CN114106587A - 一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法 - Google Patents
一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法 Download PDFInfo
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 78
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title claims abstract description 76
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- 229920002545 silicone oil Polymers 0.000 claims abstract description 34
- -1 methyl hydrogen Chemical class 0.000 claims abstract description 33
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 31
- 239000001257 hydrogen Substances 0.000 claims abstract description 31
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 17
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 6
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 150000002632 lipids Chemical class 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
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- 238000005303 weighing Methods 0.000 claims description 6
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- QLVWOKQMDLQXNN-UHFFFAOYSA-N dibutyl carbonate Chemical compound CCCCOC(=O)OCCCC QLVWOKQMDLQXNN-UHFFFAOYSA-N 0.000 claims description 4
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 4
- PKPOVTYZGGYDIJ-UHFFFAOYSA-N dioctyl carbonate Chemical compound CCCCCCCCOC(=O)OCCCCCCCC PKPOVTYZGGYDIJ-UHFFFAOYSA-N 0.000 claims description 4
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- 239000002994 raw material Substances 0.000 abstract description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003889 chemical engineering Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 231100000086 high toxicity Toxicity 0.000 abstract description 2
- 229910052749 magnesium Inorganic materials 0.000 abstract description 2
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
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- 238000012360 testing method Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 3
- 239000000347 magnesium hydroxide Substances 0.000 description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 3
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- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000010459 dolomite Substances 0.000 description 2
- 229910000514 dolomite Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
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- 239000001095 magnesium carbonate Substances 0.000 description 2
- 235000014380 magnesium carbonate Nutrition 0.000 description 2
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 2
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
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- 229910000976 Electrical steel Inorganic materials 0.000 description 1
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- 239000004566 building material Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
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- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
本发明属于镁基材料与化学工程的结合应用中溶剂的选择及改性领域,具体涉及一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,配方成分按重量百分比为:电工级氧化镁90‑99%,甲基含氢硅油、酯类溶剂和气相二氧化硅三者总和占1‑10%,三者之间的重量比为1~10:0.3~5:1~10。合成方法采用的是常温混合法,以廉价易得的氧化镁砂、甲基含氢硅油为原料,选择低碳类脂类为稀释剂,取代毒性较大的二甲苯溶剂,在常温条件下优化电工级覆膜氧化镁。该方法原料简单,供货渠道稳定,操作简单,环保无毒,适合化工企业大规模生产。
Description
技术领域
本发明属于镁基材料与化学工程的结合应用中溶剂的选择及改性领域,具体涉及一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法。
技术背景
氧化镁呈白色粉末,无味,无臭,无毒,是一种典型的碱土金属氧化物。它在自然界中主要以菱镁矿、白云石,氯化镁矿石形式存在。通过热解菱镁矿或白云石或用消石灰处理得到氢氧化镁,灼烧氢氧化镁得到氧化镁。氧化镁随着高新技术功能材料市场发展需求,主要分为食品级、药品级、硅钢级、轻烧、高纯氧化镁等产品,被广泛应用于建材,电子,医学,机械,农业等领域。氧化镁具有高的熔点(2852℃)和沸点(3600℃),结构性能稳定,具有很好的耐碱性、电绝缘性、热膨胀系数和导热率,在成为电工级氧化镁之后,常被作为高温耐热材料或绝缘材料。然而,氧化镁易于吸潮结块,导致氧化镁粉末团聚,结块变脆,品级下降无法使用,吸收二氧化碳使溶解度增加与水反应生成氢氧化镁,使绝缘电阻迅速下降,容易发生电流泄露,引发安全事故。
甲基含氢硅油是硅油中重要产品之一,现已成为国内、外十分畅销的有机硅产品。然而,甲基含氢硅油与甲基羟基硅油乳液共用,虽然可以防水,但是导致其具有高粘性和弱流动性,使氧化镁覆膜后的粉体易于粘连成块,降低产品的持久性。传统的工艺方法使用甲苯、二甲苯等有机溶剂来稀释甲基含氢硅油,但因其的毒性大,故此寻找一种环保型的稀释剂也成为了工业生产的重要需求之一。溶剂类涂料使用寿命长,具有优异的覆膜特性,对环境的适应能力强,常常被应用于涂料工业中。
发明内容
本发明的目的是提供一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,克服现有技术的不足,采用常温混合法,使用环保型酯类溶剂,在室温下制备电工级覆膜氧化镁,用作电缆绝缘层填料与电热管绝缘层填料。
为了实现上述技术目的,本发明是采用以下方案实现的:
技术方案之一:一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,配方成分按重量百分比为:电工级氧化镁90-99%,甲基含氢硅油、酯类溶剂和气相二氧化硅三者总和占1-10%,三者之间的重量份比为1~10:0.3~5:1~10。所述脂类溶剂是邻苯二甲酸二丁酯、碳酸二甲酯、碳酸二丁酯、碳酸二乙酯、碳酸二辛酯中的任一种。所述电工级氧化镁中氧化镁的含量≥97%。所述甲基含氢硅油为工业级。所述酯类溶剂为工业级。
技术方案之二:一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,其制备步骤如下:1)取电工级氧化镁,将其置于80~90℃的烘箱中加热1~2h,除去其吸收的水分,处理得到干燥的氧化镁,转入干料搅拌器中;2)称量全部配方量的甲基含氢硅油和酯类溶剂混合均匀,缓缓倒入干料搅拌器中,然后称量气相二氧化硅并加入干料搅拌器中;3)将干料搅拌器转速设定为50~75r/min,时间设定为60~80分钟,充分搅拌;4)将3)中混合均匀后的产物取出后,室温摊平晾晒30~60分钟,即得到电工级覆膜氧化镁产品,产品表面包裹一层通过脂类溶剂稀释后的甲基含氢硅油,氧化镁直径为1-2µm,甲基含氢硅油膜的厚度为10-20nm。
所述的电工级覆膜氧化镁在电热管和电缆的制备中添加量按重量百分比计为1~5%。
与现有技术相比,本发明的有益效果是:
1)由电工级氧化镁与甲基含氢硅油、脂类溶剂作为稀释剂、气相二氧化硅作为润滑粉制备而成,工业原料廉价易得,通过干料常温搅拌后晾晒处理即可使用,常温操作,节能且操作简便。
2)本专利选择邻苯二甲酸二丁酯、碳酸二甲酯、碳酸二丁酯、碳酸二乙酯、碳酸二辛酯中的任一种溶剂取代有毒的二甲苯制备电工级氧化镁。这些脂类溶剂不溶于水,不与甲基含氢硅油和氧化镁反应,因此可作为硅油的稀释剂,降低硅油的粘性,达到分散效果,将氧化镁颗粒均匀包裹形成疏水膜。气相二氧化硅银企比表面积大,吸附性强,在本发明中作为润滑粉,用来改善电工级氧化镁的流动性。
3)本发明制备出的电工级覆膜氧化镁是在原始的电工级氧化镁基础上,添加甲基含氢硅油,基于甲基含氢硅油的低温成膜特性,增加了材料的疏水性,使覆膜后的氧化镁具有良好的绝缘性。
4)环保型脂类溶剂取代常用毒性二甲苯稀释剂,覆膜氧化镁材料作为绝缘层填料应用于电缆可有效的防止电流泄露,应用于电热管可使热传递效应明显提升,应用于加热管可增强电阻,通过了漏电、流速、绝缘、耐压、防水测试等专业测试,在电加热管、电缆领域具有广阔前景。
具体实施方式
下面结合实施例对本发明的实施方式作进一步说明:
下面将详细地描述本公开的示例性实施方式,然而应当理解,可以以各种形式实现本公开而不应被这里阐述的实施方式所限制。相反,提供这些实施方式是为了能够更透彻地理解本公开,并且能够将本公开的范围完整的传达给本领域的技术人员。
实施例1
一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,配方成分按重量百分比为:电工级氧化镁98.86%,甲基含氢硅油、酯类溶剂和气相二氧化硅三者总和占1.14%,三者之间的重量比为1:0.3:1,具体制备过程如下:
1)取200g电工级氧化镁,将其置于80℃烘箱中加热1h,除去其吸收的水分,得到干燥的电工级氧化镁,转入2L的干料搅拌器中;
2)称量1g甲基含氢硅油和0.3g邻苯二甲酸二丁酯置于试管中混合均匀,缓缓倒入干料搅拌器中,然后称量1g气相二氧化硅并加入干料搅拌器中;
3)将干料搅拌器转速设定为50r/min,时间设定为60分钟,以便于充分搅拌;
4)将3)混合均匀后的产物取出后,室温摊平晾晒30分钟,即得到目标产物覆膜电工级氧化镁。作为实施例1。
实施例2
将2)中的酯类溶剂调整为碳酸二甲酯,其余条件均不变,将生产出的产品作为实施例2;
实施例3
将2)中的酯类溶剂调整为碳酸二乙酯,其余条件均不变,将生产出的产品作为实施例3;
实施例4
将2)中的酯类溶剂调整为碳酸二丁酯,其余条件均不变,将生产出的产品作为实施例4;
实施例5
将2)中的酯类溶剂调整为碳酸二辛酯,其余条件均不变,将生产出的产品作为实施例5。
实施例效果展示:
以上实施例中,本发明以电工级氧化镁为原料,甲基含氢硅油为改性剂,酯类溶剂作为稀释剂,气相二氧化硅作为润滑粉,将甲基含氢硅油、酯类溶剂和气相二氧化硅与氧化镁颗粒混合,在电工级氧化镁颗粒上包裹有一层甲基含氢硅油-气相二氧化硅薄膜,使得该电工级氧化镁在具有自身特性的同时,也提高了样品的疏水性,在空气中长时间保持干燥不团聚。
将市售的某品牌电工级氧化镁作为对比例与本发明生产出的氧化镁装入电缆中,对其进行一系列性能测试。实验过程动/静态流速测试与绝缘性能测试参数对比见如下表1和表2。
表1 动/静态流速测试参数对比:
表2 绝缘性能测试参数对比:
技术总结:本发明使用环保型酯类溶剂制备电工级覆膜氧化镁的制备方法,通过调整酯类溶剂用量稀释甲基含氢硅油,降低甲基含氢硅油的粘度,均匀涂覆在氧化镁的表面。产品达到流速大,在常态绝缘性良好,潮态浸水后电阻衰退不明显,依然能保持优异的绝缘性。通过选择酯类溶剂作为稀释剂,气象二氧化硅作为润滑剂。使得工业上电工级覆膜氧化镁具有较好的流动性和较高的阻抗值,作为电缆的绝缘层填料,可以导热,绝缘,降低环境污染以及有毒性溶剂的使用;通过酯类稀释剂与甲基含氢硅油的配比调控,使得电工级氧化镁在制成电缆后,具有优良的防潮性能并保留其绝缘性能。
Claims (7)
1.一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,配方成分按重量百分比为:电工级氧化镁90-99%,甲基含氢硅油、酯类溶剂和气相二氧化硅三者总和占1-10%,三者之间的重量份比为1~10:0.3~5:1~10。
2.根据权利要求1所述的一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,所述脂类溶剂是邻苯二甲酸二丁酯、碳酸二甲酯、碳酸二丁酯、碳酸二乙酯、碳酸二辛酯中的任一种。
3.根据权利要求1所述的一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,所述电工级氧化镁中氧化镁的含量≥97%。
4.根据权利要求1所述的一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,所述甲基含氢硅油为工业级。
5.根据权利要求1所述的一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,所述酯类溶剂为工业级。
6.一种用环保型酯类溶剂制备电工级覆膜氧化镁的方法,其特征在于,其制备步骤如下:
1)取电工级氧化镁,将其置于80~90℃的烘箱中加热1~2h,除去其吸收的水分,处理得到干燥的氧化镁,转入干料搅拌器中;
2)称量全部配方量的甲基含氢硅油和酯类溶剂混合均匀,缓缓倒入干料搅拌器中,然后称量气相二氧化硅并加入干料搅拌器中;
3)将干料搅拌器转速设定为50~75r/min,时间设定为60~80分钟,充分搅拌;
4)将3)中混合均匀后的产物取出后,室温摊平晾晒30~60分钟,即得到电工级覆膜氧化镁产品,产品表面包裹一层通过脂类溶剂稀释后的甲基含氢硅油,氧化镁直径为1-2µm,甲基含氢硅油膜的厚度为10-20nm。
7.一种用环保型酯类溶剂制备电工级覆膜氧化镁的应用,其特征在于,权利要求1-6所述的电工级覆膜氧化镁在电热管和电缆的制备中添加量按重量百分比计为1~5%。
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