抗氧化耐酸分离CO_2膜制备及性能研究
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摘要
分离CO_2的固定载体膜是一类很有发展前景的分离膜。其中，研究较多的氨基载体膜长期使用可能被氧化，影响其分离含氧化剂（主要是非酸性氧化剂O_2及酸性氧化剂SO_2）烟道气中CO_2时的使用寿命。针对于此，本文采用不同的载体固定方法将羧酸根载体引入膜内，制备出具有较好透过分离性能、抗氧化性能和耐酸的固定载体膜，以适用于烟道气CO_2分离。
用自由基聚合的方法将羧酸根载体引入膜内。以丙烯酸钠为单体，合成聚丙烯酸钠(PAAS)。以PAAS水溶液为涂膜液，聚砜(PS)为支撑层制得PAAS/PS复合膜。用丙烯酰胺(AAm)调节载体含量，制得聚（丙烯酸钠-丙烯酰胺）/聚砜(P(AAS-co-AAm)/PS)复合膜。利用全反射红外光谱(ATR-FTIR)表征了气体组分与膜之间的相互作用，考察了膜的气体透过性能，由此分析了CO_2和N2在膜内的传递机理。研究了AAS含量及湿涂层厚度对膜透过分离性能的影响规律。考察了复合膜的抗氧化和耐酸性能。结果表明，所制膜具有良好的CO_2透过分离性能、抗氧化性和耐酸性。对于CO_2/N2混合气（体积比15/85），AAS含量为47.68mol%，湿涂层厚度为200μm的复合膜在进料气压力为0.11MPa时，CO_2渗透速率为163GPU，分离因子为90。
用共混的方法将羧酸根载体引入膜内。将PAAS与聚乙二醇(PEG)的共混物水溶液涂敷在PS支撑层上制备PAAS-PEG/PS共混复合膜。研究了共混物中PEG分子量以及PAAS/PEG质量比对复合膜CO_2/N2渗透选择性能的影响。结果表明，所制膜具有较高的CO_2透过分离性能，对于CO_2/N2混合气，PEG分子量为20,000，PAAS:PEG质量比为1:2的涂膜液制备的复合膜在进料气压力为0.11MPa时，CO_2渗透速率为700GPU，CO_2/N2分离因子为80。
用界面聚合的方法将羧酸根载体引入膜内。以均苯三甲酰氯(TMC)为有机相单体，二氨基苯甲酸钠(DAmBS)为水相单体，在涂敷了硅橡胶(PDMS)的PS基膜上进行界面聚合制备聚(DAmBS-TMC)/PDMS/PS复合膜。在水相中加入4,7,10-三氧-1,13-癸烷二胺(DEGBAmPE)以调节载体含量及聚合物链段的柔性，从而制备了聚(DAmBS-DEGBAmPE-TMC)/PDMS/PS复合膜。研究了制膜因素对复合膜结构和性能的影响。考察了复合膜的抗氧化性和耐酸性。结果表明，所制膜具有良好的CO_2透过分离性能、抗氧化和耐酸性能。对于CO_2/N2混合气，用0.003mol/L TMC，0.004mol/L DAmBS和0.006mol/L DEGBAmPE所制复合膜在进料气压力为0.11MPa时，CO_2渗透速率为5831GPU，CO_2/N2分离因子为86。
以界面聚合制备的复合膜为例，对烟道气CO_2分离和捕集的过程进行了经济性分析，结果表明，本文制备的CO_2分离膜具有明显的经济优势。
Fixed carrier membranes for CO_2separation are promising membranes. However,most of the fixed carrier membranes contain amine groups as carriers, which may beoxidized by the oxidant gases (mainly O_2) and react with the acidic gas (mainly SO_2)contained in the flue gas. In this work, different methods are used to fixed thecarboxylate group as the carrier in the membrane to get excellent permselectivity,antioxidizability and acid resistance.
The method of the radical polymerization was used to fixed the carboxylate groupas the carrier. Poly(sodium acrylate)(PAAS) and a seriers of poly(sodiumacrylate-co-acrylamide)(P(AAS-co-AAm)) were synthesized by sodium acrylate andmixture of sodium acrylate and acrylamide through radical polymerization. Thecomposite membranes were developed respectively with the above materials as activelayers and polysulfone (PS) as the supports. ATR-FTIR was employed to characterizethe possible reactions between the gases and the membrane, and the permselectivityof the membrane was measured with CO_2/N2mixed gas. The transport mechanisms ofCO_2and N2in the membrane were hence studied. The effects of AAS content of thepolymer and the wet coating thickness of the active layer on the membranepermselectivity were investigated. The antioxidizability and the acid resistance of thiskind of membrane were verified. The results showed that the membranes possessedgood CO_2separation performance, antioxidizability and acid resistance. In the testswith CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), the membraneprepared by using P(AAS-co-AAm) containing47.68mol%AAS with wet coatingthickness of200μm had a CO_2permeance of163GPU and CO_2/N2selectivity of90at0.11MPa feed pressure.
The method of polymer blending was used to fixed the carboxylate group as thecarrier. The composite membranes were developed with the blend materialPAAS-PEG as the active layers and PS as the supports. The effects of the molecularweight of PEG and the mass ratio of PAAS to PEG on the membrane permselectivitywere investigated. The results showed that the membranes possessed good CO_2separation performance. In the tests with CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), when MWPEGwas20,000，mPAAS:mPEGwas1:2, the PAAS-PEG/PS blend composite membrane had a CO_2permeance of700GPU and CO_2/N2selectivityof80at0.11MPa feed pressure.
Interfacial polymerization (IP) was used to fixed the carboxylate group as thecarrier. The (DAmBS-TMC)/PDMS/PS membrane and(DAmBS-DEGBAmPE-TMC)/PDMS/PS membranes were developed withcrosslinked polydimethylsiloxane (PDMS) coating PS as support membranes,trimesoyl chloride (TMC) as monomer of organic phase, sodium3,5-Diaminobenzoate (DAmBS) or mixture of DAmBS and diethylene glycolbis(3-aminopropyl) ether (DEGBAmPE) as monomers of aqueous phase. The effectsof various parameters on membrane performance were investigated. The resultsshowed that the membranes possessed good CO_2separation performance. Theantioxidizability and the acid resistance of this kind of membrane were verified. Theresults showed that the membranes possessed good CO_2separation performance,antioxidizability and acid resistance. In the tests with CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), the membrane prepared with0.003mol/L of TMC,0.004mol/L of DAmBS and0.006mol/L of DGBAmPE had a CO_2permeance of5831GPU and CO_2/N2selectivity of86at0.11MPa feed pressure.
Taking the (DAmBS-DEGBAmPE-TMC)/PDMS/PS membrane prepared in thiswork for example, the energy and the total cost required for the process werecalculated. The results showed that the membrane prepared in this work wascompetitive with the traditional chemical absorption method, and had a potential to beused for CO_2separation from the flue gas.
用自由基聚合的方法将羧酸根载体引入膜内。以丙烯酸钠为单体，合成聚丙烯酸钠(PAAS)。以PAAS水溶液为涂膜液，聚砜(PS)为支撑层制得PAAS/PS复合膜。用丙烯酰胺(AAm)调节载体含量，制得聚（丙烯酸钠-丙烯酰胺）/聚砜(P(AAS-co-AAm)/PS)复合膜。利用全反射红外光谱(ATR-FTIR)表征了气体组分与膜之间的相互作用，考察了膜的气体透过性能，由此分析了CO_2和N2在膜内的传递机理。研究了AAS含量及湿涂层厚度对膜透过分离性能的影响规律。考察了复合膜的抗氧化和耐酸性能。结果表明，所制膜具有良好的CO_2透过分离性能、抗氧化性和耐酸性。对于CO_2/N2混合气（体积比15/85），AAS含量为47.68mol%，湿涂层厚度为200μm的复合膜在进料气压力为0.11MPa时，CO_2渗透速率为163GPU，分离因子为90。
用共混的方法将羧酸根载体引入膜内。将PAAS与聚乙二醇(PEG)的共混物水溶液涂敷在PS支撑层上制备PAAS-PEG/PS共混复合膜。研究了共混物中PEG分子量以及PAAS/PEG质量比对复合膜CO_2/N2渗透选择性能的影响。结果表明，所制膜具有较高的CO_2透过分离性能，对于CO_2/N2混合气，PEG分子量为20,000，PAAS:PEG质量比为1:2的涂膜液制备的复合膜在进料气压力为0.11MPa时，CO_2渗透速率为700GPU，CO_2/N2分离因子为80。
用界面聚合的方法将羧酸根载体引入膜内。以均苯三甲酰氯(TMC)为有机相单体，二氨基苯甲酸钠(DAmBS)为水相单体，在涂敷了硅橡胶(PDMS)的PS基膜上进行界面聚合制备聚(DAmBS-TMC)/PDMS/PS复合膜。在水相中加入4,7,10-三氧-1,13-癸烷二胺(DEGBAmPE)以调节载体含量及聚合物链段的柔性，从而制备了聚(DAmBS-DEGBAmPE-TMC)/PDMS/PS复合膜。研究了制膜因素对复合膜结构和性能的影响。考察了复合膜的抗氧化性和耐酸性。结果表明，所制膜具有良好的CO_2透过分离性能、抗氧化和耐酸性能。对于CO_2/N2混合气，用0.003mol/L TMC，0.004mol/L DAmBS和0.006mol/L DEGBAmPE所制复合膜在进料气压力为0.11MPa时，CO_2渗透速率为5831GPU，CO_2/N2分离因子为86。
以界面聚合制备的复合膜为例，对烟道气CO_2分离和捕集的过程进行了经济性分析，结果表明，本文制备的CO_2分离膜具有明显的经济优势。
Fixed carrier membranes for CO_2separation are promising membranes. However,most of the fixed carrier membranes contain amine groups as carriers, which may beoxidized by the oxidant gases (mainly O_2) and react with the acidic gas (mainly SO_2)contained in the flue gas. In this work, different methods are used to fixed thecarboxylate group as the carrier in the membrane to get excellent permselectivity,antioxidizability and acid resistance.
The method of the radical polymerization was used to fixed the carboxylate groupas the carrier. Poly(sodium acrylate)(PAAS) and a seriers of poly(sodiumacrylate-co-acrylamide)(P(AAS-co-AAm)) were synthesized by sodium acrylate andmixture of sodium acrylate and acrylamide through radical polymerization. Thecomposite membranes were developed respectively with the above materials as activelayers and polysulfone (PS) as the supports. ATR-FTIR was employed to characterizethe possible reactions between the gases and the membrane, and the permselectivityof the membrane was measured with CO_2/N2mixed gas. The transport mechanisms ofCO_2and N2in the membrane were hence studied. The effects of AAS content of thepolymer and the wet coating thickness of the active layer on the membranepermselectivity were investigated. The antioxidizability and the acid resistance of thiskind of membrane were verified. The results showed that the membranes possessedgood CO_2separation performance, antioxidizability and acid resistance. In the testswith CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), the membraneprepared by using P(AAS-co-AAm) containing47.68mol%AAS with wet coatingthickness of200μm had a CO_2permeance of163GPU and CO_2/N2selectivity of90at0.11MPa feed pressure.
The method of polymer blending was used to fixed the carboxylate group as thecarrier. The composite membranes were developed with the blend materialPAAS-PEG as the active layers and PS as the supports. The effects of the molecularweight of PEG and the mass ratio of PAAS to PEG on the membrane permselectivitywere investigated. The results showed that the membranes possessed good CO_2separation performance. In the tests with CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), when MWPEGwas20,000，mPAAS:mPEGwas1:2, the PAAS-PEG/PS blend composite membrane had a CO_2permeance of700GPU and CO_2/N2selectivityof80at0.11MPa feed pressure.
Interfacial polymerization (IP) was used to fixed the carboxylate group as thecarrier. The (DAmBS-TMC)/PDMS/PS membrane and(DAmBS-DEGBAmPE-TMC)/PDMS/PS membranes were developed withcrosslinked polydimethylsiloxane (PDMS) coating PS as support membranes,trimesoyl chloride (TMC) as monomer of organic phase, sodium3,5-Diaminobenzoate (DAmBS) or mixture of DAmBS and diethylene glycolbis(3-aminopropyl) ether (DEGBAmPE) as monomers of aqueous phase. The effectsof various parameters on membrane performance were investigated. The resultsshowed that the membranes possessed good CO_2separation performance. Theantioxidizability and the acid resistance of this kind of membrane were verified. Theresults showed that the membranes possessed good CO_2separation performance,antioxidizability and acid resistance. In the tests with CO_2/N2mixed gas (containing15vol%CO_2and85vol%N2), the membrane prepared with0.003mol/L of TMC,0.004mol/L of DAmBS and0.006mol/L of DGBAmPE had a CO_2permeance of5831GPU and CO_2/N2selectivity of86at0.11MPa feed pressure.
Taking the (DAmBS-DEGBAmPE-TMC)/PDMS/PS membrane prepared in thiswork for example, the energy and the total cost required for the process werecalculated. The results showed that the membrane prepared in this work wascompetitive with the traditional chemical absorption method, and had a potential to beused for CO_2separation from the flue gas.
引文
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