Radical polymerization of itaconic anhydride and reactions of the resulting polymers with amines and alcohols

Itaconic anhydride was polymerized in the presence of a radical initiator under various conditions. The bulk polymerization at 75°C yielded polymer with molecular weight of more than 20000. The reactions of the resulting polymer with water and alcohols gave poly(itaconic acid) and its esters, respectively. The polymers prepared by such reactions were found to have similar thermal properties to those prepared by homopolymerizations of the respective itaconic acid derivatives. Poly(N-substituted itaconomic acid)s, which are difficult to obtain by direct polymerization of their monomers, were prepared by the reactions of poly(itacononic anhydride) with amines. Copolymerizations of itaconic anhydride with electron-donating monomers, styrene and isobutyl vinyl ether, gave alternating copolymers which were then converted by esterification to the respective copolymers of dialkyl itaconates with such electron-donating monomers.     

水洗法脱除CPP-g-MAH中的聚马来酸酐

用溶液法制备了CPP-g-MAH接枝共聚物,用水洗法脱除了CPP-g-MAH中的副产物——聚马来酸酐,考查了温度对水洗率的影响,证明了水洗法的可行性,并用FT-IR对水洗产物进行了表征。     

水解聚马来酸酐的合成工艺及其性能测试

研究了以水为溶剂,w(H2O2)=30%为引发剂,在自制催化剂作用下,一步合成了水解聚马来酸酐(HPMA),并探讨了水解聚马来酸酐的用量、pH值、硬度、碱度、温度、时间与水解聚马来酸酐对CaCO3阻垢性能的关系。结果表明:该水解聚马来酸酐对CaCO3具有良好的阻垢性能,在pH=6～9,ρ(Ca2 )=250mg/L,ρ(HCO-3)=250mg/L,ρ(HPMA)=0.5mg/L时,阻垢率达99.87%,且具有较好的耐温性和时效性。     

聚马来酸酐的溶解性及与其他树脂相容性研究

聚马来酸酐是聚烯烃、氯化聚烯烃用马来酸酐接枝改性的副产物。研究其基础物性对接枝反应产物的使用和分离具有一定的价值。本文测定了聚马来酸酐在 2 8种溶剂中的溶解性能 ,表明该物质能完全溶解在酮类、醇类、醚类、酯类等极性溶剂中 ,而在非极性的脂肪烃、芳烃类溶剂中不溶。用特性黏度法测定了该聚合物的溶解度参数为 2 2 .10 (J·cm-3 ) 1/2 。用共溶剂法研究了聚马来酸酐与其他树脂的相容性 ,发现该聚合物可以和氨基树脂 ,醇酸树脂 ,聚氨酯 ,丙烯酸树脂等完全相容。     

水解聚马来酸酐的绿色合成研究

以水为溶剂,质量分数30%的过氧化氢为引发剂,NFL4Fe(SO4)2/V2O5/Cr2O3的复配产物为催化剂,m(马来酸酐):m(水):m(过氧化氢)=12:11:9的条件下,控制反应温度85℃,反应3 h.一步合成了水解聚马来酸酐(HPMA).实验结果表明,产品在投加质量浓度为0.5 mg/L时,对CaCO3的阻垢率达99.87%.     

水解聚马来酸酐的绿色合成研究

以水为溶剂,30%的过氧化氢为引发剂,在自制催化剂、m(马来酸酐)∶m(水)∶m(过氧化氢)=12∶11∶9的条件下,控制反应温度85℃,反应3 h,一步合成了水解聚马来酸酐。结果表明,产品在加量为0.5 mg/L时,对CaCO3的阻垢率达99.87%。     

水解聚马来酸酐的最新合成工艺研究

以水为溶剂,30%的过氧化氢为引发剂,NH4Fe(SO4)2/V2O5/Cr2O3为催化剂,m(马来酸酐)∶m(水)∶m(过氧化氢)=12∶11∶9的条件下控制反应温度90℃,反应2 h,一步合成水解聚马来酸酐。实验结果表明,该产品对CaSO4的阻垢效果好,可用作油田注水的阻垢剂。     

水处理剂合成工艺的绿色化研究——水解聚马来酸酐的绿色合成技术

以绿色化学为基础,研究了水解聚马来酸酐(HPMA)的绿色合成工艺,结果表明:以H2O2替代过氧化苯甲酰(BPO)引发剂,用水替代有机溶剂,通过一釜多步串联反应,可实现HPMA的清洁生产,彻底消除传统工艺对环境的污染,采用该工艺合成的产品溴值低,相对分子质量高,阻垢性能好,达到国家优等品标准.     

水解聚马来酸酐的最新合成工艺研究

将顺酐与苯酚室温下混合合成一种电荷转移配合物,然后用此配合物进行聚合反应,采用偶氮二异丁腈为引发剂,在反应温度55℃,反应时间5 h,引发剂用量为7.5%比较缓和的条件下,合成的水解聚马来酸酐(HPMA)对碳酸钙阻垢性能良好,阻垢剂浓度为60 mg/L时,对碳酸钙的阻垢率达到91.25%。     

Preparation of potentially electroactive thallium polymers derived from the acidic copolymers of maleic anhydride

Maleic anhydride copolymers with vinyl ethyl ether and N-vinyl-2-pyrrolidone were prepared in tetrahydrofuran at 60°C, using AIBN as initiator. Copoly (MA-VEE) was hydrolysed to various degrees of hydrolysis and the extent of hydrolysis monitored by i.r. Various acidic derivatives of copoly (MA-VEE), copoly(MA-N-vinyl-2-pyrrolidone) and copoly(MA-ethylene) were prepared and characterized by elemental analysis and spectroscopy. The inter- and intramolecular crosslinking of carboxylic groups in copoly(succinic acid-VEE) were studied by g.p.c. Also thallium (III) derivatives of several acidic polymers were prepared and characterized.     

含膦水解聚马来酸酐的绿色合成研究

探讨了以水为溶剂,以体积分数30%的过氧化氢为引发剂,在催化剂作用下,一步合成含膦水解聚马来酸酐(PHPMA)的最佳条件.实验结果表明,合成含膦水解聚马来酸酐的最佳条件为:m(MA):m(NaH2PO2·H2O)=9:3,V(H2O):V(H2O2)=11:9,反应温度95℃,反应时间3.0 h.在此条件下所得含膦水解聚马来酸酐比水解聚马来酸酐稳定.含膦量低于3%,不会对水体造成污染,所得的产品在加药质量浓度为0.5 mg/L时,阻垢率达97.96%,缓蚀率达83.47%.     

水解聚马来酸酐阻垢性能评价方法的改进和商核

分析了常规的静态阻垢法在阻垢剂阻垢率测定方面存在的片面之处,尝试着改进了该方法结果分析时的钙离子测定过程.以水解聚马来酸酐为阻垢剂进行实验验证,结果表明,此种改进方法使加热前后溶液中钙离子的含量变化反映出的阻垢率更加全面、准确.     

仲醇衍生的表面活性剂

详细论述了仲醇乙氧基化物（SAE）的生产工艺,并说明了其化学特性及物理性质。义中还将SAE的性能与非离子表面活性剂伯醇乙氧基化物（PAE）、壬基酚乙氧基化物（NPE）阴离子表面活性剂十二烷基苯磺酸盐（LAS）进行了比较。对仲醇乙氧基化物在家庭及工业领域内的应用做了介绍。     

低膦水解聚马来酸酐阻垢剂合成研究

以水为溶剂,均相催化引发H2O2产生.OH,合成了低膦水解聚马来酸酐(PHPMA)阻垢剂。研究了原料质量配比、反应温度、催化剂加量、反应时间及阻垢剂加量对阻垢效果的影响。得出最佳合成工艺:m(马来酸酐)∶m(次亚磷酸钠)∶m(引发剂)∶m(水)=12∶4.5∶13∶12,催化剂用量为0.05%,反应时间3 h,温度95℃。PHPMA投加质量浓度为4 mg/L时,其静态阻垢率达99.61%。结果表明,采用均相催化能够合成低膦水解聚马来酸酐高效阻垢剂。     

含膦水解聚马来酸酐对硫酸钙的阻垢性能研究

研究了含膦水解聚马来酸酐(PHPMA)对硫酸钙的阻垢性能,探讨了阻垢剂浓度、pH值、Ca2+浓度、时间、温度等因素对硫酸钙阻垢性能的影响。结果表明,当PHPMA浓度为5 mg/L,Ca2+浓度<3.5 g/L,pH=4~11,时间<30 h,温度<80℃的范围使用时,PHPMA对硫酸钙具有良好的阻垢性能,阻垢率达87%以上。     

Polymer networks derived from the anhydride curing of tetraepoxides

The cure of a technical-grade TGDDM (N,N,N′N′-tetraglycidyl-4,4′-diaminodiphenylmethane) with two different anhydride hardeners (hexahydrophthalic anhydride [HHPA] and tetrahydrophthalic anhydride [THPA]) is reported. The reaction was followed by differential scanning calorimetry (DSC), in situ infrared spectroscopy (FTIR), and viscosity measurements at constant temperature. Onset values of the glass transition temperatures of fully reacted networks under stoichiometric conditions were 206°C with HHPA and 184°C with THPA. THPA was more reactive than was HHPA but it was necessary to heat the mixture above its melting point to generate a homogeneous solution (HHPA remained in solution at room temperature). A first-order kinetics was observed after an induction period necessary to establish a pseudo-steady-state concentration of OH and COOH groups. A catalytic effect of the KBr used in the FTIR measurements was found, in agreement with other authors. Formulations containing an epoxy excess exhibited a higher reactivity due to the increase in the hydroxyl concentration introduced by the epoxy monomer. An increase in the heat of reaction expressed per anhydride equivalent was ascribed to the presence of the epoxy homopolymerization as a side reaction. It was estimated that about 38% of excess epoxy groups over the anhydride groups are homopolymerized in the case of HHPA and 17% in the case of THPA. Full conversions of both epoxy and anhydride groups are obtained for formulations with stoichiometric ratios, r (anhydride/epoxy groups) = 0.72 in the case of HHPA and 0.85 in the case of THPA. These values are in the range where the maximum glass transition temperature has been reported for epoxy-anhydride formulations. © 1997 John Wiley & Sons, Inc. J Appl Polym Sci 64: 157–166, 1997     

Heterocyclic compounds derived from aliphatic amines

The photolytic rearrangement of N-chloroamines derived from secondary fatty amines, such as N-methyloctadecylamine, has been investigated. The intermediate δ- or ε-chloroamines, or both, were not isolated from the reaction medium but were converted directly to their corresponding N-methyl-2-alkylpyrrolidine or piperidine analogs, or both, by treatment with alkali. The synthetic utility of this reaction has been extended to include the two functionally substituted secondary amines, N,N-dimethylazelaylamine and methyl 11-methylaminoundecanoate. The yields of isolated pure products are in the range of 50–80%. Presented at the AOCS Meeting, New York, October, 1968. ARS, USDA.     

Studies of reactions with polymers. I. The reaction of maleic anhydride with PVA and the properties of the resultant

Graft copolymerization of maleic anhydride (MA) onto PVA was carried out both in the presence and absence of the initiator. In the former case, the resultant was a copolymer containing a carboxylic acid and a keto-olefinic side chain. Therefore, the reaction product, viscosity, gel content, and mechanical properties differed from the resultant of the latter, which was obtained by esterification of PVA by MA. Both resultants showed polyelectrolytes characteristics. The dependence of the grafting percentage on the concentration of the initiator, the concentration of the monomer, the reaction temperature, and the reaction medium was studied. Grafted copolymers after heat treatment showed remarkable mechanical strength in the wet state when compared with original PVA.     

On the reaction of (S)-trifluoroacetoxysuccinic anhydride with amines to produce hydroxysuccinamic (malamic) acid derivatives

L-Malic acid ( 2 ) reacts with trifluoroacetic anhydride under anhydrous conditions to give (S)-trifluoroacetoxy-succinic acid anhydride ( 3 ). The anhydride 3 undergoes regioselective ring opening with an excess of anilines or primary aliphatic amines leading to N-substituted-(S)-3-hydroxy-succinamic acids ( 4a – g ). Structural elucidation of the reaction products 4a – g was based on analytical and spectroscopic data and on an X-ray structure analysis of 4b . Secondary aliphatic amines react with 3 by condensation and subsequent elimination to furnish N,N′-disubstituted fumaric acid amides 5a , b . Some N-substituted-2-hydroxysuccinamic acids ( 7a , b ) were also prepared for spectral comparison with the 3-hydroxy compounds.