CN108219443A - 一种盾构管片中空密封条充填用的聚氨酯弹性体及其制备方法 - Google Patents
一种盾构管片中空密封条充填用的聚氨酯弹性体及其制备方法 Download PDFInfo
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- CN108219443A CN108219443A CN201810006146.5A CN201810006146A CN108219443A CN 108219443 A CN108219443 A CN 108219443A CN 201810006146 A CN201810006146 A CN 201810006146A CN 108219443 A CN108219443 A CN 108219443A
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- Prior art keywords
- polyurethane elastomer
- plasticizer
- component
- polyalcohol
- sealing strip
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Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
本发明涉及一种盾构管片中空密封条充填用的低硬度聚氨酯弹性体的制备方法,由以下(A)(B)(C)(D)四种成份采用半预聚体法聚合反应而成,该弹性体可在压力装置下填充到盾构管片中空密封条中固化成聚氨酯弹性体,替代水泥填充或微孔聚氨酯弹性体填充。其中(A)是端羟基聚醚二元醇或多元醇,(B)是多异氰酸酯,(C)是低分子多元醇、醇类及胺类扩链剂及交联剂,(D)是增塑剂、催化剂。本发明具有硬度范围广、力学性能好、无增塑剂析出、密封性能和老化性能优异等特点。
Description
技术领域
本发明涉及一种盾构管片中空密封条充填用的聚氨酯弹性体的制备方法,特别是一种具有硬度范围广、力学性能好、无增塑剂析出、密封性能好、老化性能好等特点,主要用于盾构管片中空密封条充填用的聚氨酯弹性体,尤其突出的案例是在隧道建造过程中,填充到盾构管片的中空密封条中固化成聚氨酯弹性体,替代水泥或微孔弹性体填充,形成一种密封性优异的新的填充材料。
背景技术
盾构管片是盾构施工的主要装配构件,是隧道的最内层屏障,承担着抵抗土层压力、地下水压力以及一些特殊荷载的作用。盾构管片是盾构法隧道的永久衬砌结构,盾构管片质量直接关系到隧道的整体质量和安全,影响隧道的防水性能及耐久性能。
盾构管片的生产通常采用高强抗渗混凝土,以确保可靠的承载性和防水性能,生产主要利用成品管片模具在密封浇灌混凝土后即可成型。盾构推进结束后,一般采取错缝拼接迅速拼装管片成环。盾构管件表面附有环形沟槽,环形沟槽上会嵌合中空的密封条,中空密封条内部会填充材料,以保证盾构管片的承载性、密封性和防水性。现有的水泥填充材料虽也能起到一定的支撑和填充作用,但存在固化后密封不严的缺陷;微孔聚氨酯弹性体填充材料不仅生产加工过程较复杂,无法保证在中空密封条中泡孔均匀一致,发泡体不能与密封条处处紧密接触,且泡孔在负荷作用下容易压扁,载荷性能下降的同时也会影响到密封性;另外还存在发泡受温度限制等缺点。因此,急需提供一种盾构管片中空密封条充填用材料,克服水泥填充材料和微孔聚氨酯弹性体填充材料的缺陷。
发明内容
本发明的目的是提供一种可用于盾构管片中空密封条充填用的硬度范围广、力学性能好、密封性能和老化性能优异的聚氨酯弹性体材料的制备方法。
本发明的目的是这样实现的:一种可用于盾构管片中空密封条充填用的聚氨酯弹性体材料,由以下(A)(B)(C)(D)四种主要成份采用半预聚体法聚合反应而成,其中:
(A)端羟基聚醚二元醇或多元醇,是由环氧丙烷、环氧乙烷、四氢呋喃、甘油、乙二醇、三羟甲基丙烷中一种以上成分聚合成聚醚二醇或多元醇。
(B)多异氰酸酯,是甲苯二异氰酸酯(TDI-65、TDI-80、TDI-100)、二苯基甲烷二异氰酸酯(纯MDI、液化改性MDI)、多苯基甲烷多异氰酸酯(PAPI)中的一种或两种以上混合物。
(C)低分子多元醇、二醇类及胺类扩链剂或交联剂,所述扩链剂或交联剂为3,3′-二氯-4,4′-二氨基二苯基甲烷(MOCA)、2,4-(2,6-)二氨基-3,5-甲硫基甲苯(DMTDA)、2,4-(2,6-)二氨基-3,5-乙基甲苯(DETDA)、2,4-(2,6-)二氨基-3,5-甲硫基氯苯、2,4-(2,6-)二氨基-3,5-甲硫基乙苯、乙二醇(EG)、1,4-丁二醇(BD)、二甘醇(DEG)、三羟甲基丙烷(TMP)、三异丙醇胺(TIPA)、三乙醇胺(TGA)、二甲硫基氯苯二胺(HC-600)、对苯二酚双-β-羟乙基醚(HQEE)、间苯二酚双-β-羟乙基醚(HER)中的一种以上成分。
扩链剂优选采用乙二醇(EG)与HC-600(二甲硫基氯苯二胺)或MOCA与三羟甲基丙烷并用,两种扩链剂的比例优选为20:80。
(D)增塑剂,所述增塑剂为邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二甲氧乙基酯(DMEP)、邻苯二甲酸二异癸酯(DIDP)、氯化石蜡、石蜡油、芳烃油、溶剂油中的一种或两种以上的混合物。
增塑剂优选为DOP与氯化石蜡并用,优选以7:3的比例复配。
还可以加入催化剂,所述催化剂为二月桂酸二丁基锡、辛酸亚锡、异锌酸铅、异锌酸锌中的一种或混合物。
所述的半预聚体法聚合反应分别为:
异氰酸酯(B)与部分多元醇(A)及部分增塑剂(D)的异氰酸酯封端反应得到组分甲;
剩余部分多元醇(A)、扩链剂(C)及剩余部分(D)的均匀混合得到组分乙;
组分甲及组分乙的混合反应
其中:甲组分异氰酸酯封端反应中异氰酸酯(B)与多元醇(A)的摩尔比为1.5~3.5,设定的异氰酸根质量百分数ω(NCO)为5%~10%;甲乙组分扩链反应中(A)、(B)反应生成的异氰酸酯封端的半预聚体与(C)的摩尔比为0.80~1.05,扩链固化时设定的异氰酸根质量百分数ω(NCO)为0.5%~2.5%,增塑剂(D)加入量为20%~60%,催化剂加入量为0.1/千~0.5/千。
充填盾构管片中空密封条的聚氨酯弹性体的制备方法,上述两个步骤的反应为液体的聚合反应过程,制品的生产采用液体注射工艺。
采用不发泡低硬度聚氨酯弹性体填充盾构管片中空密封条,则具有硬度范围广、力学性能好、无增塑剂析出、密封性能和老化性能优异等特点。
盾构管件中空密封条填充用聚氨酯弹性体材料,采用半预聚物法合成,分为异氰酸酯组分和扩链剂组分,将两组分根据一定比例均匀混合,采用注射设备注入盾构管件中空密封条中,室温或加热固化即可。
本发明的优势在于:
1、硬度范围宽:通过配方调整,可制得硬度范围ShoreA0~60的不发泡弹性体,硬度范围广,适合于盾构管片中空密封条的填充。
2、使用温度范围宽,生热低:采用聚醚型聚氨酯弹性体体系制备的聚氨酯体系具有良好的柔顺性,材料的生热低,通过DSC(差示扫描量热法)检测,材料在-50℃下无变硬现象,仍可使用。
3、弹性好、力学性能好:低硬度的聚氨酯填充材料通常通过外压注入盾构管件的中空密封条内腔,并在外压作用下反应固化,固化物几乎没有体积收缩,没有水泥材料出现的密封不严或微孔弹性体受温度限制的缺点;同时固化后的材料拉断强度通常大于1.2MPa,拉断伸长率大于500%,完全满足了盾构管片中空密封条对填充聚氨酯弹性体的要求。
4、无增塑剂析出,老化性能好:聚氨酯弹性体填充材料由于原材料均为饱和结构,无不饱和键结构,同时聚醚多元醇具有较好的耐水性能,所以,材料的耐老化性能好;同时极性的增塑剂和聚氨酯材料具有良好的相容性,材料固化后在使用过程中不宜从固化物种析出。
本发明的制备工艺特点是:采用液体弹性体合成、注射成型工艺制备填充盾构管片中空密封条的聚氨酯弹性体,有别于传统的水泥填充及微孔聚氨酯弹性体填充,水泥填充材料固化后硬度大,且成型后易留有空隙,密封不良;而微孔聚氨酯弹性体填充盾构管片中空密封条,则易出现泡孔不均匀导致密封性和承载性差,另外,还容易出现受温度影响而难以发泡的问题。
本发明的一种盾构管件中空密封条充填用聚氨酯弹性体的制备方法及反应的主要说明:
聚醚聚合物多元醇及增塑剂的混合物在100-120℃下真空脱水0.5-1.5小时,冷却降温到70-80℃,加入异氰酸酯在80±5℃加热搅拌反应2-3小时制得组分甲;部分聚醚聚合物多元醇及增塑剂、催化剂等混合均匀得组分乙,甲乙组分在室温到50℃均匀混合,注入盾构管片的中空密封条中,60℃加热固化或室温下熟化24小时即可。
具体实施方式
下面结合具体实施例,进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的保护范围。此外应理解,在阅读本发明讲授的内容之后,本领域技术人员可以对本发明做各种改动或修改,这些等价形式同样属于本申请所附权利要求书所限定的范围。
以下就本发明的盾构管件中空密封条充填用的聚氨酯弹性体进行说明,该发明的聚氨酯弹性体由两个组分混合反应而成,即异氰酸酯组分与多元醇组分混合反应而成,异氰酸酯组分与多元醇组分混合比例为1:1,通过静态混合器混合注入盾构管件中空密封条中后室温或加热硫化一定时间。异氰酸酯组分与多元醇组分所用原料如下,本发明的实施例材料性能列于表1-6,实施例中的“份”指重量份。
多元醇A:分子量6000-6500聚醚三元醇330N,山东东大化工有限公司
多元醇B:分子量4000聚醚二醇ACCLAIM4220,德国BAYER公司
多元醇C:分子量2000聚醚二元醇220,山东东大化工有限公司
多元醇D:分子量6000-6500聚醚三元醇ACCLAIM6300,德国BAYER公司
多元醇E:分子量8000-8500聚醚三元醇ACCLAIM8200,德国BAYER公司
异氰酸酯A:甲苯二异氰酸酯TDI,德国BAYER公司
异氰酸酯B:液化MDI-100LL,烟台万华聚氨酯有限公司
增塑剂A:DOP,山东淄博增塑剂厂
增塑剂B:氯化石蜡,青岛金山化工有限公司
增塑剂C:芳烃油,山东东营石油公司
扩链剂A:乙二醇,上海试剂公司
扩链剂B:MOCA,苏州湘圆化工有限公司
扩链剂C:HC-600,青岛荣发化工有限公司
扩链剂D:三羟甲基丙烷,德国LANXESS公司
催化剂:锡类催化剂,上海试剂公司
实施例1
分别将100份聚醚多元醇A、B、C、D、E与22份DOP与芳烃油的混合物与TDI反应制备预聚体,预聚体的游离NCO%=7%。将80.1份330N、3.4份MOCA、0.4份乙二醇、2.4份DOP与芳烃油的混合物及0.05份催化剂混合均匀得多元醇组分,将预聚体组分与多元醇组分按1:1在50℃混合均匀,60℃或室温下熟化24小时,性能如下。
表1
实施例2
分别将78.6份聚醚二元醇220,与21.4份异氰酸酯A反应制备预聚体,预聚体的游离NCO%=7%。将330N、MOCA、乙二醇、DOP与芳烃油的混合物及份催化剂混合均匀得多元醇组分,预聚体与多元醇组分混合固化时设定的NCO%为1.5%、2.0%、2.5%、3.0%、3.5%,DOP与芳烃油或氯化石蜡的混合物占混合总量的40%,预聚体组分与多元醇组分按1:1在50℃混合均匀,60℃或室温下熟化,性能如下。
表2
实施例3
分别将78.6份聚醚二元醇220,20份DOP与芳烃油的混合物与21.4份异氰酸酯A/异氰酸酯B(70/30)反应制备预聚体,预聚体的游离NCO%=7%。将330N与MOCA、乙二醇、HC-600、三羟甲基丙烷中的一种或几种及DOP与芳烃油的混合物及份催化剂混合均匀得多元醇组分,预聚体与多元醇组分混合固化时设定的NCO%为3.0%,DOP与芳烃油的混合物占混合总量的40%,预聚体组分与多元醇组分按1:1在50℃混合均匀,60℃或室温下熟化24小时,性能如下表。
表3
实施例4
分别将78.6份聚醚二元醇220与21.4份TDI反应制备预聚体,预聚体的游离NCO%=7%。将71.15份330N、11.54份MOCA和乙二醇的混合物及0.05份催化剂混合均匀得多元醇组分,DOP及氯化石蜡或芳烃油混合物占总量的10%、15%、20%、25%、30%、35%、40%,将预聚体组分与多元醇组分按1:1在50℃混合均匀,60℃或室温下熟化24小时,性能如下表。
表4
实施例5
分别将78.6份聚醚二元醇220与21.4份TDI反应制备预聚体,预聚体的游离NCO%=7%。将49.8份330N、7.14份HC-600混合均匀得多元醇组分,DOP及氯化石蜡或芳烃油混合物占总量的20%,改变催化剂用量,将预聚体组分与多元醇组分按1:0.8在50℃混合均匀,60℃或室温下熟化24小时,性能如下表。
表5
实施例6
分别将100份聚醚多元醇A与TDI反应制备预聚体,预聚体的游离NCO%=7%。将80.1份330N、3.4份MOCA、0.4份乙二醇、0.05份催化剂混合均匀得多元醇组分,增塑剂加入量为25%,改变增塑剂种类及配比,预聚体组分与多元醇组分按1:1在50℃混合均匀,60℃或室温下熟化24小时,性能如下表。
表6
以上所述,仅是本发明的较佳实施例而已,并非是对本发明作其它形式的限制,任何熟悉本专业的技术人员可能利用上述揭示的技术内容加以变更或改型为等同变化的等效实施例。但是凡是未脱离本发明技术方案内容,依据本发明的技术实质对以上实施例所作的任何简单修改、等同变化与改型,仍属于本发明技术方案的保护范围。
Claims (10)
1.一种盾构管片中空密封条充填用的聚氨酯弹性体,由(A)、(B)、(C)、(D)四种主要成份采用半预聚体法聚合反应而成,其中:
(A)端羟基聚醚二元醇或多元醇,
(B)多异氰酸酯,
(C)低分子多元醇、二醇类或胺类扩链剂,
(D)增塑剂,
所述的半预聚体法聚合反应为:
多异氰酸酯(B)与部分端羟基聚醚二元醇或多元醇(A)及部分增塑剂(D)进行异氰酸酯封端反应得到组分甲;
剩余部分端羟基聚醚二元醇或多元醇(A)、扩链剂(C)及剩余部分增塑剂(D)均匀混合得到组分乙;
组分甲及组分乙混合反应。
2.根据权利要求1所述的聚氨酯弹性体,其特征在于:端羟基聚醚二元醇或多元醇(A)是由环氧丙烷、环氧乙烷、四氢呋喃、甘油、乙二醇、三羟甲基丙烷中一种以上成分聚合成聚醚二醇或多元醇。
3.根据权利要求1所述的聚氨酯弹性体,其特征在于:多异氰酸酯(B)是甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、多苯基甲烷多异氰酸酯中的一种或两种以上混合物。
4.根据权利要求1所述的聚氨酯弹性体,其特征在于:所述扩链剂或交联剂为3,3′-二氯-4,4′-二氨基二苯基甲烷(MOCA)、2,4-(2,6-)二氨基-3,5-甲硫基甲苯(DMTDA)、2,4-(2,6-)二氨基-3,5-乙基甲苯(DETDA)、2,4-(2,6-)二氨基-3,5-甲硫基氯苯、2,4-(2,6-)二氨基-3,5-甲硫基乙苯、乙二醇(EG)、1,4-丁二醇(BD)、二甘醇(DEG)、三羟甲基丙烷(TMP)、三异丙醇胺(TIPA)、三乙醇胺(TGA)、二甲硫基氯苯二胺(HC-600)、对苯二酚双-β-羟乙基醚(HQEE)、间苯二酚双-β-羟乙基醚(HER)中的一种以上成分;扩链剂优选采用乙二醇(EG)与HC-600或MOCA与三羟甲基丙烷并用。
5.根据权利要求1所述的聚氨酯弹性体,其特征在于:所述增塑剂为邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二甲氧乙基酯(DMEP)、邻苯二甲酸二异癸酯(DIDP)、氯化石蜡、石蜡油、芳烃油、溶剂油中的一种或两种以上的混合物。
6.根据权利要求5所述的聚氨酯弹性体,其特征在于:增塑剂优选为DOP与氯化石蜡并用,优选以7:3的比例复配。
7.根据权利要求1-6任一项所述的聚氨酯弹性体,其特征在于:甲组分异氰酸酯封端反应中异氰酸酯(B)与多元醇(A)的摩尔比为1.5~3.5,设定的异氰酸根质量百分数ω(NCO)为5%~10%;甲乙组分扩链反应中(A)、(B)反应生成的异氰酸酯封端的半预聚体与(C)的摩尔比为0.80~1.05,扩链固化时设定的异氰酸根质量百分数ω(NCO)为0.5%~2.5%,增塑剂(D)加入量为20%~60%。
8.根据权利要求1-6任一项所述的聚氨酯弹性体,其特征在于:所述的聚氨酯弹性体材料不发泡。
9.权利要求1-8任一项所述的聚氨酯弹性体的用途,其特征在于:填充盾构管片中空密封条,代替水泥填充及微孔聚氨酯弹性体填充。
10.权利要求1-8任一项所述的聚氨酯弹性体的制备方法,其特征在于:聚醚聚合物多元醇及增塑剂的混合物在100-120℃下真空脱水0.5-1.5小时,冷却降温到70-80℃,加入异氰酸酯在80±5℃加热搅拌反应2-3小时制得组分甲;部分聚醚聚合物多元醇及增塑剂、催化剂等混合均匀得组分乙,甲乙组分在室温到50℃均匀混合,注入盾构管片的中空密封条中,60℃加热固化或室温下熟化24小时即可。
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