CN109070493B - 在聚氨酯的基础上制备拉挤制品的方法 - Google Patents
在聚氨酯的基础上制备拉挤制品的方法 Download PDFInfo
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- CN109070493B CN109070493B CN201780024504.9A CN201780024504A CN109070493B CN 109070493 B CN109070493 B CN 109070493B CN 201780024504 A CN201780024504 A CN 201780024504A CN 109070493 B CN109070493 B CN 109070493B
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- diisocyanate
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Classifications
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C70/00—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts
- B29C70/04—Shaping composites, i.e. plastics material comprising reinforcements, fillers or preformed parts, e.g. inserts comprising reinforcements only, e.g. self-reinforcing plastics
- B29C70/28—Shaping operations therefor
- B29C70/40—Shaping or impregnating by compression not applied
- B29C70/50—Shaping or impregnating by compression not applied for producing articles of indefinite length, e.g. prepregs, sheet moulding compounds [SMC] or cross moulding compounds [XMC]
- B29C70/52—Pultrusion, i.e. forming and compressing by continuously pulling through a die
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/163—Catalysts containing two or more components to be covered by at least two of the groups C08G18/166, C08G18/18 or C08G18/22 covered by C08G18/18 and C08G18/22
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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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- C08G18/08—Processes
- C08G18/16—Catalysts
- C08G18/18—Catalysts containing secondary or tertiary amines or salts thereof
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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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- C08G18/20—Heterocyclic amines; Salts thereof
- C08G18/2045—Heterocyclic amines; Salts thereof containing condensed heterocyclic rings
- C08G18/2063—Heterocyclic amines; Salts thereof containing condensed heterocyclic rings having two nitrogen atoms in the condensed ring system
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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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- C08G18/225—Catalysts containing metal compounds of alkali or alkaline earth metals
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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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- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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- C08G18/48—Polyethers
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- C08G18/4816—Two or more polyethers of different physical or chemical nature mixtures of two or more polyetherpolyols having at least three hydroxy groups
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Abstract
本发明涉及一种制备拉挤制品的方法,其中将(a)二异氰酸酯或多异氰酸酯、(b)具有至少两个对异氰酸酯呈反应性的基团的化合物、(c)催化剂、(d)脱模剂和任选地(e)其它助剂物质和添加剂混合以形成拉挤成型树脂体系并用其使纤维材料润湿并硬化,其中二异氰酸酯和多异氰酸酯(a)与多元醇组分(B)混合,所述多元醇组分(B)包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)、催化剂(c)、脱模剂(d)和任选地其它助剂物质和添加剂(e),且多元醇组分(B)的pH值范围为6.5至8.5。本发明进一步涉及可根据该方法获得的拉挤制品。
Description
本发明涉及一种制备拉挤制品的方法,所述方法通过混合以下物质以得到拉挤成型树脂体系并用其使纤维材料润湿并硬化:(a)二异氰酸酯或多异氰酸酯、(b)具有至少两个对异氰酸酯呈反应性的基团的化合物、(c)催化剂、(d)脱模剂和任选地(e)其它助剂和添加剂,其中二异氰酸酯和多异氰酸酯(a)与多元醇组分(B)混合,所述多元醇组分(B)包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)、催化剂(c)、脱模剂(d)和任选地其它助剂和添加剂(e),且多元醇组分(B)的pH范围为6.5至8.5。本发明进一步涉及可通过该方法获得的拉挤制品。
拉挤成型是一种制备具有恒定横截面的纤维增强型材的连续方法。拉挤成型体系通常由浸渍装置和热模、以及为该方法提供动力的输出系统组成。将纤维浸渍在开口浴中或封闭的注射盒中。这是树脂使增强材料(例如玻璃纤维粗纱或玻璃纤维垫)润湿的地方。然后成型在热模中进行,复合材料的硬化也是如此。通过输出系统从模具中拉出成品型材,最后切割成所需的长度。
为了实现尽可能高效的拉挤成型方法,在拉挤制品的非常好的机械性能和高表面质量以外,还期望高的加工速度。此处的一个重要因素是复合材料在模具表面上的低附着力。
拜耳(Bayer)、亨斯迈(Huntsman)、Milgard Manufacturing Incorporated、ResinSystem Inc.以及其他机构已经描述了使用双组分聚氨酯体系用于拉挤方法。主要使用的材料是官能度为3.0的聚醚多元醇,它们在胺和金属络合物各自地作为催化剂以及多种添加剂的存在下与异氰酸酯(常常是聚合MDI)反应。在此还已经发现,随着加工速度的增加,表面质量变得更差。在型材表面上常常观察到完全反应的聚氨酯或PU粉末。高的输出速度对润湿质量有不利影响,因此对拉挤制品的机械性能也有不利影响。这些现象又对加工速度上升施加了限制。
在WO 2005/049301中,亨斯迈(Huntsman)通过使用两种金属催化剂来应对这个问题。拜耳(Bayer)使用基于DMC多元醇的体系(US 2008/0090921)或基于接枝多元醇的体系(US 2008/0087373),以及使用不混溶的PU体系(US 2008/0090996)。此外,拜耳和亨斯迈都提到原则上使用酸进行胺催化的部分中和,即封闭。WO 2005038118中提及的具体实例包括甲酸、乙酸、2-乙基己酸和油酸。
在US 2007/0113983、US 2007/0116941和US 2007/0117921中,MilgardManufacturing Incorporated认为,原则上可以通过向聚氨酯体系中添加降低树脂收缩的聚合物添加剂来改善表面质量。这些“低-收缩添加剂”的加入浓度基于整个树脂体系计优选为4至10%。此处的表述聚合物添加剂意指聚苯乙烯、苯乙烯-丙烯酸酯共聚物、甲基丙烯酸酯树脂、聚乙酸乙烯酯和受保护的聚环氧丙烷。
WO 2011/067246描述了一种拉挤成型方法,其中将沸点为至少200℃且具有相对高官能度的酸加入至拉挤成型树脂体系中。虽然这降低了输出的力并改善了拉挤制品的表面,但这些参数仍然需要改进。
因此,本发明的一个目的是提供一种方法,该方法可以制备拉挤制品并且进一步降低拉挤制品从模具中输出所需的力,并且该方法得到改善的拉挤制品表面。这与高于1米/分钟的高输出速度和/或复杂模制品几何形状的工业要求是特别相关的。
所述目的已籍由一种制备拉挤制品的方法来实现,所述方法通过混合以下物质以得到拉挤成型树脂体系并用其使纤维材料润湿并硬化:(a)二异氰酸酯或多异氰酸酯、(b)具有至少两个对异氰酸酯呈反应性的基团的化合物、(c)催化剂、(d)脱模剂和任选地(e)其它助剂和添加剂,其中二异氰酸酯和多异氰酸酯与多元醇组分(B)混合,所述多元醇组分(B)包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)、催化剂(c)、脱模剂(d)和任选地其它助剂和添加剂(e),且多元醇组分(B)的pH范围为6.5至8.5。本发明进一步涉及可通过该方法获得的拉挤制品。
出于本发明的目的,表述拉挤成型树脂体系意指一种由多种组分组成的并且在组分已混合在一起之后适合于用纤维材料形成拉挤制品的体系。
可使用的二异氰酸酯或多异氰酸酯(a)包括任何已知用于制备聚氨酯的脂族、脂环族或芳族异氰酸酯。实例为二苯基甲烷2,2'-二异氰酸酯、二苯基甲烷2,4'-二异氰酸酯和二苯基甲烷4,4'-二异氰酸酯;单体二苯基甲烷二异氰酸酯和具有较多数量的环的二苯基甲烷二异氰酸酯的同系物(聚合MDI)的混合物;异佛尔酮二异氰酸酯(IPDI)及其低聚物;甲苯二异氰酸酯(TDI),实例为甲苯二异氰酸酯异构体,例如甲苯2,4-二异氰酸酯或甲苯2,6-二异氰酸酯以及它们的混合物;四亚甲基二异氰酸酯及其低聚物;六亚甲基二异氰酸酯(HDI)及其低聚物;亚萘基二异氰酸酯(NDI)及其混合物。
所用的二异氰酸酯或多异氰酸酯(a)优选地包含基于二苯基甲烷二异氰酸酯的异氰酸酯,特别是聚合MDI。二异氰酸酯和多异氰酸酯(a)的官能度优选为2.0至2.9,特别优选为2.1至2.8。根据DIN 53019-1至3,这些二异氰酸酯或多异氰酸酯(a)在25℃下的粘度优选为5-600mPas,特别优选为10-300mPas。
二异氰酸酯和多异氰酸酯(a)也可以以多异氰酸酯预聚物的形式使用。这些多异氰酸酯预聚物可通过以下方式获得:使过量的上述多异氰酸酯(成分(a-1))与具有至少两个对异氰酸酯呈反应性的基团的化合物(成分(a-2))在例如30℃至100℃、优选地在约80℃的温度下反应得到预聚物。本发明的多异氰酸酯预聚物的NCO含量优选为20至33重量%的NCO,特别优选为25至32重量%的NCO。
具有至少两个对异氰酸酯呈反应性的基团的化合物(a-2)是本领域技术人员已知的并且在“Kunststoffhandbuch,7,Polyurethane”[Plastics handbook,7,Polyurethanes],Carl Hanser-Verlag,1993年第3版,第3.1章中作为例子描述。因此,例如使用的具有至少两个对异氰酸酯呈反应性的基团的化合物可以包括聚醚醇或聚酯醇,例如下面(b)中所述的那些。优选地,使用的具有至少两个对异氰酸酯呈反应性的基团的化合物(a-2)包含含有仲OH基团的聚醚醇或聚酯醇,实例为聚环氧丙烷。此处聚醚醇或聚酯醇的官能度优选为2至4,特别优选为2至3。
特别优选不使用多异氰酸酯预聚物。
使用的具有至少两个对异氰酸酯呈反应性的基团的化合物(b)——出于本发明目的另一个用于它们的术语是“多元醇”——可包含任何具有至少两个对异氰酸酯呈反应性的基团(例如OH、SH、NH、NH2、COOH和CH-酸性基团)的化合物,其中仲OH基团的比例基于对异氰酸酯呈反应性的基团数量计为至少50%,优选至少60%,特别优选至少70%,并且特别是至少80%。
通常使用的材料是具有2至8个异氰酸酯-反应性氢原子的聚醚醇和/或聚酯醇以及低分子量多元醇例如丙三醇、二丙二醇和/或三丙二醇。这些化合物的OH值范围通常为30至2000mg KOH/g,优选为40至1000mgKOH/g。本文中使用的所有的具有至少两个对异氰酸酯呈反应性的基团的化合物(b)的平均OH值为100-1000mg KOH/g,优选为300-900mgKOH/g。
聚醚醇通过已知方法获得,例如在催化剂的存在下在添加至少一种包含2-8个、优选2-6个、特别优选2-4个反应性氢原子的起始分子的情况下通过环氧烷烃的阴离子聚合获得。使用的催化剂可包括碱金属氢氧化物,如氢氧化钠或氢氧化钾,或碱金属醇盐,如甲醇钠、乙醇钠、乙醇钾或异丙醇钾,或在阳离子聚合的情况下,路易斯酸如五氯化锑,三氟化硼醚化物或漂白土。此外,双金属氰酸盐化合物,称为DMC催化剂,也可用作催化剂。
使用的环氧烷烃优选地包含一种或更多种在亚烷基部分中具有2-4个碳原子的化合物,例如四氢呋喃、环氧乙烷、1,2-环氧丙烷或1,2-环氧丁烷或2,3-环氧丁烷,在每种情况下单独地或以混合物的形式,优选1,2-环氧丙烷和/或环氧乙烷,特别是1,2-环氧丙烷。
可使用的起始分子的实例为乙二醇、二乙二醇、丙三醇、三羟甲基丙烷、季戊四醇、糖衍生物如蔗糖、己糖醇衍生物如山梨糖醇、甲胺、乙胺、异丙胺、丁胺、苄胺、苯胺、甲苯胺、甲苯二胺、萘胺、乙二胺、二亚乙基三胺、4,4'-亚甲基二苯胺、1,3-丙二胺、1,6-己二胺、乙醇胺、二乙醇胺、三乙醇胺,以及其他二元醇或多元醇或单官能胺或多官能胺。
使用的聚酯醇主要通过具有2-12个碳原子的多元醇(例如乙二醇、二乙二醇、丁二醇、三羟甲基丙烷、丙三醇或季戊四醇)与具有2-12个碳原子的多元羧酸(例如琥珀酸、戊二酸、己二酸、辛二酸、壬二酸、癸二酸、癸烷二羧酸、马来酸、富马酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸和萘二羧酸或其酸酐的异构体)缩合而制备。
在聚酯的制备中还可同时使用的其他起始材料包括疏水性物质。疏水性物质是不溶于水且包含非极性有机部分的物质,其还具有至少一个选自羟基、羧酸、羧酸酯及其混合物的反应性基团。疏水材料的当量重量优选为130-1000g/mol。可使用的材料的实例为脂肪酸,例如硬脂酸、油酸、棕榈酸、月桂酸或亚油酸;以及脂肪和油类,例如蓖麻油、玉米油、向日葵油、大豆油、椰子油、橄榄油或妥尔油。当聚酯包含疏水性物质时,疏水性物质的比例基于聚酯醇的全部单体含量计优选为1-30摩尔%,特别优选为4-15摩尔%。
使用的聚酯醇的官能度优选为1.5至5,特别优选为1.8至3.5。
在一个特别优选的实施方案中,使用的具有对异氰酸酯呈反应性的基团的化合物(b)包括聚醚醇,特别地仅包括聚醚醇。优选地,聚醚醇的实际平均官能度优选为2至4,特别优选为2.5至3.5,特别是2.8至3.2,它们的OH值为300-900mg KOH/g,它们的仲OH基团的含量为至少50%,优选地至少60%,特别优选地至少70%,特别是至少80%。本文中使用的聚醚醇优选地包含基于丙三醇作为起始剂和1,2-环氧丙烷的聚醚醇。
使用的催化剂(c)可包括任何常规用于制备聚氨酯的催化剂。这些催化剂在例如“Kunststoffhandbuch,Band 7,Polyurethane”[Plastics handbook,第7卷,Polyurethanes],Carl Hanser Verlag,1993第3版,第3.4.1章中作为例子描述。本文中使用的材料是例如有机金属化合物,例如锡络合物、锌络合物、钛络合物、锆络合物、铁络合物、汞络合物或铋络合物,优选有机锡化合物,例如有机羧酸的锡(II)盐,例如乙酸锡(II)、辛酸锡(II)、乙基己酸锡(II)和月桂酸锡(II),以及有机羧酸的二烷基锡(IV)盐,例如二乙酸二丁基锡、二月桂酸二丁基锡、马来酸二丁基锡和二乙酸二辛基锡;以及新癸酸苯基汞;羧酸铋,例如新癸酸铋(III)、2-乙基己酸铋和辛酸铋;及其混合物。其他可能的催化剂是高碱性胺催化剂。它们的实例是脒,例如2,3-二甲基-3,4,5,6-四氢嘧啶;叔胺,例如三乙胺,三亚乙基二胺,三丁胺,二甲基苄胺,N-甲基吗啉、N-乙基吗啉、N-环己基吗啉,N,N,N',N'-四甲基乙二胺、N,N,N',N'-四甲基丁二胺、N,N,N',N'-四甲基-己二胺、五甲基二亚乙基三胺、四甲基二氨基乙基醚、双-(二甲基氨基丙基)脲、二甲基哌嗪、1,2-二甲基咪唑、1-氮杂双环[3.3.0]辛烷以及优选地1,4-二氮杂双环[2.2.2]辛烷、1,8-二氮杂双环[5.4.0]十一碳烯-7-烯;和链烷醇胺化合物,例如三乙醇胺、三异丙醇胺、N-甲基二乙醇胺和N-乙基二乙醇胺和二甲基乙醇胺。催化剂可单独使用或以混合物的形式使用。任选地使用的催化剂(c)包括金属催化剂和碱性胺催化剂的混合物。催化剂(c)优选地包含胺催化剂,特别优选地不使用金属催化剂。
在一个特别的实施方案中,这些催化剂,特别是胺催化剂,以封闭型催化剂的形式使用,例如被质子供体封闭的催化剂。使用的质子供体可优选地包含羧酸或酚和/或其他芳族醇。使用的质子供体特别优选地包含芳族醇。本文中,质子供体中作为质子供体起作用的基团与胺催化剂中的可质子化的胺基团的摩尔比优选为0.9:1.0至1.1:1.0。特别优选地,本文中使用的封闭型胺催化剂包含封闭型1,8-二氮杂双环[5.4.0]十一碳-7-烯。可能使用的封闭剂可包括酚或羧酸衍生物,例如苯酚或苯二甲酸。
本文中催化剂(c)的比例优选为0.05-10重量%,特别优选为0.1-5重量%,特别地为0.1-2.5重量%,基于组分(b)至(e)的总重量计。本文中催化剂优选以以下方式使用:其使得在将组分(a)-(e)混合后本发明的拉挤成型树脂体系在25℃下的凝胶时间大于10分钟、特别地大于12分钟且小于60分钟,特别是大于15分钟且小于60分钟。此外,催化剂的选择使得在将组分(a)-(e)混合后在220℃下本发明的拉挤成型树脂体系在60秒内、特别优选0-45秒内且特别是5-30秒内完全硬化。
本文中开口时间确定为这样的一段时间,在该时间期间,在恒定温度下,反应混合物的粘度增加到一定程度,使得所需的搅拌力超过Shyodu100凝胶时间测试仪(Gel Timer)(2012版本)的规定的搅拌力。本文中,在每种情况下,放入200g反应混合物,并在高速混合器中以1950rpm混合30秒,并在室温下在直径为7cm的PP烧杯中使用具有相关线网搅拌器(wire stirrer)的Shyodu 100凝胶时间测试仪(2012版本)以20rpm搅拌130g所述混合物,直至所述粘度,以及因此反应混合物所需的搅拌力超过所述凝胶时间测试仪的搅拌力。
为了确定在220℃下的完全硬化,将用于制备聚氨酯反应混合物的组分在室温下称重至烧杯中,并通过高速混合器以2000转/分钟混合30秒。使用巴斯德吸管(Pasteurpipette)将10mL体系置于表面温度为220℃的板上。从施加至板到完全硬化的时间(以s计)是在相应温度下的固化时间。当样品与木制刮刀接触不再显示出粘附力时,已达到完全硬化。
使用的脱模剂(d)可包括任何常规用于制备聚氨酯的脱模剂,实例为长链羧酸,特别是脂肪酸,例如硬脂酸;长链羧酸的胺,例如,硬脂酰亚胺(stearimide);脂肪酸酯;长链羧酸的金属盐,例如硬脂酸锌;和硅氧烷。特别合适的材料是专门用于拉挤成型的内部脱模剂,其可从例如Axel Plastics或Würtz获得。在一个特别优选的实施方案中,使用的内部脱模剂包括来自Würtz的Pul5K脱模剂。
通常使用的脱模剂的量基于组分(a)至(e)的总重量计为0.5-10重量%,优选为1-6重量%,特别是1.5-4重量%。
使用的助剂和添加剂(e)可包括任何已知用于制备聚氨酯的助剂和添加剂。可提及的实例是表面活性物质、附着力促进剂、填料、染料、颜料、阻燃剂、水解稳定剂、降粘剂、除水剂、消泡剂,以及抑制真菌的物质和抑制细菌的物质。这些物质是已知的并且在“Kunststoffhandbuch,Band 7,Polyurethane”[Plastics handbook,第7卷,Polyurethanes],Carl Hanser Verlag,1993年第3版,第3.4.4章和第3.4.6至3.4.11章中作为例子描述。
因此,可用于水吸附的添加剂可包括例如选自铝硅酸钠、铝硅酸钾、铝硅酸钙、铝硅酸铯、铝硅酸钡、硅铝酸镁、硅铝酸锶的铝硅酸盐;铝磷酸钠、铝磷酸钾、铝磷酸钙;及其混合物。特别优选使用蓖麻油中的铝硅酸钠、铝硅酸钾和铝硅酸钙的混合物作为载体。
用于水吸收的添加剂的数均粒径优选不大于200μm,特别优选不大于150μm,特别是不大于100μm。用于水吸收的本发明添加剂的孔宽优选为2-5埃。
如果添加用于水吸收的添加剂,则其添加量优选大于1重量份,特别优选范围为0.5-5重量份,基于组分(b)至(e)的总重量计。
使用的附着力促进剂可包括硅烷,例如异氰酸酯硅烷、环氧硅烷或氨基硅烷。这些物质在E.P.Plueddemann,Silane Coupling Agents,2nd edn.,Plenum Press,纽约,1991以及in2.K.L.Mittal,edn.,Silanes and OtherCoupling Agents,VSP,Utrecht,1992中作为例子描述。
使用的降粘剂可包括例如γ-丁内酯、碳酸亚丙酯,以及反应性稀释剂,例如二丙二醇,二乙二醇和三丙二醇。
本发明的拉挤成型树脂体系优选包含小于2重量%、特别优选小于1重量%的在标准压力下沸点低于200℃的物质。在组分(a)至(e)刚混合后,拉挤成型树脂体系的粘度根据DIN 53019-1至3在25℃下优选小于1500mPas,特别优选小于1200mPas,特别是小于1000mPas。本文中组分(a)至(e)的混合定量比例优选地使得异氰酸酯指数为90至140,特别优选100至130,特别是115至125。出于本发明目的,本文中表述异氰酸酯指数意指异氰酸酯基团与异氰酸酯-反应性基团的化学计量比乘以100。本文中表述异氰酸酯-反应性基团意指反应混合物中包含的所有异氰酸酯-反应性基团,但不是异氰酸酯基团本身。
在本方法中,将本发明的拉挤成型树脂体系的组分混合,得到聚氨酯反应混合物,并用所得的反应混合物润湿纤维材料。这通常以双组分方法进行。为此目的,首先制备多元醇组分(B),其包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)和催化剂(c)以及脱模剂(d)和任选地其它助剂和添加剂(e)。然后使该组分与异氰酸酯反应,得到拉挤成型树脂体系。
然后将润湿的纤维材料模塑,并使反应混合物硬化。出于本发明的目的,表述反应混合物代表当反应转化率基于异氰酸酯基团计低于90%时组分(a)至(e)的混合物。
本文中本发明的拉挤成型树脂体系的组分的混合可以以常规制备基于聚氨酯的反应混合物的方式进行,例如在高压或低压方法中。
对本发明必要的是,在与二异氰酸酯或多异氰酸酯(a)混合时,具有至少两个对异氰酸酯呈反应性的基团的化合物(b)的pH范围为6.5至8.5,优选7.0至8.5,特别是7.5至8.4。如果使用双组分方法,则对于本发明必要的是,与二异氰酸酯或多异氰酸酯(b)混合时,多元醇组分(B)具有适当的pH。
pH可通过添加影响pH的物质来建立,例如通过添加氢供体或氢受体。可能的氢供体的实例包括羧酸例如乙酸或柠檬酸,和无机酸例如磷酸。可能的质子受体的实例是碱,例如胺化合物和弱酸的盐,例如羧酸的碱金属盐或多元无机酸(如磷酸)的盐。特别优选的实施方案将质子供体和质子受体以一种混合比一起使用,以使得具有至少两个对异氰酸酯呈反应性的基团的化合物(b)的pH稳定在6.5至8.5的范围内。本文中影响pH的物质优选不具有对异氰酸酯呈反应性的基团,例如羧酸基团或氨基基团。本文中特别优选的质子供体和质子受体的组合包括碱金属磷酸氢盐,特别是磷酸氢钠。特别地,使用由磷酸氢二钠和磷酸二氢钠制成的体系。
本文中优选的是,pH-稳定的组分中——例如具有至少两个对异氰酸酯具有反应性的基团的化合物(b)中或多元醇组分(B)中——的水含量最小化。因此,组分(b)至(e)中水含量优选为至多1重量%,特别优选至多0.5重量%,特别是0.2重量%,在每种情况下基于组分(b)至(e)的总重量计。本文中水含量基于可用于与异氰酸酯的反应的游离水计。当限定最大含水量时,忽略结合水,例如除水剂内结合的水。
所用的纤维材料可包括任何类型的连续纤维。本文中表述连续纤维是指长度至少为数米的纤维材料。这些材料例如是从卷上展开的。本文中使用的纤维材料可包括单根纤维(称为纤维粗纱)、编织纤维、纤维毡、铺置纤维稀松布(laid fiber scrims)和机织纤维。特别地,在复合纤维材料如编织纤维、加捻纤维、铺置纤维稀松布或机织纤维的情况下,包含在这些纤维结构中的单根纤维也可包含更短的单根纤维,但实际复合纤维材料必须采取连续材料的形式。优选地,纤维材料优选包含以下物质或由以下物质组成:玻璃纤维、玻璃毡、碳纤维、聚酯纤维、天然纤维、芳族聚酰胺纤维、玄武岩纤维或尼龙纤维或其组合;特别优选使用碳纤维或玻璃纤维,或碳纤维和玻璃纤维的组合。
纤维材料的润湿优选在闭合模具中进行。在纤维材料润湿期间的温度优选低于100℃,优选为0℃至75℃,特别优选为10℃至50℃,特别是15℃至35℃。本文中纤维材料的比例基于成品拉挤制品计优选为10-90重量%,特别优选30-90重量%,特别是60-90重量%。
润湿后,优选地,将用反应混合物润湿的纤维材料穿过模具拉出。本文中模具在垂直于湿润的纤维材料的拉出方向上的横截面形状,可以根据需要,但尽可能恒定,例如狭缝形或圆形、L形、T形或者更复杂的形状。本文中模具的温度优选为150℃至250℃,其中使聚氨酯反应混合物硬化,得到成品聚氨酯。
优选地,拉挤制品以大于每分钟一米的速度从模具中拉出。输出速度特别优选地大于1.5米/分钟,特别是大于2.0米/分钟。通常将得到的拉挤制品切成所需长度。在一个特别优选的实施方案中,拉挤制品的横截面不同于扁平型材的横截面,实例是L型材、V型材和U型材以及更复杂的型材。
本发明进一步提供了可通过本发明的方法获得的拉挤制品。该拉挤制品表现出优异的表面质量和润湿质量。在扁平型材的情况下,拉挤制品的机械性能在输出速度为0.5米/分钟和输出速度为1.5米/分钟时是相同的。
下面将参考实施例对本发明进行说明:
起始材料:
多元醇1:丙三醇-起始的聚环氧丙烷,OH值为400mg KOH/g
多元醇2:丙三醇-起始的聚丙烯/聚环氧乙烷,官能度为2.7,OH值为42mg KOH/g
多元醇3:丙三醇-起始的聚环氧丙烷,其中OH值为805mg KOH/g
多元醇4:聚丙二醇,其中OH值为55mg KOH/g
多元醇5:二丙二醇
催化剂1:苯酚-封闭的1,8-二氮杂双环[5.4.0]十一碳-7-烯(摩尔比1:1)
催化剂2:乙酸钾,溶于单乙二醇中(重量比2:3)
IMR 1:基于脂肪酸的脱模剂
pH:多元醇组分的pH
Iso 1:聚合二苯甲烷二异氰酸酯
Iso 2:单体二苯甲烷二异氰酸酯
Iso 3:包含羰酰亚胺-改性(carbonidimide-modified)的二苯基甲烷二异氰酸酯的单体二苯基甲烷二异氰酸酯
酸:磷酸
缓冲液:包含磷酸氢二钠和磷酸二氢钠的缓冲液体系
在由镀铬钢制成的模具中,在0.2-1.0m/min的输出速度下制造具有矩形横截面(35×4mm2)并且纤维含量为约54体积%的型材。此处使用的纤维材料包括来自JohnsManville Slovakia的StarRov 907 4800特克斯玻璃纤维。
表1整理了聚氨酯体系的精确组成,以及所得拉挤制品的表征。此处的第一步产生了具有不同pH的多元醇组分。此处的比较例1不包含pH调节添加剂;比较2包含磷酸。
表1
表1示出了,通过将pH调节至6.5至8.5的范围,获得了具有特别低的输出力和优异表面的拉挤制品。本文中pH使用玻璃电极(具有Methrom 6.0229.100电极的DMP Titrino785测试仪)测定。使用的校准溶液来自Methrom:pH 4缓冲液,pH 7磷酸盐缓冲液和pH 9硼酸盐缓冲液。
Claims (14)
1.一种制备拉挤制品的方法,所述方法通过混合以下物质以得到拉挤成型树脂体系并用其使纤维材料润湿并硬化:
a)二异氰酸酯或多异氰酸酯,
b)具有至少两个对异氰酸酯呈反应性的基团的化合物,
c)催化剂,
d)脱模剂和任选地,
e)其他助剂和添加剂,
其中二异氰酸酯或多异氰酸酯(a)与多元醇组分(B)混合,所述多元醇组分(B)包含具有至少两个对异氰酸酯呈反应性的基团的化合物(b)、催化剂(c)、脱模剂(d)和任选地其它助剂和添加剂(e),多元醇组分(B)的pH为6.5至8.5。
2.根据权利要求1所述的制备拉挤制品的方法,其中多元醇组分(B)中的水含量小于1重量%,基于组分(B)的总重量计。
3.根据权利要求1或2所述的制备拉挤制品的方法,其中多元醇组分(B)包含含有多元无机酸的缓冲液体系。
4.根据权利要求1或2所述的制备拉挤制品的方法,其中催化剂(c)包含胺催化剂。
5.根据权利要求1或2所述的制备拉挤制品的方法,其中所述脱模剂包含脂肪酸和/或脂肪酸酯。
6.根据权利要求1或2所述的制备拉挤制品的方法,其中使用的二异氰酸酯或多异氰酸酯(a)包含平均官能度为2.1至2.8的聚合MDI。
7.根据权利要求1或2所述的制备拉挤制品的方法,其中具有至少两个对异氰酸酯呈反应性的基团的化合物(b)包含平均官能度为2-4且仲OH基团含量至少为50%的聚醚醇。
8.根据权利要求1或2所述的制备拉挤制品的方法,其中具有至少两个对异氰酸酯呈反应性的基团的化合物(b)的平均OH值为100-1000mg KOH/g。
9.根据权利要求1或2所述的制备拉挤制品的方法,其中在刚混合后拉挤成型树脂体系的粘度在25℃下小于1500mPas。
10.根据权利要求1或2所述的制备拉挤制品的方法,其中拉挤成型树脂体系包含小于2.0重量%的在标准压力下沸点低于200℃的物质。
11.根据权利要求1或2所述的方法,其中将润湿的纤维材料穿过模具拉出并硬化,其中模具的温度为150℃至250℃。
12.根据权利要求1或2所述的方法,其中将湿润的纤维材料穿过模具拉出的输出速度大于每分钟一米。
13.根据权利要求1或2所述的方法,其中纤维材料含量为30-90重量%。
14.一种拉挤制品,其可通过根据权利要求1-13中任一项所述的方法制备。
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