CN110157518A - 一种改性氧化石墨烯在拉丝液中的应用和拉丝液及其制备方法 - Google Patents
一种改性氧化石墨烯在拉丝液中的应用和拉丝液及其制备方法 Download PDFInfo
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- CN110157518A CN110157518A CN201910319377.6A CN201910319377A CN110157518A CN 110157518 A CN110157518 A CN 110157518A CN 201910319377 A CN201910319377 A CN 201910319377A CN 110157518 A CN110157518 A CN 110157518A
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- wire drawing
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- graphene oxide
- modified graphene
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1896—Compounds having one or more Si-O-acyl linkages
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M139/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00
- C10M139/04—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing atoms of elements not provided for in groups C10M127/00 - C10M137/00 having a silicon-to-carbon bond, e.g. silanes
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M173/00—Lubricating compositions containing more than 10% water
- C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/11—Compounds covalently bound to a solid support
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/04—Elements
- C10M2201/041—Carbon; Graphite; Carbon black
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
- C10M2201/14—Inorganic compounds or elements as ingredients in lubricant compositions inorganic compounds surface treated with organic compounds
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/02—Hydroxy compounds
- C10M2207/021—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
- C10M2207/022—Hydroxy compounds having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms containing at least two hydroxy groups
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
- C10M2207/10—Carboxylix acids; Neutral salts thereof
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Abstract
本发明涉及金属加工技术领域，具体公开一种改性氧化石墨烯在拉丝液中的应用和拉丝液及其制备方法。所述改性氧化石墨烯由质量比为8‑12:1的氨基硅氧烷与氧化石墨烯制得，所述拉丝液包括所述的改性氧化石墨烯。本发明提供的拉丝液对环境友好，具有良好的润滑性能，极压耐磨性好，抗腐蚀性好，贮存稳定性好，能满足金属工件在高速拉拔时对拉丝液的需求。
Description
技术领域
本发明涉及金属加工技术领域，尤其涉及一种改性氧化石墨烯在拉丝液中的应用和拉丝液及其制备方法。
背景技术
金属线材拉拔时的润滑剂，通常分为两种：干式拉丝润滑剂(俗称拉丝粉、拔丝粉)和湿式拉丝润滑剂(水相拉丝润滑剂)，其中，拉丝液作为湿式拉丝润滑剂，由于其以水溶液形式存在，具有较好的水冷效果，可形成较薄的润滑膜，使金属丝表面光洁度好，成为现阶段研究的主要方向。
目前，拉丝液中多含有硫、磷、氯等元素，对环境污染性较大。为满足当今社会对节能、环保日益苛刻的要求，对拉丝液提出了以下几点要求：热氧化安定性好、挥发性低、粘度指数高、低硫或无硫、黏度低、对环境友好。因此，继续研究并开发新型或改进型拉丝液意义重大。
发明内容
针对现有拉丝液中多含有硫、磷、氯等元素，污染环境以及拉丝液热氧化稳定性差等问题，本发明提供一种改性氧化石墨烯在拉丝液中的应用和拉丝液及其制备方法。
为达到上述发明目的，本发明实施例采用了如下的技术方案：
一种改性氧化石墨烯在拉丝液中的应用，所述改性氧化石墨烯由质量比为8-12:1的氨基硅氧烷与氧化石墨烯制得，用于拉丝液的极压耐磨剂中。
进一步地，所述氧化石墨烯为纯度>95％，厚度为0.335-1.0nm，碳含量40-45％，氧含量45-60％，硫含量<1.5％，片层直径0.2-10μm，层数为1-5层的纳米氧化石墨烯，控制硫含量，有助于减小环境污染，控制氧化石墨烯中的氧含量，保证有充足的含氧官能团与氨基硅氧烷进行反应，引入极压元素(极压剂中的活性元素N)，得到改性氧化石墨烯石墨烯，此外，石墨烯具备自润滑性能，且具有优异的机械强度和拓扑结构，在金属表面形成氧化石墨烯膜，起到自润滑减磨、抗磨作用，与极压元素共同作用改善拉丝液的润滑性和耐磨性。
进一步地，所述改性氧化石墨烯的制备方法为：所述氨基硅氧烷水解后与所述氧化石墨烯发生脱水缩合反应得到改性氧化石墨烯。
进一步地，所述脱水缩合反应的温度为65℃-80℃，时间为6h-12h。
进一步地，所述氨基硅氧烷为γ-氨丙基三乙氧基硅烷、γ-氨丙基三甲氧基硅烷、N-(β氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基甲基二乙氧基硅烷、N-(β氨乙基)-γ-氨丙基三乙氧基硅烷、N-(β氨乙基)-γ-氨丙基三甲氧基硅烷、γ-二乙烯三胺丙基甲基二甲氧基硅烷、N-苯基-γ-氨丙基三甲氧基硅烷或仲氨基硅烷中的至少一种。
进一步地，所述改性氧化石墨烯的制备方法为：在水和醇比例为1-2:1的混合体系中，加入质量比为8-12:1的氨基硅氧烷与氧化石墨烯，加热至65℃-80℃，反应6h-12h，在该反应体系中，氨基硅氧烷遇水先发生水解反应，然后与氧化石墨烯发生脱水缩合反应，反应结束后用蒸馏水洗涤、烘干，得到改性氧化石墨烯。反应流程如下(以γ―氨丙基三乙氧基硅烷为例)：
本发明还提供了一种拉丝液，包括上述的改性氧化石墨烯。
进一步地，所述的拉丝液，包括质量分数如下的原料组分：油性剂10％-20％；极压耐磨剂5％-15％；抗氧剂0.5％-3％；乳化剂13％-20％；消泡剂0.05％-0.5％；防锈剂5％-8％；蒸馏水余量，所述极压耐磨剂为质量比为0.6-1.6:1的所述改性氧化石墨烯与过碱性磺酸盐的混合物。
进一步地，所述过碱性磺酸盐为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡、二壬基萘磺酸钙中的至少一种。
进一步地，所述油性剂为丙三醇、十二醇、十六醇、硬脂酸、蓖麻油酸、硬脂酸钙、硬脂酸钠、蓖麻油酸钠或三羟甲基丙烷油酸酯中的至少一种。
进一步地，所述乳化剂为壬基酚聚氧乙烯醚、卞基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、脂肪胺聚氧乙烯醚、脂肪酸环氧乙烷加成物或蓖麻油环氧乙烷加成物中的至少一种，采用两相混合法，有助于油相与水相自发的形成以O/W或W/O的形式存在的分散体，得到透明或半透明的体系。所述抗氧剂为二苯胺、二异辛基二苯胺、β-萘胺、N-苯基-α-萘胺、2,6-二叔丁基对甲苯酚或十二烷基砷中的至少一种；所述消泡剂为二甲基硅油；所述防锈剂为十二烯基丁二酸、十二烯基丁二酸半酯或苯并三氮唑中的至少一种。
本发明还提供了上述拉丝液的制备方法，包括以下步骤：
将所述油性剂、极压耐磨剂、抗氧剂、乳化剂、消泡剂、防锈剂混合后，升温至70℃-85℃，搅拌均匀，加入所述蒸馏水，继续搅拌进行乳化至体系均一透明，得到拉丝液原液。
进一步地，在加入蒸馏水之前以500-700r/min搅拌0.5-1.5h，加入蒸馏水后，以1000-1500r/min搅拌2.5-3.5h，至体系均匀。
使用时将拉丝液原液与蒸馏水按1:5-10混合均匀，即为使用所用拉丝液。
相对于现有技术，采用本发明提供的技术方案，可以获得功能化的改性氧化石墨烯，与过碱性磺酸盐配合使用作为极压耐磨剂。过碱性磺酸盐对金属无腐蚀性且不污染环境，氨基硅氧烷改性氧化石墨烯中的极压元素为氮元素，也不会对环境产生不良影响，且纳米级石墨烯的使用能够有效对减小金属间的边界摩擦。同时，由于磺酸盐中的硫元素与改性氧化石墨烯中的氮元素的协同作用，可以形成硫-氮系多种元素极压添加剂，所形成的极压添加剂的承载能力强，同时具有一定的抗氧化与防锈的能力。将改性氧化石墨烯与过碱性磺酸盐用于拉丝液中，与抗氧剂、防锈剂等助剂共同作用，使拉丝液具有较好的抗腐蚀性，热氧化稳定性，且在贮存过程中性能稳定；该拉丝液在使用中以水溶液形式存在，具有较好的水冷效果，且挥发性较小，有毒污染物排放量少，对环境污染小，在金属表面能形成稳定的润滑薄膜，对拉丝面磨损较小，并对于钢帘线表面腐蚀性较小；所的产品表面光洁度好，具有较好的防锈性能。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。
实施例1
一种改性氧化石墨烯，由质量比为10:1的γ-氨丙基三乙氧基硅烷与氧化石墨烯制得，所述氧化石墨烯是层数为1层的纳米氧化石墨烯，片层直径0.2-2μm，纯度97％，厚度为0.335-0.5nm，碳含量43％，氧含量45％，硫含量1.2％，制备过程如下：
重量比为10:1的γ-氨丙基三乙氧基硅烷与氧化石墨烯加入到乙醇和水比例为1:1的混合体系中，加热至70℃，水解后的γ-氨丙基三乙氧基硅烷与氧化石墨烯发生脱水缩合反应，反应10h后，用蒸馏水洗涤，得到γ-氨丙基三乙氧基硅烷改性氧化石墨烯。
实施例2
一种改性氧化石墨烯，由质量比为8:1的γ-氨丙基甲基二甲氧基硅烷与氧化石墨烯制得，所述氧化石墨烯是层数为3层的纳米氧化石墨烯，片层直径3-6μm，纯度98％，厚度为0.7-1.0nm，碳含量40％，氧含量50％，硫含量1.0％，制备过程如下：
重量比为8:1的γ-氨丙基甲基二甲氧基硅烷与氧化石墨烯加入到乙醇和水比例为2:1的混合体系中，加热至80℃，水解后的γ-氨丙基甲基二甲氧基硅烷与氧化石墨烯发生脱水缩合反应，反应6h后，用蒸馏水洗涤，得到γ-氨丙基甲基二甲氧基硅烷改性氧化石墨烯。
实施例3
一种改性氧化石墨烯，由质量比为12:1的γ-氨丙基三甲氧基硅烷与氧化石墨烯制得，所述氧化石墨烯是层数为5层的纳米氧化石墨烯，片层直径7-10μm，纯度96％，厚度为0.6-0.8nm，碳含量45％，氧含量60％，硫含量1.1％，制备过程如下：
重量比为12:1的γ-氨丙基三甲氧基硅烷与氧化石墨烯加入到乙醇和水比例为2:1的混合体系中，加热至65℃，水解后的γ-氨丙基三甲氧基硅烷与氧化石墨烯发生脱水缩合反应，反应12h后，用蒸馏水洗涤，得到γ-氨丙基三甲氧基硅烷改性氧化石墨烯。
实施例4
一种拉丝液，包括质量分数如表1所示的原料组分：
表1
上述拉丝液的制备方法，包括以下步骤：
将上述油性剂、极压耐磨剂、抗氧剂、乳化剂、消泡剂、防锈剂混合后，升温至85℃，以600r/min搅拌1h，缓慢地加入蒸馏水，蒸馏水加入完毕后，以1200r/min继续搅拌3h，至体系均匀透明，得到拉丝液原液。
使用时将拉丝液原液与蒸馏水按1:5混合均匀，即为使用所用拉丝液。
实施例5
一种拉丝液，包括质量分数如表2所示的原料组分：
表2
上述拉丝液的制备方法，包括以下步骤：
将上述油性剂、极压耐磨剂、抗氧剂、乳化剂、消泡剂、防锈剂混合后，升温至80℃，以600r/min搅拌0.5h，缓慢地加入蒸馏水，蒸馏水加入完毕后，以1500r/min继续搅拌2.5h，至体系均匀透明，得到拉丝液原液。
使用时将拉丝液原液与蒸馏水按1:8混合均匀，即为使用所用拉丝液。
实施例6
一种拉丝液，包括质量分数如表3所示的原料组分：
表3
上述拉丝液的制备方法，包括以下步骤：
将上述油性剂、极压耐磨剂、抗氧剂、乳化剂、消泡剂、防锈剂混合后，升温至70℃，以700r/min搅拌1.5h，缓慢地加入蒸馏水，蒸馏水加入完毕后，以1000r/min继续搅拌3.5h，至体系均匀透明，得到拉丝液原液。
使用时将拉丝液原液与蒸馏水按1:10混合均匀，即为使用所用拉丝液。
实施例7-11
实施例7-11提供的拉丝液，包括质量分数如表4所示的原料组分：
表4
上述拉丝液的制备方法与实施例4相同。
为了更好的说明本发明实施例提供的拉丝液的特性，下面将实施例4-6制备的拉丝液进行相应性能的测试，结果如表5所示。
表5
注：1.耐磨性测试标准：GB/T12583-98；2.铜片腐蚀测试标准：GB-T 7326。
由以上数据可知，本发明实施例提供的拉丝液对环境友好，具有良好的润滑性能，极压耐磨性好，抗腐蚀性好，贮存稳定性好，能满足金属工件在高速拉拔时对拉丝液的需求。实施例7-11中得到的拉丝液的性能与实施例4-6中相当。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换或改进等，均应包含在本发明的保护范围之内。
Claims (10)
1.一种改性氧化石墨烯在拉丝液中的应用，其特征在于：所述改性氧化石墨烯由质量比为8-12:1的氨基硅氧烷与氧化石墨烯制得，用于拉丝液的极压耐磨剂中。
2.如权利要求1所述的改性氧化石墨烯在拉丝液中的应用，其特征在于，所述改性氧化石墨烯的制备方法为：所述氨基硅氧烷水解后与所述氧化石墨烯发生脱水缩合反应得到改性氧化石墨烯。
3.如权利要求2所述的改性氧化石墨烯在拉丝液中的应用，其特征在于：所述脱水缩合反应的温度为65℃-80℃，时间为6h-12h。
4.如权利要求1所述的改性氧化石墨烯在拉丝液中的应用，其特征在于：所述氨基硅氧烷为γ-氨丙基三乙氧基硅烷、γ-氨丙基三甲氧基硅烷、N-(β氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基甲基二甲氧基硅烷、γ-氨丙基甲基二乙氧基硅烷、N-(β氨乙基)-γ-氨丙基三乙氧基硅烷、N-(β氨乙基)-γ-氨丙基三甲氧基硅烷、γ-二乙烯三胺丙基甲基二甲氧基硅烷、N-苯基-γ-氨丙基三甲氧基硅烷或仲氨基硅烷中的至少一种。
5.一种拉丝液，其特征在于：包括权利要求1-4任一项中所述的改性氧化石墨烯。
6.如权利要求5所述的拉丝液，其特征在于：包括质量分数如下的原料组分：油性剂10％-20％；极压耐磨剂5％-15％；抗氧剂0.5％-3％；乳化剂13％-20％；消泡剂0.05％-0.5％；防锈剂5％-8％；蒸馏水余量，所述极压耐磨剂为质量比为0.6-1.6:1的所述改性氧化石墨烯与过碱性磺酸盐的混合物。
7.如权利要求6所述的拉丝液，其特征在于：所述过碱性磺酸盐为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡或二壬基萘磺酸钙中的至少一种。
8.如权利要求6所述的拉丝液，其特征在于：所述油性剂为丙三醇、十二醇、十六醇、硬脂酸、蓖麻油酸、硬脂酸钙、硬脂酸钠、蓖麻油酸钠或三羟甲基丙烷油酸酯中的至少一种。
9.如权利要求6所述的拉丝液，其特征在于：所述乳化剂为壬基酚聚氧乙烯醚、卞基酚聚氧乙烯醚、苯乙基酚聚氧乙烯醚、脂肪醇聚氧乙烯醚、脂肪胺聚氧乙烯醚、脂肪酸环氧乙烷加成物或蓖麻油环氧乙烷加成物中的至少一种；所述抗氧剂为二苯胺、二异辛基二苯胺、β-萘胺、N-苯基-α-萘胺、2,6-二叔丁基对甲苯酚或十二烷基砷中的至少一种；所述消泡剂为二甲基硅油；所述防锈剂为十二烯基丁二酸、十二烯基丁二酸半酯或苯并三氮唑中的至少一种。
10.权利要求6～9任一项所述的拉丝液的制备方法，其特征在于：包括以下步骤：
将所述油性剂、极压耐磨剂、抗氧剂、乳化剂、消泡剂、防锈剂混合后，升温至70℃-85℃，搅拌均匀，加入所述蒸馏水，继续搅拌进行乳化至体系均一透明，得到拉丝液原液。
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