washing the precipitate with ethanol water solution for 3 times, filtering, drying and grinding to obtain the starch grafted amino attapulgite; And (4) adding starch grafted amino attapulgite, deionized water, acrylamide and acryloyloxyethyl trimethyl ammonium chloride into a flask provided with a condensing reflux device under the nitrogen atmosphere, uniformly mixing, stirring for 30-40min, adding ammonium persulfate and sodium bisulfite, heating to 50-60 ℃, stirring for reacting for 4-5h, pouring the product into absolute ethyl alcohol for precipitation, washing the precipitate with absolute ethyl alcohol for 3 times, filtering, and drying to obtain the modified attapulgite.
  2. 2. The aluminum ferric sulfate salt flocculant according to claim 1, wherein the concentration of the hydrochloric acid solution is 1-3mol/L, the concentration of the sodium hydroxide solution is 3-6wt%, and the volume fraction of ethanol in the ethanol water solution is 20-30%.
  3. 3. The aluminum ferric sulfate salt flocculant according to claim 1, wherein the mass ratio of the attapulgite to the hydrochloric acid solution in the step (1) is 10 (100-120).
  4. 4. The aluminum ferric sulfate salt flocculating agent according to claim 1, wherein the mass ratio of the ethanol aqueous solution, the 3-aminopropyl triethoxysilane and the acidified attapulgite in the step (2) is (100-150): (0.2-1): 10.
  5. 5. The aluminum ferric sulfate salt flocculating agent according to claim 1, wherein the mass ratio of the amino attapulgite, deionized water, corn starch and epichlorohydrin in the step (3) is 10 (150-200): 3-10): 0.03-1.
  6. 6. The aluminum ferric sulfate salt flocculating agent according to claim 1, wherein the mass ratio of the starch grafted amino attapulgite, deionized water, acrylamide, acryloyloxyethyl trimethyl ammonium chloride, ammonium persulfate and sodium bisulfate in the step (4) is 100 (1000-2000): (120-220): (20-100): (0.12-1.75): (0.06-0.88).
  7. 7. A method for preparing the aluminum ferric sulfate salt flocculating agent according to any one of claims 1 to 6, wherein the method for preparing the aluminum ferric sulfate salt flocculating agent comprises the following steps: Adding modified attapulgite and deionized water into a flask, performing ultrasonic treatment for 20-30min, adding aluminum sulfate, ferric sulfate and carbide slag, dropwise adding a sodium hydroxide solution under stirring to adjust the pH to 5-6, heating to 40-60 ℃, stirring for reaction for 1-2h, adding a sodium silicate solution with the concentration of 8-10wt%, stirring and mixing for 20-30min, standing and curing for 18-20h, drying to constant weight at 80-90 ℃, and crushing to obtain the aluminum ferric sulfate salt flocculating agent.
  8. 8. The method for preparing the aluminum ferric sulfate salt flocculant according to claim 7, wherein the addition amount of the deionized water is 8-15 times of the total mass of the modified attapulgite, aluminum sulfate, ferric sulfate and carbide slag.

Description

Aluminum ferric sulfate flocculating agent and preparation method thereof Technical Field The invention relates to the technical field of water treatment flocculating agents, in particular to an aluminum ferric sulfate flocculating agent and a preparation method thereof. Background Along with the rapid development of industrialization and urban treatment, the water environment pollution problem is increasingly serious, and the development of efficient and economic water treatment technology is of great importance. The chemical flocculation method is one of the core processes of water treatment because of simple and convenient operation and obvious effect, and the efficiency of the chemical flocculation method is greatly dependent on the performance of the flocculant. At present, commonly used flocculating agents mainly comprise aluminum salt systems (such as polyaluminum chloride), iron salt systems (such as polymeric ferric sulfate) and inorganic polymer flocculating agents. The aluminum salt flocculating agent has good turbidity removal effect, but aluminum ions are easy to remain in the water body after treatment, potential ecological and health risks exist, and the flocculating body formed by the ferric salt flocculating agent is compact, quick in sedimentation and strong in corrosiveness. Single inorganic flocculants generally have the problems of low charge density, small molecular weight, limited removal effect on soluble organic matters, and the like. Meanwhile, the preparation of a flocculating agent or coagulant aid by using natural minerals (such as attapulgite) as raw materials is also attracting attention. Attapulgite has unique nanofiber structure and adsorption performance, but the original soil has single surface inertia and charge property, and has limited direct use effect, and the attapulgite is usually modified to improve the efficiency. However, most of the existing modification methods are simple acid treatment or roasting, or only single type of organic grafting is carried out, and the skeleton effect of inorganic minerals, bridging capability of organic polymers and electric neutralization advantage of specific functional groups (such as strong cationic groups) are not fully integrated and synergistically exerted, so that further improvement of the performance is limited. Therefore, the novel composite flocculating agent which can deeply integrate the characteristics of inorganic minerals and organic polymers, has the advantages of high-efficiency turbidity removal, deep decolorization, rapid sedimentation and good economical and environmental protection performance is developed, and has important practical significance for promoting the progress of water treatment technology. Disclosure of Invention The technical problems to be solved are as follows: Aiming at the defects of the prior art, the invention provides the aluminum ferric sulfate flocculating agent and the preparation method thereof, which solve the problems of inherent defects of the existing aluminum salt or ferric salt flocculating agent, poor removal effect on soluble organic matters due to insufficient function synergy of the conventional composite flocculating agent, poor performance of the natural attapulgite as a flocculating material after direct or simple modification, and the like. (II) technical scheme: In a first aspect, the invention provides an aluminum ferric sulfate salt flocculating agent, wherein the aluminum ferric sulfate salt flocculating agent comprises 8-15 parts by weight of aluminum sulfate, 15-30 parts by weight of ferric sulfate, 10-25 parts by weight of modified attapulgite, 1-5 parts by weight of carbide slag and 3-10 parts by weight of sodium silicate. Further, the preparation method of the modified attapulgite comprises the following steps: and (1) adding the attapulgite and the hydrochloric acid solution into a beaker, stirring and reacting for 2-3 hours, filtering, washing with water, drying a filter cake, and grinding to obtain the acidified attapulgite. Adding an ethanol aqueous solution and 3-aminopropyl triethoxysilane into a flask with a condensing reflux device, uniformly mixing, adding a hydrochloric acid solution to adjust the pH to 4-5, stirring at room temperature for reaction for 20-30min, adding acidified attapulgite, heating to 75-80 ℃, stirring for reaction for 2-3h, centrifuging, washing with absolute ethanol, centrifuging for 3 times, and drying to obtain the aminated attapulgite. Adding the aminated attapulgite and deionized water into a beaker, carrying out ultrasonic treatment for 20-30min, adding corn starch, heating to 80-90 ℃, stirring and reacting for 20-30min, cooling to 40-50 ℃, adding sodium hydroxide solution to adjust pH to 10-11, dropwise adding epichlorohydrin, stirring and reacting for 2-3h, finally dropwise adding hydrochloric acid solution to neutralize pH of a system to 6-7, pouring the product into absolute ethyl alcohol for precipitation, washing the pre