CO_2刺激响应吸油树脂的制备及其可控油-水吸附性能

以2,3-二溴-1,4-丁二醇为主体,在碱性条件下与二乙胺反应制备含胺基可交联烯烃单体,然后与苯乙烯通过悬浮聚合得到含胺基苯乙烯交联共聚物吸油树脂。对产物进行了测试与表征,并对其进行了吸油性能测试和CO_2刺激响应测试。结果表明:制备了多孔结构微球,产物结构与预期一致,所得吸油树脂对甲苯具有一定的吸附性,其饱和吸附率为1.11 g/g;吸油树脂吸附甲苯后在CO_2作用下,胺基完成了亲油-亲水的转变并释放所吸附甲苯,脱附率为82.3%。     

典型液体危化品吸附材料性能

目前用于典型液体危化品吸附的材料类型主要有树脂型和有机高聚物超细纤维型,两种类型中分别选取甲基丙烯酸酯吸油树脂和聚丙烯纤维吸附材料,对此两种吸附材料的吸附相关特性进行了对比实验研究,包括吸附倍率与时间的关系、吸附选择性以及循环吸附/解吸特性等。结果表明,两种吸附材料吸附甲苯的吸附平衡时间均为4 s左右,其中聚丙烯纤维吸附材料的平衡吸附倍率为17.82 g/g,为甲基丙烯酸酯吸油树脂的2.2倍;两种吸附材料都具有较好的吸附选择性;聚丙烯纤维吸附材料在吸附甲苯后能够通过挤压方式解吸附实现循环使用,平均解吸率在80%以上;甲基丙烯酸酯吸油树脂在吸附甲苯后无法通过挤压方式进行解吸附。实验结果将为基于吸附材料的水面液体危化品回收设备的研发奠定基础。     

多元共聚高吸油树脂合成及性能研究

以(甲基)丙烯酸酯类、苯乙烯为主要共聚单体,双甲基丙烯酸乙二醇酯(EGDMA)、二乙烯基苯(DVB)等为交联剂,采用悬浮共聚工艺合成了一系列高吸油树脂.研究了树脂共聚单体组成、丙烯酸单体链长、交联剂种类、交联度、引发剂量以及聚合工艺等因素对吸油树脂吸油量等性能的影响.结果表明:采用EGDMA交联时以丙烯酸十四酯的效果最佳,采用DVB交联时以丙烯酸十二酯效果最佳;交联剂种类及交联度大小对树脂吸油性能及树脂形态有明显影响;树脂交联度的大小明显影响树脂共聚物的转化率与可溶性分率,也明显影响树脂产品的收率.在最佳合成条件下制备的高吸油树脂具有较佳的吸油性能,对甲苯的吸附量可达17.32 g/g树脂.     

DDMA/S树脂的合成及吸油性能

以甲基丙烯酸十二酯(DDMA)和苯乙烯(S)为单体,采用悬浮聚合法合成了DDMA/S树脂,利用FTIR对合成树脂进行结构表征,测试了树脂的吸油性能。结果发现,该类树脂的吸油能力随着树脂中DDMA含量增加而增加,对油品的吸油能力为甲苯汽油柴油豆油,当DDMA/S树脂单体组成为2∶3时,对甲苯和汽油的吸油率分别为9.5386 g/g和7.0153g/g,并对不同油品的吸油能力进行了讨论。     

P(BMA/2-EHM/St)高吸油树脂的微波合成

以BMA、2-EHM和St为合成原料,BPO为引发剂,DVB为交联剂,PVA为分散剂,在微波辐射条件下合成了P(BMA/2-EHM/St)高吸油树脂。主要探讨了微波功率、反应温度和反应时间对高吸油树脂吸油倍率的影响。结果表明:当微波功率700W,聚合温度80℃,反应时间70min时,所制得高吸油树脂对甲苯的吸收倍率可达到18. 84g/g。     

沉淀白炭黑表面改性工艺研究

采用正辛醇对沉淀白炭黑进行改性,通过正交实验讨论温度、改性剂用量、改性时间等对沉淀白炭黑活化度、吸油值、沉降体积的影响。通过数据处理,综合分析得出正辛醇改性该沉淀白炭黑的优化工艺条件:改性温度为80℃,改性时间为50 min,每10 g SiO2的改性剂正辛醇用量为40 mL、溶剂甲苯为10 mL、催化剂对甲苯磺酸为2.0 g。在该改性条件下,改性后的沉淀白炭黑产品活化度为91.0%、吸油值为2.80 mL/g、沉降体积为4.10 mL/g。改性白炭黑与胶料的相容性明显提高。     

EPDM-DVB-α-MSt新型高吸油树脂的制备

以三元乙丙橡胶(EPDM)、α-甲基苯乙烯(α-MSt)为单体,二乙烯基苯(DVB)为交联剂,过氧化二苯甲酰(BPO)为引发剂,甲苯、环己烷为致孔剂,明胶、磷酸三钙为分散剂,采用悬浮聚合法合成了高吸油树脂。利用傅里叶变换红外光谱仪、热重分析仪、扫描电子显微镜等研究了吸油树脂的结构、吸油倍率、饱和吸油时间、吸油树脂重复使用后的二次饱和吸油倍率以及吸油前后的内部形态。结果表明:m(α-MSt)/m(EPDM)为4:6,DVB和BPO用量均为1 g,溶剂甲苯与环己烷体积比为4:1,明胶与磷酸三钙的质量比为2:1,搅拌速率为500 r/min,水油体积比为5:1时,吸油树脂对柴油的吸油倍率最高为11.5 g/g,吸油饱和时间最短为3天;吸油树脂经乙醇萃取后反复使用,饱和吸油倍率几乎不变;吸油树脂内部存在分布不均的网孔结构。     

熔体微分电纺PLA/ATBC纳米纤维膜吸油性能

静电纺丝制备的纳米纤维孔隙率高、吸附能力强,可用于高效地处理化工行业油污染问题。聚乳酸（PLA）作为生物可降解材料,来源广泛且不会造成二次污染,具有广阔的应用前景。本文利用自制的熔体微分电纺装置,制备了PLA/乙酰基柠檬酸三丁酯（ATBC）纤维膜,探究了物料性质和增塑剂ATBC含量对PLA纤维形貌及吸油性能的影响,并获得了最佳的纺丝温度和ATBC含量。研究表明,在纺丝温度为240℃、ATBC质量分数为10%时制备的纤维直径为320nm。该纤维膜水接触角为145°,表现出良好的疏水性能,吸油倍率为138.4g/g,是市售PP无纺布吸油性能的4～5倍,保油倍率为85.8g/g。重复吸/放油5次循环后,纤维膜仍具有良好的强度而未发生断裂且可继续进行吸油,重复使用性能较好,可被应用于化工行业油污染处理。     

一种高吸油性树脂的合成工艺及性能研究

采用悬浮聚合法,以水为分散相,甲基丙烯酸十二酯(DMA)为长链单体,苯乙烯(St)为短链单体,二乙烯基苯(DVB)为交联剂,过氧化苯甲酰(BPO)为引发剂,合成了低交联度的高吸油性树脂,研究了单体配比、引发剂用量、交联剂用量对树脂性能的影响,测定了树脂的DSC-TG曲线,以及树脂吸油前后的SEM形貌表征。结果表明:合成的高吸油性树脂吸油效果较为理想,其中对甲苯的吸收倍率可达到7.03g/g,煤油的吸收倍率可达到6.59g/g,航空煤油的吸收倍率可达到6.12g/g,并且树脂具有良好的热稳定性。     

聚甲基丙烯酸十六酯的合成及其吸油性

以甲基丙烯酸、十六醇为反应物,对甲苯磺酸为催化剂,对苯二酚为阻聚剂合成了甲基丙烯酸十六酯。以N,N'-亚甲基双丙烯酰胺为交联剂,偶氮二异丁腈为引发剂,通过溶液聚合得到聚甲基丙烯酸十六酯树脂。以树脂吸收甲苯的质量为考察指标得出最佳合成条件:交联剂用量为0.8 phr,引发剂用量为1.0 phr,反应温度为80℃。此条件下得到的树脂吸油倍率可达14.1g/g。树脂经过甲苯洗涤后的二次吸油倍率可提高到21.4g/g,吸油速率变化不大。傅里叶变换红外光谱分析表明,树脂中不再含有单体中的碳碳双键。     

Saline solution absorbency and structure study of poly (AA-AM) water superabsorbent by inverse microemulsion polymerization

A series of novel copolymer superabsorbents based on acrylamide (AM), acrylic acid(AA) were prepared by inverse microemulsion copolymerization using ammonium persulfate (APS) as the initiator and N,N-methylenebisacrylamide (MBA) as the crosslinking agent and OP-10 and SDS as complex surfactants. The synthetic variables (amount of crosslinking agent and initiator, water/oil ratio, monomer/surfactant ratio and AA/ Am ratio) and their effects on the absorbencies of the synthesized superabsorbents were investigated. The experimental results of superabsorbent polymers (SAPs) showed the maximum saline solution absorbency of 130 g/g within 75 min, and the saline solution absorbency of 111 g/g within 30 min. FTIR indicated the structure of the acrylic acid and acrylamide copolymer. SEM indicated that the particles prepared with higher crosslinker content (0.03%) showed smaller pore sizes and less porous structures compared with those with less crosslinker content (0.01%) and the number of the micropores largely decreased with the water/oil ratio increasing from 8% to 14%.     

丙烯酰胺/甲基丙烯酸丁酯改性纤维素的研究

以纤维素为基体,丙烯酰胺(AM)、甲基丙烯酸丁酯(BMA)为接枝单体,过硫酸钾为引发剂,N,N'-亚甲基双丙烯酰胺为交联剂,聚乙烯吡咯烷酮为分散剂,通过悬浮接枝聚合法制备出了纤维素基吸水吸油材料;考察了单体用量、引发剂用量、反应时间、反应温度及交联剂用量等因素对接枝聚合物的吸水、吸油性能的影响。结果表明:在单体与纤维素的质量比为3.0∶1.0,AM∶BMA的质量比为2.0∶1.0,相对于单体,引发剂质量分数为6.0%,交联剂质量分数为0.5%,分散剂质量分数为0.5%,反应温度为70℃,反应时间为4 h的条件下,得到纤维素-AM-BMA接枝共聚物,其吸油倍率为11.55 g/g,吸水倍率为23.51 g/g,聚合度为534.6。     

环境友好型聚天冬高吸水性树脂的合成

以可生物降解的高分子材料聚琥珀酰亚胺为原料,二胺为交联剂,合成了环境友好型聚天冬高吸水性树脂。考察了原料分子量、交联剂种类、交联剂用量、吸水温度以及吸水时间等对树脂吸水倍率的影响。结果表明,交联剂用量显著影响树脂的吸水倍率,以分子量为67500的聚琥珀酰亚胺为原料,己二胺为交联剂,交联剂浓度为1.5%时,树脂吸水倍率为1480。     

A novel polyacrylamide‐based superabsorbent with temperature switch for steam breakthrough blockage

A novel high‐temperature resistant superabsorbent polymer (SAP) with a temperature switch to control its water absorbency was prepared through solution polymerization of acrylamide (AM), using N,N‐methylenebisacrylamide (NMBA) and tetraallylammonium chloride (TAAC) as crosslinking agents. The SAPs were structurally characterized by Fourier transform infrared (FTIR) spectroscopy and energy dispersive X‐ray spectroscopy (EDX). The factors that influence the water absorbency such as total crosslinker concentration, molar ratio of NMBA to TAAC and temperature were investigated. The SAP with optimized crosslinker concentration showed a swelling ratio less than 10 g/g at 25°C, and drastically enhanced water absorption capacity (190 g/g) at 300°C. The water absorption characteristics can be tuned by varying the temperature. Swelling experimental results combined with crosslinking density study and morphology observation by scanning electron microscopy (SEM) clearly demonstrated that the hydrolysis of amide bonds on NMBA played a critical role in creating these previously unreported SAPs, and that the use of TAAC with an appropriate amount rendered the SAPs high‐temperature resistance. This kind of SAPs has high application potentials as plugging material for steam breakthrough and channeling in heavy oil reservoirs. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42067.     

Research on butyl methacrylate–lauryl methacrylate copolymeric fibers for oil absorbency

By adding hydroethyl methacrylate as potential crosslinker, the butyl methacrylate‐lauryl methacrylate copolymeric (CPMA) fibers with oil‐absorptive function were prepared using heat crosslinking technology after spinning. The effect of monomer feed ratio showed that by controlling the monomer ratio, crosslinker concentration, and crosslinking conditions, the maximum absorbencies of prepared fibers to different oil were 8 g (kerosene)/g (fiber), 15 g (toluene)/g (fiber), and 34.75 g (chloroform)/g (fiber). The structures of fibers were characterized by FTIR, DSC, and SEM. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 101: 1248–1251, 2006     

Swelling and network parameters of high oil‐absorptive network based on 1‐octene and isodecyl acrylate copolymers

Crosslinked 1‐octene‐isodecyl acrylate copolymers were synthesized and evaluated for oil‐absorbency applications. The copolymer was crosslinked at different concentrations of ethylene glycol diacrylate (EGDA) and EG dimethacrylate (EGDMA) crosslinkers via catalytic initiation or by electron‐beam irradiation at a dose rate 80 kGy. The concentration of both crosslinkers was varied from 0.5 to 2%. The effects of the crosslinking conditions such as crosslinker concentration, method of polymerization and monomer concentrations on the conversion and gel fraction were examined through oil‐ absorption tests using petroleum crude oil. It was found that the oil absorbency was influenced mainly by the degree of crosslinking and the hydrophobicity of the copolymer units. The final equilibrium oil content, volume fraction of the polymer, and swelling capacity were determined at 298 K. The effective crosslinking density, average molecular weight between the crosslinks, and polymer–toluene interaction parameter were determined from stress–strain measurements. The crosslinking efficiencies of EGDA and EGDMA toward copolymers were determined. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 97: 80–91, 2005     

Synthesis and properties of oil absorption resins filled with polybutadiene

Polybutadiene (PB) is used to fill an oil absorption resin as a physical crosslinker to construct a kind of 3‐dimensional network with a high degree crosslinking and low crosslink density. A series of acrylic resin particles with various compositions are prepared by suspension polymerization, using benzoyl peroxide (BPO) as an initiator and ethylene glycol dimethacrylate (EGDMA) as a chemical crosslinker. The effects of the polymerization temperature, initiator concentration, monomer feed ratio, and chemical and physical crosslinker concentrations on the oil absorbency and gel fraction (degree of crosslinking) are studied. The recipe and operation conditions are optimized as follows: a mass ratio of 3:1 for styrene (St)/dodecyl methacrylate or St/butyl acrylate, 0.5 wt % BPO, and 80°C for 7–8 h. The effect of the physical crosslinker (PB) concentration is complex. The oil absorbency increases with increasing PB at lower EGDMA concentrations. However, under this same condition, particles cannot be formed if the PB concentration is higher than a certain value. By contrast, there is an optimum PB concentration when the EGDMA concentration is higher. The oil absorption speed is also investigated. The presence of PB can speed up absorption. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 89: 3309–3314, 2003     

丙烯酸-丙烯酰胺共聚物/聚乙烯醇高吸水纤维研制

采用潜交联剂丙烯酸羟丙酯与丙烯酸、丙烯酰胺等单体共聚后与聚乙烯醇共混配制成纺丝原液, 湿法纺丝成形后经后交联处理赋予纤维三维网状结构,制得具有较好吸水性能的丙烯酸-丙烯酰胺共聚物/ 聚乙烯醇共混纤维,研究了后交联处理条件对纤维结构及性能的影响。结果表明,随着交联温度的升高,交联时间的延长,纤维的饱和吸水率降低。纤维经130℃交联处理12 min后,其饱和吸水率可达405 g/g。     

An efficient preparation method for superabsorbent polymers

High water‐absorbent polyacrylates could be prepared by concentrated aqueous solution polymerization within a short time period, heating the monomer mixture by water bath. The influences of initiator content, bath temperature, crosslinker content (Cc), and degree of neutralization on water absorbency (Q) were investigated. The temperature changing of the monomer mixture during polymerization was thoroughly analyzed. The increase of initiator content as well as the increase of bath temperature results in the increase of water absorbency and reduces the crosslinking efficiency. The results are in conformity with Flory's network theory and also illustrate that lower crosslinking efficiency occurs when the polymerization rate is faster. An empirical relation of Q = 1.40 Cc^−0.665 is obtained and its exponent is very close to −0.6 in a derived relation. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 74: 119–124, 1999     

真空制备木薯淀粉超吸水材料

采用真空技术成功制备了一种木薯淀粉（CS）-g-丙烯酸（AA）超吸水材料。在AA与cS质量比2．5：l,过硫酸钾0．07g,30％wt氢氧化钠水溶液中和度（摩尔比）20％,N,N’-弧甲基双丙烯酰胺0．14％（占AA重）条件下,65℃真空恒温反应3h,干燥后得超吸水材料（cs．SAP）。一定温度湿度条件下,不同形状CS—SAP吸液能力及保水性能有一定差别,保留4％凝胶残重的材料保水时间最长可达28d：材料吸去离予水倍率高达1316．8（g／g）、自来水673．1（g／g）、0．9％NaCI水溶液54．8（g／g）、人工尿液63．0（g／g）。接枝反应及材料吸水结构经FTIR．SEM,PM表征。