CN112409568A - 一种风能风机叶片用聚脲弹性体及其制备方法 - Google Patents

一种风能风机叶片用聚脲弹性体及其制备方法 Download PDF

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CN112409568A
CN112409568A CN202011246290.XA CN202011246290A CN112409568A CN 112409568 A CN112409568 A CN 112409568A CN 202011246290 A CN202011246290 A CN 202011246290A CN 112409568 A CN112409568 A CN 112409568A
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polyurea elastomer
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陈旨进
卓聪聪
周琪权
李阜阳
吴俊杰
李欣
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Wuxi Bojin Polymer Research And Development Co ltd
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Abstract

本发明属于高分子材料合成领域,具体涉及一种风能风机叶片用的聚脲弹性体的制备方法，使用多元醇和二异氰酸酯为基础原料合成NCO封端的预聚体，使用胺类、醇类、醇胺类及三官聚醚作为扩链剂，辅以功能助剂浇注成型，通过预聚体与扩链剂的相互反应形成大分子，达到交联固化目的，从而获得聚脲弹性体。该聚脲弹性体机械性能同时达到拉伸强度大于30Mpa，断裂伸长率大于600％，硬度60‑84A，有效满足风机叶片户外使用的恶劣环境。

Description

一种风能风机叶片用聚脲弹性体及其制备方法
技术领域
本发明属于高分子材料合成领域,具体涉及一种风能风机叶片用的聚脲弹性体及其制备方法。
背景技术
风力发电为国际社会重点发展的绿能产业，风电机组所获得的风能大小和叶片长度的平方近似成正比，而风能风机整个叶片直接受到风沙、雨水、冰雹和其他颗粒等的撞击，从而对叶片造成侵蚀与磨损，破坏风机叶片的基本形状，对风力发电空气动力学的效率及风机叶片的保护带来不利影响。在我国，南方风能发电主要以抗台风，耐腐蚀为主，北方主要以抗沙尘、抗腐蚀为主，为此叶片表面在涂有一定保护涂层(环氧树脂等)的同时，还会添加一层保护套，该保护套可以定期更换，耐磨、耐腐蚀、耐低温，满足不同的气候条件，实现对风能风机叶片的保护。
在风能叶片实际应用中，叶片外端的保护套需要3年左右的时间更换一次，几十米高的风轮需要停机运转，维修时需要填胶、固化、打磨、涂层等工序，耗时费力，影响发电效益，给风能发电企业带来非常庞大的开支。目前还没有理想的方案可以解决风能叶片保护套定期更换的弊病，且全球市场上能够提供相关技术的企业只有丹麦Polytech一家，因此迫切需要我国相关企业在相关领域实现更高性能的突破，使风能叶片保护套能够更加抵抗恶劣的户外环境。
发明内容
针对现有技术中的问题，本发明提供一种风能风机叶片用聚脲弹性体的制备方法，解决了耐候型风能风机保护套的匮乏，利用NCO封端的预聚体与扩链剂形成反应，形成聚脲弹性体，且制备方法成本低，易操作，无特殊设备，耐候性好，机械性能优于现有产品。
为实现以上技术目的，本发明的技术方案是：
一种风能风机叶片用聚脲弹性体的制备方法，将含NCO封端的预聚体与扩链剂反应得到聚脲弹性体，然后采用浇注工艺形成最终产品。
具体步骤如下：
步骤1，将含NCO封端的预聚体加热40-120℃，并将其作为A组分；将扩链剂加热至40-130℃，并将其作为B组分；
步骤2，将A组分和B组分在60-120℃下快速搅拌，充分混合并确保无气泡产生，然后倒入至90-130℃的模具中；
步骤3，弹性体在90-130℃的模具中固化0.15-3h后脱模，并在110℃硫化16h以上，室温静置7天后得到聚脲弹性体产品。
进一步的，所述扩链剂采用胺类扩链剂、醇类扩链剂、醇胺类扩链剂、三官聚醚大分子中的一种或几种。
进一步的，所述胺类扩连剂包括MOCA、E-300、E-100、MDEA、MCDEA、MDA、MOEA、4200、4100，天冬聚脲树脂，作为主要小分子扩连剂；醇类扩连剂包括EG、BDO、PG、TMP、HQEE、HG、DEG、HER、GY、蓖麻油，甘油，作为辅助扩链剂；醇胺类扩链剂包括TIPA、HPA、乙醇胺、二乙醇胺；三官聚醚包括不同活性及起始剂的聚醚多元醇，分子量Mw＝1000-6000，如佳化化学股份旗下的Puranol G310、Puranol G4030、Puranol G5030或具有相似功能的其他牌号产品。
所述步骤2中的A组分与B组分的摩尔比为0.95-1.45。
所述步骤1中的B组分还设置有助剂，且该助剂包括填料、色浆、抗老化助剂(包括抗氧剂、抗水解剂、UV吸收剂等)、阻燃剂、除水剂等其他有助于加工的助剂或功能性助剂，助剂加入量是B组分质量的0.5-10％，优选为1-6％。
再进一步的，弹性体的质量配比为：A组分预聚体65-95％、胺类扩连剂4-15％、醇类扩连剂0-10％、醇胺类扩链剂0-5％、三官聚醚2-40％、助剂0.5-10％。
所述A组分的制备方法，包括如下步骤：
步骤a，将多元醇和第二助剂加入至反应容器内，充分搅拌并加热至100-120℃除水0.5h以上，所述第二助剂为抗氧剂1010、Irganox245中的一种或两种，加入量是多元醇质量的0-3％；
步骤b，将反应容器降温至50-80℃，然后加入多异氰酸酯，并在80-110℃反应2-3h；
步骤c，经检测预聚体内NCO含量，达标后密封保存待用。
进一步的，所述步骤a中的多元醇包含聚酯多元醇，采用聚己二酸系列多元醇，聚己二酸乙二醇酯二醇、聚己二酸二乙二醇酯二元醇、聚己二酸乙二醇二乙二醇酯二醇、聚己二酸丁二醇酯二醇、聚己二酸乙二醇丁二醇酯二醇、聚己二酸丁二醇二乙二醇酯二醇、聚己二酸丁二醇乙二醇二乙二醇酯二醇中的一种或多种混合物。
所述步骤a中的多元醇包含聚己内酯多元醇，聚碳酸酯多元醇，聚烯烃多元醇，环氧树脂，丙烯酸酯多元醇中的一种或多种。
所述步骤a中的多元醇包含聚醚多元醇，可以为聚氧化丙烯多元醇，聚氧化丙烯氧化乙烯共聚醚多元醇和聚四氢呋喃多元醇中的一种或多种混合物。
所述步骤a中的多元醇的分子量为1000-6000，优选为1800-3000。
所述步骤b中的多异氰酸酯为MDI，TDI，HDI，NDI，IPDI，HMDI，PPDI，TODI，XDI中的一种或者多种混合物。
所述步骤c中的预聚体NCO含量为2-15％，优选为3-8％，更优选为4-6％。
再进一步的，所述含NCO预聚体的质量配比如下：双官聚醚多元醇10-80％、三官聚醚多元醇0-10％、聚酯多元醇10-80％、聚己内酯多元醇0-80％、聚碳酸酯或其他多元醇0-30％、第二助剂0-3.0％。
所述聚脲弹性体用于风能风机叶片保护套。
从以上描述可以看出，本发明具备以下优点：
1.本发明解决了耐候型风能风机保护套的匮乏，利用NCO封端的预聚体与扩链剂形成反应，形成聚脲弹性体，且制备方法成本低，易操作，无特殊设备，耐候性好，机械性能优于现有产品。
2.本发明利用可控性的NCO封端预聚体实现了预聚体的粘度调节，从而有效的控制了浇注工艺。
3.本发明制备的聚脲弹性体，拉伸强度＞30Mpa，断裂伸长率＞600％，硬度范围60-80A，满足风机叶片在户外使用要求。
4.本发明的配比中NCO封端的预聚体(A组份)中含有至少10％的聚己内酯或聚酯多元醇，B组份中含有至少4％胺类扩连剂，2％三官聚醚，有效保障了弹性体的机械性能。10％的聚己内酯或聚酯多元醇具备更加优良的耐水解性和低温柔韧性，较高的结晶性使其具有更好的耐热性、耐候性，且制备得到的弹性体强度更高。添加聚醚后,聚酯和聚醚两种混合的软段材料和不同的分子链长度可以更好地吸收外界能量,显示出较好的弹性。而胺类扩链剂与NCO形成聚脲，脲基团极性大，可以形成更多的氢键，形成风机叶片弹性体的保障。
5.本发明利用A组分和B组分的配合，辅以合适的制备工艺，更加耐磨，能够保证聚脲弹性体具备较高的合格率，生产效率大幅度提升。
具体实施方式
结合实施例详细说明本发明，但不对本发明的权利要求做任何限定。
实施例1
一种聚脲弹性体
步骤1，A组分(NCO封端预聚体)的制备：
将50重量份聚己二酸乙二醇酯(Mw＝2000)，50重量份聚己内酯(Mw＝2000)，100质量份聚四氢呋喃醚二醇(Mw＝2000)，0.3质量份抗氧剂1010于反应釜中，加热至110℃，充分搅拌下抽真空除水0.5h；降温至70℃，加入60质量份MDI-50，N2保护条件下，90-110℃反应2h，测定NCO含量为4.3％，粘度＝9200mPa.S(60℃)，将预聚体密封保存；
步骤2，B组分(扩链剂)的制备
将15重量份MOCA，5质量份Un i l ink 4200，40质量份Purano l G 5030(佳化化学)，0.5质量份紫外线吸收剂UV-328，0.5质量份I rganox245,0.5质量份光稳定剂292，0.4质量份色浆组合物，4.0质量份3000目滑石粉，0.5质量份聚碳化二亚胺UN-025，充分混合均匀，110℃下抽真空除水0.5h；
步骤3，弹性体的制备：
将A组分加热至100℃，并加入B组分快速搅拌，A/B组份重量比＝200:66.6，充分混合，在确保无气泡的情况下倒入110℃的模具中，达到凝胶点后合模，放入110℃环境中固化16h，室温放置至7天，得到聚脲弹性体。
实施例2
一种聚脲弹性体
步骤1，A组分(NCO封端预聚体)的制备：
将80重量份聚己二酸乙二醇酯(Mw＝2000)；100质量份聚四氢呋喃醚二醇(Mw＝2000)，20质量份聚丙二醇(Mw＝2000)，0.3质量份抗氧剂于反应釜中，加热至110℃，充分搅拌下抽真空除水0.5h；降温至70℃，加入60质量份MDI-50，N2保护条件下，90-110℃反应2h，测定NCO含量为4.23％，粘度＝9820mPa.S(60℃)，将预聚体密封保存；
步骤2，B组分(扩链剂)的制备
将15重量份MOCA，3质量份HQEE，40质量份Puranol G 5030(佳化化学)，1.0质量份紫外线吸收剂UV-328，0.5质量份Irganox245，0.4质量份色浆组合物，4.0质量份3000目滑石粉，0.5质量份硅烷偶联剂KH560。充分混合均匀，110℃下抽真空除水0.5h；
步骤3，弹性体的制备：
将A组分加热至100℃，并加入B组分快速搅拌，A/B组份重量比＝200:64.7，充分混合，在确保无气泡的情况下倒入110℃的模具中，达到凝胶点后合模，放入110℃环境中固化16h，室温放置至7天，得到聚脲弹性体。
实施例3
一种聚脲弹性体
步骤1，A组分(NCO封端预聚体)的制备：
将20重量份聚己二酸乙二醇酯(Mw＝2000)，50重量份聚己内酯(Mw＝2000)，100质量份聚四氢呋喃醚二醇(Mw＝2000)，30质量份聚碳酸酯(Mw＝2000)，0.4质量份抗氧剂于反应釜中，加热至110℃，充分搅拌下抽真空除水0.5h；降温至70℃，加入60质量份MDI-50，N2保护条件下，90-110℃反应2h，测定NCO含量为7.23％，粘度＝5320mPa.S(60℃)，将预聚体密封保存；
步骤2，B组分(扩链剂)的制备：
将15重量份MOCA，10质量份蓖麻油，40质量份Puranol G 4030(佳化化学)，15质量份Unilink 42006，0.5质量份紫外线吸收剂UV-328，0.5质量份Irganox245，0.4质量份色浆组合物，2.6质量份3000目滑石粉，充分混合均匀，110℃下抽真空除水0.5h；
步骤3，弹性体的制备：
将A组分加热至100℃，并加入B组分快速搅拌，A/B组份重量比＝200:81.7，充分混合，在确保无气泡的情况下倒入110℃的模具中，达到凝胶点后合模，放入110℃环境中固化16h，室温放置至7天，得到聚脲弹性体。
实施例4
一种聚脲弹性体
步骤1，A组分(NCO封端预聚体)的制备：
将100重量份聚己二酸乙二醇酯(Mw＝2000)，40重量份聚己内酯(Mw＝2000)，60质量份聚四氢呋喃醚二醇(Mw＝2000)，10质量份Puranol G310，0.3质量份抗氧剂于反应釜中，加热至110℃，充分搅拌下抽真空除水0.5h；降温至70℃，加入50质量份HDI，N2保护条件下，90-110℃反应2h，测定NCO含量为5.62％，粘度＝8600mPa.S(60℃)，将预聚体密封保存；
步骤2，B组分(扩链剂)的制备
将18重量份MOCA，10质量份蓖麻油，30质量份Puranol G 5030(佳化化学)，5质量份E-300，0.6质量份紫外线吸收剂UV-765，0.5质量份Irganox245，0.5质量份光稳定剂292，0.4质量份色浆组合物，2.0质量份3000目滑石粉，充分混合均匀，110℃下抽真空除水0.5h；
步骤3，弹性体的制备：
将A组分加热至100℃，并加入B组分快速搅拌，A/B组份重量比＝200:63，充分混合，在确保无气泡的情况下倒入110℃的模具中，达到凝胶点后合模，放入110℃环境中固化16h，室温放置至7天，得到聚脲弹性体。
对比例1
步骤1，A组分(NCO封端预聚体)的制备：
将100重量份聚己二酸乙二醇酯(Mw＝2000)，40重量份聚己内酯(Mw＝2000)，60质量份聚四氢呋喃醚二醇(Mw＝2000)，10质量份Puranol G310，0.3质量份抗氧剂于反应釜中，加热至110℃，充分搅拌下抽真空除水0.5h；降温至70℃，加入50质量份HDI，N2保护条件下，90-110℃反应2h，测定NCO含量为5.62％，粘度＝8600mPa.S(60℃)，将预聚体密封保存；
步骤2，B组分(扩链剂)的制备
将13重量份HQEE，10质量份蓖麻油，30质量份Puranol G 5030(佳化化学)，2质量份1,4-丁二醇，0.6质量份紫外线吸收剂UV-765，0.5质量份Irganox245，0.5质量份光稳定剂292，0.4质量份色浆组合物，2.0质量份3000目滑石粉，充分混合均匀，110℃下抽真空除水0.5h；
步骤3，弹性体的制备：
将A组分加热至100℃，并加入B组分快速搅拌，A/B组份重量比＝200:63，充分混合，在确保无气泡的情况下倒入110℃的模具中，达到凝胶点后合模，放入110℃环境中固化16h，室温放置至7天，得到聚脲弹性体。
性能检测
将实施例1-4中的聚酯弹性体进行性能检测
硬度/邵A 拉伸强度/Mpa 断裂伸长率
实施例1 74 39 790％
实施例2 72 36 840％
实施例3 74 48 650％
实施例4 68 31 920％
对比例1 35 2.2 620％
其中，机械性能测试参照GBT/528-2009，硬度测试参照GBT/1698-2003。
可以理解的是，以上关于本发明的具体描述，仅用于说明本发明而并非受限于本发明实施例所描述的技术方案。本领域的普通技术人员应当理解，仍然可以对本发明进行修改或等同替换，以达到相同的技术效果；只要满足使用需要，都在本发明的保护范围之内。

Claims (9)

1.一种风能风机叶片用聚脲弹性体的制备方法，其特征在于：将含NCO封端的预聚体与扩链剂反应得到聚脲弹性体，然后采用浇注工艺形成最终产品。
2.根据权利要求1所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述方法的具体步骤如下：
步骤1，将含NCO封端的预聚体加热40-120℃，并将其作为A组分；将扩链剂加热至40-130℃，并将其作为B组分；
步骤2，将A组分和B组分快速搅拌，充分混合并确保无气泡产生，然后倒入至90-130℃的模具中；
步骤3，弹性体在90-130℃的模具中固化0.15-3h后脱模，并在110℃硫化16h以上，室温静置7天后得到聚脲弹性体产品。
3.根据权利要求2所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述扩链剂采用胺类扩链剂、醇类扩链剂、醇胺类扩链剂、三官聚醚大分子中的一种或几种。
4.根据权利要求2所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述步骤2中的A组分与B组分的摩尔比为0.95-1.45。
5.根据权利要求4所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：A组分与B组分的摩尔比为1.05-1.3。
6.根据权利要求2所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述步骤1中的B组分还设置有助剂，且该助剂包括填料、色浆、抗老化助剂、阻燃剂、除水剂等其他有助于加工的助剂或功能性助剂，助剂加入量是B组分质量的0.5-10％。
7.根据权利要求2所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述A组分的制备方法，包括如下步骤：
步骤a，将多元醇和第二助剂加入至反应容器内，充分搅拌并加热至100-120℃除水0.5h以上；
步骤b，将反应容器降温至50-80℃，然后加入多异氰酸酯，并在80-110℃反应2-3h；
步骤c，经检测预聚体内NCO含量，达标后密封保存待用。
8.根据权利要求1所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述聚脲弹性体机械性能如下：拉伸强度大于30Mpa，断裂伸长率大于600％，硬度60-84A。
9.根据权利要求1所述的风能风机叶片用聚脲弹性体的制备方法，其特征在于：所述聚脲弹性体用于风能风机叶片保护套。
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