低成本改性PAE树脂的制备及应用研究
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摘要
聚酰胺多胺环氧氯丙烷树脂简称PAE树脂，在用作纸张增强剂中属于一种环保型树脂，目前使用比较广泛，它的优点在于产品中不含游离甲醛，对环境和人体污染较小，在造纸行业中具有良好的应用价值。本文在前人工作的基础上采用熔融缩聚法，利用低成本原料对PAE树脂进行改性，所得产品的性能优良，便于使用。
实验所用的原料为环氧氯丙烷、二乙烯三胺、己二酸和尿素，采用熔融缩聚法制备出改性的PAE树脂。研究了反应时间、反应温度、原料配比等因素对中间体（PPC）黏度的影响，探讨了胺值、酸值以及最终产物的黏度受反应过程中各种因素的影响，同时考察了各因素对产物中有机氯含量及稳定性的影响及改性树脂添加量对纸张抗张效果的影响。结果表明，当己二酸和二乙烯三胺之间的摩尔比为1:1.05，合成中间体反应温度为180℃，反应时间为210min时所得聚合产物的酸值为20.10%；选择脱氨化反应较佳温度为125℃，时间为4h时所得产物的胺值为42.40%；交联化反应中温度为80℃，时间为60min时所得最终产物的黏度为993mPa·s。有机氯含量为0.95%，产品最终固含量为12.50%，pH值为3.0~4.5；制备的改性PAE添加量为绝干浆的1.20%~1.40%时，湿强度最高可达35.60%。采用红外、热重、扫描电镜等对产物的结构及热稳定性等进行了分析。
用熔融缩聚法以二乙烯三胺、己二酸、环氧氯丙烷和乙醇胺为原料制备出改性PAE树脂。研究了反应时间、反应温度、原料配比等因素对中间体（PPC）黏度、胺值、酸值以及最终产物黏度的影响，同时考察了各因素对产物中有机氯含量、稳定性等的影响，探讨了改性树脂添加量对纸张抗张效果的影响。结果表明，当二乙烯三胺、己二酸、乙醇胺的比例为7:10:3，合成中间体反应温度为170℃，反应时间为160min时所得聚合产物的酸值为28.21%；脱氨化反应较佳温度为125℃,时间为4h，所得产物的胺值为43.79%；交联化反应中温度为80℃，时间70min，所得最终产物的黏度为984mPa·s。有机氯含量为1.16%，产品最终固含量达12.50%，pH值为3.0~4.5，制备的改性PAE添加量为绝干浆的1.40%~1.60%时，湿强度最高可达25.80%。采用红外、热重、扫描电镜对产物进行了结构及性能分析。
Polyamide polyamine epichlorohydrin is shorted as the PAE resin,which isthe most widely used environment-friendly paper reinforcing agent resin. Itsadvantage is that not containing harmful formaldehyde to have a good value inthe paper industry, on the basis of previous work,This paper use the meltpolycondensation method and low-cost materials to modify the PAE resin, theresult shows that the product has excellent performance and ease of use.
The modified PAE resin was prepared by diethylenetriamine, adipic acid,epichlorohydrin and urea as raw materials with melt polycondensationmethod.The effects of reaction time, reaction temperature, the ratio of rawmaterials to the intermediates’ viscosity (PPC)were studied, and the impact ofthe reaction of various factors on the viscosity of the amine value, acid value,and the final product were also studied, meanwhile the impact of various factorson the organochlorine content and the stability of the product was investigatedand finally the impact of the modified resin content on the paper tensile effectswas investigated. When the ratio of diethylenetriamine and adipic acid is1.05:1,the reaction temperature is180℃, the reaction time is210min that the syntheticintermediate polymers’ acid value is20.10%; when the de-ammoniation reactiontemperature is125℃,reaction time4h for the product amine value is42.40%;when the crosslinking reaction temperature is80℃the reaction time is60minthat the viscosity of the final product is993mPa s and the percent of organicchlorine is0.95%, the final solid content of product is12.50%, the pH value ofproduct is3.0~4.5, the wet strength value reached to35.60%when thepreparation of modified PAE dosage is from1.20%to1.40%for dry pulp, finallythe structure of the producrt was analyzed by using infrared spectrum,thermogravimetric analysis and scanning electron microscopy (SEM)were alsoused to know the stability and the surface structure of the product.
The modified PAE resin was prepared by diethylenetriamine, adipic acid,epichlorohydrin and ethanolamine as raw materials with melt polycondensation method The effects of reaction time, reaction temperature, the ratio of rawmaterials to the intermediates’ viscosity (PPC)were studied, and the impact ofthe reaction of various factors on the viscosity of the amine value, acid value,and the final product were also studied, meanwhile the impact of various factorson the organochlorine content and the stability of the product were investigatedand finally the impact of the modified resin content on the paper tensile effectswere investigated. When the ratio of diethylenetriamine and adipic acid andethanolamine is7:10:3, the reaction temperature is170℃, the reaction time is160min that the synthetic intermediate polymers’ acid value is28.21%; when thede-ammoniation reaction temperature is125℃and the reaction time is4h for thevalue of product amine is43.79%; when the crosslinking reaction temperature is80℃the reaction time is70min that the viscosity of the final product is984mPa s and the percent of Organic chlorine is1.16%, the final solid content ofproduct is12.50%, the pH value of product is3.0~4.5, the wet strength valuereached to25.80%when the preparation of modified PAE dosage wasfrom1.40%increased to1.60%for dry pulp, finally the structure of the producrtwas analyzed by using infrared spectrum, thermogravimetric analysis andscanning electron microscopy (SEM)were also used to know the stability and thesurface structure of the product.
实验所用的原料为环氧氯丙烷、二乙烯三胺、己二酸和尿素，采用熔融缩聚法制备出改性的PAE树脂。研究了反应时间、反应温度、原料配比等因素对中间体（PPC）黏度的影响，探讨了胺值、酸值以及最终产物的黏度受反应过程中各种因素的影响，同时考察了各因素对产物中有机氯含量及稳定性的影响及改性树脂添加量对纸张抗张效果的影响。结果表明，当己二酸和二乙烯三胺之间的摩尔比为1:1.05，合成中间体反应温度为180℃，反应时间为210min时所得聚合产物的酸值为20.10%；选择脱氨化反应较佳温度为125℃，时间为4h时所得产物的胺值为42.40%；交联化反应中温度为80℃，时间为60min时所得最终产物的黏度为993mPa·s。有机氯含量为0.95%，产品最终固含量为12.50%，pH值为3.0~4.5；制备的改性PAE添加量为绝干浆的1.20%~1.40%时，湿强度最高可达35.60%。采用红外、热重、扫描电镜等对产物的结构及热稳定性等进行了分析。
用熔融缩聚法以二乙烯三胺、己二酸、环氧氯丙烷和乙醇胺为原料制备出改性PAE树脂。研究了反应时间、反应温度、原料配比等因素对中间体（PPC）黏度、胺值、酸值以及最终产物黏度的影响，同时考察了各因素对产物中有机氯含量、稳定性等的影响，探讨了改性树脂添加量对纸张抗张效果的影响。结果表明，当二乙烯三胺、己二酸、乙醇胺的比例为7:10:3，合成中间体反应温度为170℃，反应时间为160min时所得聚合产物的酸值为28.21%；脱氨化反应较佳温度为125℃,时间为4h，所得产物的胺值为43.79%；交联化反应中温度为80℃，时间70min，所得最终产物的黏度为984mPa·s。有机氯含量为1.16%，产品最终固含量达12.50%，pH值为3.0~4.5，制备的改性PAE添加量为绝干浆的1.40%~1.60%时，湿强度最高可达25.80%。采用红外、热重、扫描电镜对产物进行了结构及性能分析。
Polyamide polyamine epichlorohydrin is shorted as the PAE resin,which isthe most widely used environment-friendly paper reinforcing agent resin. Itsadvantage is that not containing harmful formaldehyde to have a good value inthe paper industry, on the basis of previous work,This paper use the meltpolycondensation method and low-cost materials to modify the PAE resin, theresult shows that the product has excellent performance and ease of use.
The modified PAE resin was prepared by diethylenetriamine, adipic acid,epichlorohydrin and urea as raw materials with melt polycondensationmethod.The effects of reaction time, reaction temperature, the ratio of rawmaterials to the intermediates’ viscosity (PPC)were studied, and the impact ofthe reaction of various factors on the viscosity of the amine value, acid value,and the final product were also studied, meanwhile the impact of various factorson the organochlorine content and the stability of the product was investigatedand finally the impact of the modified resin content on the paper tensile effectswas investigated. When the ratio of diethylenetriamine and adipic acid is1.05:1,the reaction temperature is180℃, the reaction time is210min that the syntheticintermediate polymers’ acid value is20.10%; when the de-ammoniation reactiontemperature is125℃,reaction time4h for the product amine value is42.40%;when the crosslinking reaction temperature is80℃the reaction time is60minthat the viscosity of the final product is993mPa s and the percent of organicchlorine is0.95%, the final solid content of product is12.50%, the pH value ofproduct is3.0~4.5, the wet strength value reached to35.60%when thepreparation of modified PAE dosage is from1.20%to1.40%for dry pulp, finallythe structure of the producrt was analyzed by using infrared spectrum,thermogravimetric analysis and scanning electron microscopy (SEM)were alsoused to know the stability and the surface structure of the product.
The modified PAE resin was prepared by diethylenetriamine, adipic acid,epichlorohydrin and ethanolamine as raw materials with melt polycondensation method The effects of reaction time, reaction temperature, the ratio of rawmaterials to the intermediates’ viscosity (PPC)were studied, and the impact ofthe reaction of various factors on the viscosity of the amine value, acid value,and the final product were also studied, meanwhile the impact of various factorson the organochlorine content and the stability of the product were investigatedand finally the impact of the modified resin content on the paper tensile effectswere investigated. When the ratio of diethylenetriamine and adipic acid andethanolamine is7:10:3, the reaction temperature is170℃, the reaction time is160min that the synthetic intermediate polymers’ acid value is28.21%; when thede-ammoniation reaction temperature is125℃and the reaction time is4h for thevalue of product amine is43.79%; when the crosslinking reaction temperature is80℃the reaction time is70min that the viscosity of the final product is984mPa s and the percent of Organic chlorine is1.16%, the final solid content ofproduct is12.50%, the pH value of product is3.0~4.5, the wet strength valuereached to25.80%when the preparation of modified PAE dosage wasfrom1.40%increased to1.60%for dry pulp, finally the structure of the producrtwas analyzed by using infrared spectrum, thermogravimetric analysis andscanning electron microscopy (SEM)were also used to know the stability and thesurface structure of the product.
引文
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[3] Birt K W.Some observations on wet-paper[J].Ind.Paper World,1944,26(1):37-46．
[4]杨开吉，苏文强，沈静．造纸湿强剂的作用机理及进展[J]．造纸科学与技术，2006，2（25）：58-62．
[5]沈一丁，彭晓凌．聚酰胺多按环氧氯丙烷的改性及应用进展[J]．中国造纸，2005，24（4）：55-58．
[6] D.布劳恩，H.切尔德龙，W．克恩著,黄葆国等译.聚合物合成和表征技术[M]．北京:科学出版社，1981:265-267．
[7]张庆余，韩孝族，纪奎江．低聚物[M]．科学出版社，1994．
[8]林冶宪．增湿强剂的强度呈现机理及其应用[J]．天津造纸，2002：31-33．
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