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Preparation method of hydrophobically modified cationic polyacrylamide
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A polyacrylamide, hydrophobic modification technology, applied in the direction of flocculation/sedimentation water/sewage treatment, etc., can solve problems such as environmental pollution
Inactive Publication Date: 2015-05-20
NANJING UNIV OF TECH
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The preparation method of hydrophobically associated polymers is still limited to the traditional micellar copolymerization technology, that is, adding small molecule surfactants to the polymerizationsystem to solubilize hydrophobic monomers, but this method brings great harm to the polymerization process and copolymerization products. A lot of negative impacts and environmental pollution problems
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Embodiment 1
[0013] Embodiment 1. the synthesis of dimethylaminoethyl methacrylate (2)
[0014] Add 40mL dimethylaminoethanol and 100mL ether into a 250mL round bottom bottle, cool in an ice bath, slowly add 40g of methacryloyl chloride (1) dropwise under electromagnetic stirring, and finish the reaction after 4 hours. After filtration, the filtrate was concentrated and then distilled under reduced pressure, and the fraction at 55-57°C / 533.3Pa was collected to obtain the product dimethylaminoethyl methacrylate. yield: 90%, 1 H-NMR (500MHz, DMSO) δ: 6.025(s, 1H), 5.659-5.670(s, 1H), 4.159-4.198(t, 2H), 2.503-2.542(t, 2H), 2.185(s, 6H) , 1.887 (s, 3H).
Embodiment 2
[0015] Embodiment 2. The synthesis of methacryloyloxyethyl octyl ammoniumbromide (4a)
[0016] In a one-necked flask, add the substance 2 purified by distillation, and bromooctane (3a) in an amount 1.1 times that of the substance 2. Acetone is used as a solvent, and the amount added is twice the sum of the volumes of substance 2 and alkylbromide. The addition amount of p-methoxyphenol is 2mmol / L. The system was carried out at 35°C for 20 hours to terminate the reaction, and most of the acetone was removed by rotary evaporation, and an appropriate amount of anhydrousether was added to precipitate, and the product was obtained by suction filtration. The product was recrystallized three times with anhydrousethyl acetate, and dried in a vacuum oven to obtain the substance methacryloyloxyethyloctylammonium bromide (4a), yield: 83.1%, bp.=89°C-91°C , 1 H-NMR (500MHz, DMSO) δ: 6.087(s, 1H), 5.762-5.767(s, 1H), 4.535-4.544(t, 2H), 3.734-3.764(t, 2H), 3.328-3.359(t, 2H), 3.149 ...
Embodiment 3
[0017] Embodiment 3. the synthesis of methacryloyloxy ethyl decyl ammonium bromide (4b)
[0018] Dimethylaminoethyl methacrylate (2) and 1-bromodecane (3b) were prepared according to Example 2 to prepare methacryloxyethyldecylammonium bromide (4b), yield: 81.2%, bp.=90 ℃-92℃, 1 H-NMR (500MHz, DMSO) δ: 6.087(s, 1H), 5.762-5.767(s, 1H), 4.533-4.554(t, 2H), 3.744-3.774(t, 2H), 3.328-3.438(t, 2H), 3.146(s, 3H), 1.912(s, 3H), 1.259-1.682(m, 16H), 0.841-0.884(t, 3H).
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Abstract
The invention belongs to a cationic polymer flocculant, and concretely relates to a preparation method of a novel water-soluble cationic monomer, and a novel preparation method of hydrophobically modified cationic polyacrylamide based on the novel water-soluble cationic monomer. The preparation method of the hydrophobically modified cationic polyacrylamide comprises the following steps: preparing dimethylaminoethyl methacrylate from methacrylic chloride and dimethylamino ethanol, reacting dimethylaminoethyl methacrylate with long chain bromoalkane to obtain the novel water-soluble cationic monomer, and preparing the hydrophobically modified cationic polyacrylamide through adopting a hydrophobic association micropolyphase aqueous solution copolymerization technology. The preparation method of the hydrophobically modified cationic polyacrylamide does not need other surfactants, allows random micro-block structure distributed hydrophobic groups to be successfully introduced to display a unique solution property, and has good industrial prospect.
Description
technical field [0001] The invention belongs to cationic macromolecule flocculants, and specifically relates to the preparation of a novel water-soluble cationic monomer and a novel preparation method of hydrophobically modified cationic polyacrylamide based on it. technical background [0002] At present, water pollution has become one of the major environmental problems in our country. Therefore, it is of great significance to research and develop efficient and economical sewage treatment technology. Among the many water treatment methods at home and abroad, the flocculation-sedimentation method is widely used in the treatment and recycling of industrial and domestic water due to its advantages of simple process, convenient operation and high treatment efficiency. [0003] At present, flocculant products can be divided into four categories: inorganic flocculants, organic flocculants, composite flocculants, and microbial flocculants. Among them, the organic polymer floccu...
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