CN109679015B - Silicon-containing acrylic polymer for red mud sedimentation and preparation method thereof - Google Patents
Silicon-containing acrylic polymer for red mud sedimentation and preparation method thereof Download PDFInfo
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- CN109679015B CN109679015B CN201811540510.2A CN201811540510A CN109679015B CN 109679015 B CN109679015 B CN 109679015B CN 201811540510 A CN201811540510 A CN 201811540510A CN 109679015 B CN109679015 B CN 109679015B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
Abstract
The invention discloses a silicon-containing acrylic copolymer for red mud sedimentation, which is synthesized by the following raw materials: acrylic acid, acrylamide, acrylate containing silane, anti-metal agent, cosolvent and dispersant; a series of copolymerization products are prepared by controlling the proportion of acrylic acid, acrylamide and silane-containing acrylate. The acrylic copolymer has good flocculation effect on heavy metal ions and organic matters, and is expected to be used in the fields of red mud sedimentation and other sewage treatment.
Description
Technical Field
The invention relates to the technical field of high polymer material synthesis, in particular to a silicon-containing acrylic polymer for red mud sedimentation and a preparation method thereof.
Background
The red mud is waste generated in the production process of alumina, and has the advantages of soft texture, poor fluidity, small particle size, easy scabbing and small density difference between liquid and solid particles. With the development of the alumina industry in China, the separation operation of the red mud gradually becomes a bottleneck between alumina production processes, and the development of the alumina industry in China is greatly limited. The flocculation precipitation method is a simple and economic water treatment method which is generally used for improving water quality at home and abroad. Flocculation technology has evolved as one of the key links in modern municipal water supply and industrial wastewater treatment industries. The type, nature and performance of the flocculating agent are good key factors relating to the effect of the flocculation treatment.
Polyacrylic acid polymers are often used as flocculating agents to settle metal ions, are widely applied to water treatment, are low in dosage, are high in flocculation speed due to the bridging effect of macromolecules, are slightly influenced by pH value and temperature, but cannot meet the requirement of flocculation effect in certain fields, and are required to be modified in order to further improve the flocculation effect. For example, in the chinese patent CN104724808A, the inorganic polymeric flocculant is compounded with cationic polyacrylamide, but the inorganic polymeric flocculant contains aluminum ions and iron ions, which is not favorable for the flocculation effect of red mud.
Disclosure of Invention
In view of the above problems in the prior art, the present applicant provides a silicon-containing acrylic polymer for red mud sedimentation and a preparation method thereof. The polymer of the invention has low synthesis cost and good flocculation effect on red mud.
The technical scheme of the invention is as follows:
the silicon-containing acrylic polymer for red mud sedimentation uses monomers of acrylic acid, acrylamide and silane-containing acrylate, and is copolymerized by the following weight fractions:
the silane-containing acrylate is methacryloyloxymethyltrimethylsilane, 3- (methacryloyloxy) propyltrimethoxysilane, allyltrimethylsilane, 3- [ dimethoxy (meth) silyl ] propyl methacrylate, 3- [ diethoxy (meth) silyl ] propyl methacrylate, or 3- (methoxydimethylsilyl) propyl acrylate.
A preparation method of a silicon-containing acrylic polymer for red mud sedimentation comprises the following steps:
(1) mixing and stirring 100 parts of acrylic acid solution, 10-30 parts of acrylamide and 0-30 parts of silane-containing acrylate until the mixture is clear and transparent, adding tetrahydrofuran serving as a solvent to prepare a solution with the mass concentration of 15-36%, and then adding an anti-metal agent, a cosolvent and a dispersing agent;
(2) and (3) introducing nitrogen to exhaust air in the system, adding 0.05-3 parts of initiator azobisisobutyronitrile, adjusting the stirring speed to 300-800 r/min at 50-70 ℃, and reacting for 6-12 hours to obtain the silicon-containing acrylic polymer.
And adjusting the pH value of the acrylic acid solution to 6-8 by using ammonia water or sodium hydroxide.
The anti-metal agent is ethylene diamine tetraacetic acid; the cosolvent is urea; the dispersant is isopropanol, and the total mass of the anti-metal agent, the cosolvent and the dispersant accounts for 0.07-1% of the mass of the polymerization system.
The beneficial technical effects of the invention are as follows:
the acrylate containing silane has silane groups or siloxane groups, the silane groups and metal ions directly have chelation, the siloxane groups can generate hydrolysis reaction, and-R-Si-OH groups generated by the hydrolysis reaction can form stable Si-O-M bonds with heavy metal ions, so that the acrylate containing silane is introduced into the polyacrylic acid polymer, and the sedimentation effect on red mud can be effectively improved.
The silicon-containing acrylic polymer prepared by the invention is a flocculant with high molecular weight, good stability and low toxicity, the preparation process is simple, the cost is greatly reduced, and the benefit is improved. Meanwhile, a chain segment containing siloxane is introduced, so that the flocculation effect is improved, and the flocculant has a certain application prospect in flocculants.
Drawings
FIG. 1 is a photograph showing the red mud sedimentation of the silicon-containing acrylic polymer obtained in example 3 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 10g of acrylamide and 10g of methacryloxymethyl trimethyl silane, stirring until the mixture is clear and transparent, adding 700ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 0.05g of azobisisobutyronitrile, adjusting the stirring speed to 300r/min at 50 ℃, and reacting for 6 hours to obtain the polymer containing methacryloyloxymethyl trimethylsilane.
Example 2
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 15g of acrylamide and 15g of 3- (methacryloyloxy) propyl trimethoxy silane, stirring until the mixture is clear and transparent, adding 400ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 1.5g of azobisisobutyronitrile, adjusting the stirring speed to 500r/min at the temperature of 60 ℃, and reacting for 8 hours to obtain the polymer containing the 3- (methacryloyloxy) propyl trimethoxy silane.
Example 3
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 30g of acrylamide and 30g of 3- (methacryloyloxy) propyl trimethoxy silane, stirring until the mixture is clear and transparent, adding 300ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 3g of azobisisobutyronitrile, adjusting the stirring speed to 800r/min at 70 ℃, and reacting for 12 hours to obtain the polymer containing the 3- (methacryloyloxy) propyl trimethoxy silane.
Use of the Polymer of this example for Fe3+The settlement method comprises the following steps:
preparing the polymer into an aqueous solution with the mass fraction of 2%, and adding FeCl with the mass fraction of 4%3Standing the solution at room temperature for 10min, the settling effect is shown in FIG. 1, and it can be seen from FIG. 1 that for Fe3+The solution has good sedimentation effect.
Example 4
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 30g of acrylamide and 30g of allyl trimethyl silane, stirring until the mixture is clear and transparent, adding 300ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 3g of azodiisobutyronitrile, adjusting the stirring speed to 800r/min at 70 ℃, and reacting for 12 hours to obtain the polymer containing the allyl trimethylsilane.
Example 5
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 10g of acrylamide and 10g of allyl trimethyl silane, stirring until the mixture is clear and transparent, adding 700ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 0.05g of azobisisobutyronitrile, adjusting the stirring speed to 300r/min at 50 ℃, and reacting for 6 hours to obtain the polymer containing the allyl trimethylsilane.
Example 6
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution with 15g of acrylamide and 15g of 3- [ dimethoxy (methyl) silyl ] propyl methacrylate, stirring until the mixture is clear and transparent, adding 400ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 1.5g of azobisisobutyronitrile, adjusting the stirring speed to 500r/min at the temperature of 60 ℃, and reacting for 8 hours to obtain the polymer containing 3- [ dimethoxy (methyl) silyl ] propyl methacrylate.
Example 7
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution with 30g of acrylamide and 30g of 3- [ dimethoxy (methyl) silyl ] propyl methacrylate, stirring until the mixture is clear and transparent, adding 300ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 3g of azobisisobutyronitrile, adjusting the stirring speed to 800r/min at 70 ℃, and reacting for 12 hours to obtain the polymer containing 3- [ dimethoxy (methyl) silyl ] propyl methacrylate.
Example 8
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution with 10g of acrylamide and 10g of 3- [ dimethoxy (methyl) silyl ] propyl methacrylate, stirring until the mixture is clear and transparent, adding 700ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 0.05g of azobisisobutyronitrile, adjusting the stirring speed to 300r/min at the temperature of 50 ℃, and reacting for 6 hours to obtain the polymer containing 3- [ dimethoxy (methyl) silyl ] propyl methacrylate.
Example 9
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution with 15g of acrylamide and 15g of 3- [ diethoxy (methyl) silyl ] propyl methacrylate, stirring until clear and transparent, adding 400ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 1.5g of azobisisobutyronitrile, adjusting the stirring speed to 500r/min at the temperature of 60 ℃, and reacting for 8 hours to obtain the polymer containing the 3- [ diethoxy (methyl) silyl ] propyl methacrylate.
Example 10
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution with 30g of acrylamide and 30g of 3- [ dimethoxy (methyl) silyl ] propyl methacrylate, stirring until the mixture is clear and transparent, adding 300ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 3g of azodiisobutyronitrile, adjusting the stirring speed to 800r/min at 70 ℃, and reacting for 12 hours to obtain the polymer containing 3- [ diethoxy (methyl) silyl ] propyl methacrylate.
Example 11
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 10g of acrylamide and 10g of 3- (methoxydimethylsilyl) propyl acrylate, stirring until the mixture is clear and transparent, adding 700ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 0.05g of azobisisobutyronitrile, adjusting the stirring speed to 300r/min at the temperature of 50 ℃, and reacting for 6 hours to obtain the polymer containing the 3- (methoxydimethylsilyl) propyl acrylate.
Example 12
A silicon-containing acrylic polymer for red mud sedimentation is prepared by the following steps:
(1) mixing 100g of acrylic acid solution, 15g of acrylamide and 15g of 3- (methoxydimethylsilyl) propyl acrylate, stirring until the mixture is clear and transparent, adding 400ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 1.5g of azobisisobutyronitrile, adjusting the stirring speed to 500r/min at the temperature of 60 ℃, and reacting for 8 hours to obtain the polymer containing the 3- (methoxydimethylsilyl) propyl acrylate.
Comparative example
An acrylic polymer for red mud sedimentation, which comprises the following steps:
(1) mixing 100g of acrylic acid solution and 30g of acrylamide, stirring until the mixture is clear and transparent, adding 300ml of tetrahydrofuran, and then adding 2g of ethylenediamine tetraacetic acid, 8g of urea and 11g of isopropanol;
(2) and introducing nitrogen to exhaust air in the system, adding 3g of azodiisobutyronitrile, adjusting the stirring speed to 800r/min at 70 ℃, and reacting for 12 hours to obtain the acrylic polymer without the silane coupling agent.
Claims (2)
1. The silicon-containing acrylic polymer for red mud sedimentation is characterized in that monomers used by the polymer are acrylic acid, acrylamide and acrylate containing silane, and the silicon-containing acrylic polymer is copolymerized by the following weight fractions:
acrylic acid 100 parts
10-30 parts of acrylamide
10-30 parts of acrylate containing silane
0.05-3 parts of an initiator;
the preparation method of the silicon-containing acrylic polymer for red mud sedimentation comprises the following steps:
(1) mixing and stirring 100 parts of acrylic acid solution, 10-30 parts of acrylamide and 10-30 parts of acrylate containing silane until the mixture is clear and transparent, adding tetrahydrofuran serving as a solvent to prepare a solution with a mass concentration of 15-36%, and then adding an anti-metal agent, a cosolvent and a dispersing agent; the anti-metal agent is ethylene diamine tetraacetic acid; the cosolvent is urea; the dispersing agent is isopropanol, and the total mass of the anti-metal agent, the cosolvent and the dispersing agent accounts for 0.07-1% of the mass of the polymerization system;
(2) introducing nitrogen to exhaust air in the system, adding 0.05-3 parts of initiator azobisisobutyronitrile, adjusting the stirring speed to 300-800 r/min at 50-70 ℃, and reacting for 6-12 hours to obtain the silicon-containing acrylic polymer;
the silane-containing acrylate is methacryloyloxymethyltrimethylsilane, 3- (methacryloyloxy) propyltrimethoxysilane, 3- [ dimethoxy (meth) silyl ] propyl methacrylate, 3- [ diethoxy (meth) silyl ] propyl methacrylate, or 3- (methoxydimethylsilyl) propyl acrylate.
2. The silicon-containing acrylic polymer for red mud sedimentation according to claim 1, wherein the acrylic acid solution is adjusted to pH = 6-8 with ammonia water or sodium hydroxide.
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| CN111871071B (en) * | 2020-06-17 | 2022-02-15 | 吉祥三宝高科纺织有限公司 | High-temperature-resistant and corrosion-resistant microporous membrane material for processing mask filter layer |
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| CN101735376A (en) * | 2009-12-13 | 2010-06-16 | 安徽省天润功能高分子工程研究有限公司 | Preparation method of red mud sinking agent |
| CN105504163A (en) * | 2016-01-20 | 2016-04-20 | 广东溢达纺织有限公司 | Cationic flocculant and preparation method thereof |
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| CN102515228B (en) * | 2007-04-20 | 2016-08-31 | 氰特技术公司 | Silicon-containing polymer is to improving the purposes of red mud flocculation in BAYER processing |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101735376A (en) * | 2009-12-13 | 2010-06-16 | 安徽省天润功能高分子工程研究有限公司 | Preparation method of red mud sinking agent |
| CN105504163A (en) * | 2016-01-20 | 2016-04-20 | 广东溢达纺织有限公司 | Cationic flocculant and preparation method thereof |
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