Preparation of epichlorohydrin-dimethylamine cationic polymer/bentonite by inter-layer polymerization
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Dimethylamine,epichlorohydrin,and ethylenediamine were used as inter-layer reagents to prepare epicholorohydrin-dimethylamine cationic polymer/bentonite (EPI-DMA/Bt) with the monomer-insert inter-layer polymerization method.The influence of the amounts of dimethylamine,epichlorohydrin,and ethylenediamine,reaction temperature and reaction time on the performance of EPI-DMA/Bt were investigated. This composite structure was characterized with XRD and specific surface area measurement.The results showed that when the amount of dimethylamine was 3 mmol·g-1,n(epichlorohydrin/dimethylamine)=1∶1 and m[ethylenediamine/(epichlorohydrin + dimethylamine)]=2%,reacting at 65℃ for 3 h,the adsorption efficiency of active jade blue (K-GL) on the EPI-DMA/Bt product was above 90%.Keywords:
Dimethylamine
Epichlorohydrin
Cationic polymerization
Ethylene diamine
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Na-montmorillonite was organically modified by the cationic exchange method using 2,4,6-tris-(dimethylaminomethyl) phenol(DMP-30) as the modifier.The influence of the molar ratio of DMP-30 to HCl was stu-died on the organic treatment of Na-montmorillonite.The morphologies and structures of the as-obtained samples were characterized by SEM,TEM,IR and XRD.The results show that at a proper molar ratio(1∶2) of DMP -30 to HCl,the DMP-30 molecules are successfully intercalated into the layers of montmorillonite,and the space of organically modified montmorillonite layers increases from 1.34 nm to 1.81 nm.Nanocomposites were prepared by the in situ polymerization of epoxy resins in the presence of the organo-modified montmorillonite(OMMT).The structure of the nanocomposites was studied by XRD.The d001 peak of the organic montmorillonite disappeared,indicating that the organo-modified montmorillonite was completely exfoliated in the epoxy matrix.
Cationic polymerization
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Cross-linked copolymer beads were prepared by suspension polymerization of styrene (0.90 mol) and divinyl benzene (DVB) (0.10 mol) mixtures. The resulting copolymer beads with sulfonamide-based quaternary amide functions were prepared in three steps: (1) by chlorosulfonation with chlorosulfonic acid; (2) by sulfonamidation reaction with N,N-dimethylethylenediamine; and (3) by quaternization reaction with chloroacetamide. The resulting polymer resin, which had a chloroacetamide content of 2.50 mmol/g, was effective in extracting mercury from aqueous solutions. The mercury sorption capacity was around 3.0 mmol/g in non-buffered conditions. Experiments performed in identical conditions with several metal ions revealed that Cd(II), Mg(II), Zn(II), and Fe(III) ions also were extractable in low quantities (0.2–0.8 mmol/g). The sorbed mercury could be eluted by repeated treatment with hot acetic acid without hydrolysis of the amide groups.
Amide
Mercury
Sulfonamide
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The cationic polymer PEA was synthesized by ring-opening reaction and quaterisation with epichlorohydrin and β-hydroxy alkyl propyl ether amine as the main materials.Study on the efffect of rate of charge, reaction time and reaction temperature on cationic degree and epoxy value. Capability of adsorption on the sand and anti-swelling resistance were studied. The results showed that the best polymerization conditions as follows,reaction temperature was 60 °C, reaction time was 6 h, the rate of charge of epichlorohydrin toβ-hydroxy alkyl propyletheramine was 2.5:1. Under these conditions , the cationic degree of PEA was 3.962 mmol/g, epoxy value was 0.12. Then it was performed the water absorption.
Epichlorohydrin
Cationic polymerization
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The quaternary ammonium salt cationic monomer dimethyld ia llylammonium chloride (DMD C) was synthesized by two steps.Firstly,1 mole of aq ueous solution of dimethylamine was charged in a flask,1 mole of allyl chloride a nd 1 mole of 40% aqueous solution of caustic soda were added dropwise in such a way that both additions ended at the same time.The temperature was maintained be low 40 ℃.After additions the reaction was continued for 2 h.Then the upper laye r of organic phase was separated.Secondly,the organic phase obtained above was d issolved in an appropriate amount of acetone,then another 1 mole of allyl chlori d e was added while the temperature was maintained below 30 ℃ by cooling.After 4 h,the separated crystals was filtered,washed and dried.Thus the cationic monomer dimethyldiallylammonium chloride was obtained.The yield was 63% in general.The copolymer of DMD C and acrylamide(AM)(mole ratio=1∶3)was prepared in aqueous s olution with redox initiator.The reaction proceeded at 40 ℃ for 6～8 h.Stru ctures of the monomer and copolymer were characterized by IR and 1 HNMR.
Cationic polymerization
Mole fraction
Dimethylamine
Ammonium chloride
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1,2,3-Triazole-group-containing resins for palladium ion adsorption in HCl media were prepared. The monomer, synthesized from acryloyl chloride and 3-(1,2,3-triazol-1-yl) propanol, and a crosslinker, ethylene glycol dimethacrylate, was polymerized in dimethyl sulfoxide via radical polymerization. The specific surface area decreased with increasing monomer:crosslinker molar ratio. In acidic media, the adsorption of palladium ions was greater than those of platinum and ruthenium ions, because stable complexes were formed between palladium ions and triazole groups. The maximum amount of palladium ions adsorbed was 0.41 mol/kg.
Acryloyl chloride
Ethylene glycol dimethacrylate
Triazole
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A humic acid cross- linked resin was synthesized by reversed- phase suspension polymerization with natural organic macromolecular humic acid as main material,acrylic acid and N- isopropyl acrylamide as co-monomer,methylene bisacrylamide as the cross linking agent,potassium persulfate as the initiator and the span- 65 as the stabilization agent. The cross- linked resin was used as an adsorbent in a series of bath adsorption experiments for the removal of Ni( Ⅱ) from aqueous solution. The effects of adsorption temperature,p H value on adsorption property were discussed. The results showed that the removal rate of Ni( Ⅱ) were up to 99. 8 % with p H 4 at 35 ℃.
Potassium persulfate
Acrylic acid
Persulfate
Suspension polymerization
Isopropyl
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Using polystyrene ethylenediamine resin (PS-EDA-NH2) and cyanuric chloride as raw materials, polystyrene chlorotriazine resin (PS-EDA-C3N3Cl2) was prepared by nucleophilic substitution reaction. The influence factors of the reaction, such as the swelling time, reaction time and temperature, acid-capturer species and pH value, were optimized. The experimental results show that the optimal reaction conditions are as follows: the molar ratio of PS-EDA-NH2 : cyanuric chloride being 1:1.2, reaction temperature of 0～5℃, the acid-capturer being Na2CO3 and molar ratio of PS-EDA-NH2 : acid-capturer being 1:1. 30 min after the reaction was started, the reaction system was controlled under weak acidic condition (pH=3～4), then the pH of the reaction system was slowly increased to make the system become under neutral condition (pH=6～7). Under above conditions, the highest weight increasing ratio of the reaction is 27.5%, the degree of amine transformation is 61.1% and the activated chlorine atoms on the surface of the prepared PS-EDA-C3N3Cl2 reach 123.2%. As an active intermediate, many functional media could be obtained by derivatization of the prepared polystyrene chlorotriazine resins.
Cyanuric chloride
Polystyrene
Molar ratio
Ethylene diamine
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Abstract From 1‐chloro‐2,3‐epoxypropane (epichlorohydrin), soluble poly(epichlorohydrin)s were prepared with molar masses in the range of 3,7 · 10 4 to 1,7 · 10 5 g/mol, using a complex of epichlorohydrin with hexaamminecalcium. These poly(epichlorohydrin)s were modified by reaction with 2‐mercaptoethanol or thioglycolic acid. The yields of these reactions range between 40 and 60%. The drop of molecular weight due to modification oscillate between 3,8 and 48,1%. The structure of the modified polymers was confirmed by elemental analyses, thermogravimetric and mass spectroscopic investigations. These chemical modifications carried out with poly(epichlorohydrin)s lead to water‐soluble products.
Epichlorohydrin
Thioglycolic acid
Thermogravimetric analysis
Chemical modification
Molar mass
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Poly(vinylbenzylchloride/divinylbenzene); by high internal phase emulsion (poly(VBC/DVB)HIPE) was functionalized with diamines (ethylenediamine, piperazine, aminopiperidine, and imidazole) to improve carbon dioxide adsorption capacity. The amine group in the poly(VBC/DVB)HIPE was confirmed and quantified by Fourier transform infrared spectroscopy and elemental analysis. The surface area, pore size, and pore volume of the materials, after being functionalized with amines, were reduced. The order of the amine loading in the materials was ethylenediamine > piperazine > aminopiperidine > imidazole. The CO2 adsorption capacities were 2.18, 0.83, 0.66, and 0.39 mmol/g.m2.mol amine for the polyHIPE materials of ethylenediamine, piperazine, aminopiperidine, and imidazole, respectively.
Ethylene diamine
Piperazine
Divinylbenzene
Imidazole
Surface Modification
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Poly(bis(2-(trimethylamino)ethyl) 2-hydroxyl propylidene ammonium) chloride (PTMAEPAC) is one kind of oligomeric cationic polymer with a quarter nitrogen atom on its main and side chain. It was synthesized from Bis(2-trimethyl ammonium)ethyl ammonium chloride (TMAEAC) and epichlorohydrin (ECH) by copolymerization reaction, effects of reaction temperature, mole ratio of raw materials, reaction time, amount of solvent on the cationicity of product were studied. The structure of PTMAEPAC was confirmed by IR and 1H-NMR, and its anti-clay-expanding ability was studied. The results show that the cationicity of PTMAEPAC can reach 83.9% with the reaction time of 6h at 65°C when TMAEAC-to-ECH mole ratio is 1.2:1 and the amount of solvent is 30% in total. According to the IR and NMR analysis the product has the same structure with the aim compound. When the content of the product is 3 wt% it has a good anti-clay-expanding ratio of 96.1%.
Cationic polymerization
Epichlorohydrin
Ammonium chloride
Proton NMR
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