WO2016112523A1 - Nanometer aluminium oxide modified insulation paper and preparation method thereof - Google Patents

Nanometer aluminium oxide modified insulation paper and preparation method thereof Download PDF

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WO2016112523A1
WO2016112523A1 PCT/CN2015/070835 CN2015070835W WO2016112523A1 WO 2016112523 A1 WO2016112523 A1 WO 2016112523A1 CN 2015070835 W CN2015070835 W CN 2015070835W WO 2016112523 A1 WO2016112523 A1 WO 2016112523A1
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nano
alumina
insulating paper
solution
preparing
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PCT/CN2015/070835
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French (fr)
Chinese (zh)
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吕彦冬
廖瑞金
赵学童
梁宁川
张珺彦
毕雷·克里斯多夫
库利巴利·马马杜-拉明
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阿尔斯通技术有限公司
吕彦冬
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Priority to PCT/CN2015/070835 priority Critical patent/WO2016112523A1/en
Publication of WO2016112523A1 publication Critical patent/WO2016112523A1/en

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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
    • D21H17/63—Inorganic compounds
    • D21H17/67—Water-insoluble compounds, e.g. fillers, pigments
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B17/00—Insulators or insulating bodies characterised by their form
    • H01B17/56—Insulating bodies
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B19/00—Apparatus or processes specially adapted for manufacturing insulators or insulating bodies
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F27/00—Details of transformers or inductances, in general
    • H01F27/28—Coils; Windings; Conductive connections
    • H01F27/32—Insulating of coils, windings, or parts thereof

Definitions

  • the invention relates to an insulating paper product and a preparation process thereof, in particular to a nano-alumina modified insulating paper capable of improving the breakdown performance of cellulose insulating paper and a preparation method thereof.
  • Insulating paper is an insulating material widely used in various electrical equipment such as cables and coils, and generally has good insulation properties and mechanical strength. Studies have been made in the prior art to improve the electrical properties of insulating paper by means of doping.
  • the electrical properties of the modified insulating paper doped with 9% montmorillonite were studied from three aspects of power frequency breakdown field strength, relative dielectric constant and partial discharge.
  • the doping of montmorillonite can significantly improve the breakdown strength of the insulating paper, reduce the relative dielectric constant of the insulating paper, and effectively suppress the generation and development of partial discharge of the oil-paper insulation system.
  • the montmorillonite added in this document is a substance on the micro-nano level.
  • this paper only examines the influence of montmorillonite on the relative dielectric constant of insulating paper, and its influence on the dielectric loss tan ⁇ of insulating paper is not examined.
  • the inventors of the present invention have taken a different approach to modify the insulating paper by nano-alumina to obtain improved electrical properties.
  • the inventors investigated the effects of different nano-alumina content on the AC breakdown field strength, relative dielectric constant and dielectric loss factor of insulating paper, and proposed that the addition of nano-alumina can improve the breakdown performance of insulating paper. Program.
  • a method for preparing a nano-alumina modified insulating paper comprising:
  • the solution is an ethanol solution
  • the step a further comprises ultrasonically oscillating the ethanol solution in which the nano-alumina is dissolved in a water bath.
  • the method for preparing the nano-alumina modified insulating paper further comprises surface treating the nano-alumina with a silane coupling agent.
  • the step of surface treating the nano-alumina with a silane coupling agent further comprises:
  • KH-550 silane coupling agent is added to the ethanol solution and stirred;
  • the nano-alumina has a mass of at least 5 times the mass of the silane coupling agent.
  • the step b further comprises dissociating the cellulose insulating paper 5 times in a fiber disintegrator at a time of 21,000 revolutions.
  • the step c further comprises ultrasonically oscillating and synthesizing the synthetic solution in the fiber disintegrator at a time of 21,000 revolutions for at least 10 minutes.
  • the step d further comprises:
  • the vacuum dried semi-finished paper is placed in a water of the zipper bag for a predetermined time to complete the preparation.
  • a nano-alumina modified insulating paper is provided, and the content of the nano-alumina in the nano-alumina modified insulating paper is 0.2 to 2%.
  • the content of the nano-alumina in the nano-alumina modified insulating paper is 1%.
  • the present invention utilizes nano-alumina to modify the insulating paper to improve the AC breakdown strength of the insulating paper and reduce the power-frequency relative dielectric constant and dielectric loss factor of the insulating paper.
  • This not only improves the breakdown resistance of the insulating paper, but also makes the relative dielectric constant of the insulating paper and the transformer mineral oil closer.
  • the distribution of the applied electric field in the oil-paper medium is more uniform, and the overall electrical properties of the oil-paper composite insulation system. The strength is higher; at the same time, the active and reactive losses of the insulating paper are reduced, thereby reducing the probability of occurrence of insulation failure.
  • Figure 1 is a flow chart showing the basic steps of a method for preparing a nano-alumina modified insulating paper of the present invention.
  • Figure 2 shows the relationship between the AC breakdown strength as a function of nano-alumina content.
  • Figure 3 shows the relative dielectric constant curves for different nano-alumina contents.
  • Figure 4 shows a plot of dielectric loss factor for different nano-alumina contents.
  • the inventors of the present invention furtherly studied the preparation process of the nanoparticle modified insulating paper based on the preparation platform of the insulating paper handsheet, and adopted the modified insulating paper which is prepared by adding different nanometer alumina contents and has not been modified.
  • the ordinary insulating paper is vacuum immersed in oil, and the AC breakdown field strength, relative dielectric constant and dielectric loss factor of each insulating paper are tested, thereby further obtaining a related preparation process and process parameters which can significantly improve the electrical properties of the insulating paper. .
  • the nano alumina modified insulating paper preparation method 100 mainly comprises: dissolving nano alumina (for example, ⁇ type, 30 nm, porous, highly dispersed, high activity nano alumina) to form a solution (step 101); Dissolving the cellulose insulating paper at least once to form a pulp solution (step 102); adding the solution in which the nano-alumina is dissolved to the pulp solution, and mechanically oscillating and synthesizing the synthesized synthetic solution for the purpose of modifying the nano-oxidation
  • the aluminum is uniformly distributed (step 103); and the nano-alumina modified insulating paper is formed using the synthetic solution mechanically oscillated and uniformly stirred (step 104).
  • a specific embodiment of the method for preparing nano-alumina modified insulating paper shown in FIG. 1 is discussed below in conjunction with a specific example.
  • step 101 a certain amount of nano-alumina that has been surface treated (this surface treatment will be discussed in more detail below) is weighed according to the alumina content required for the insulating paper to be prepared, and the nano-alumina is Dissolved in an ethanol solution, such as a solution of ethanol at a concentration of about 95%.
  • the ethanol solution in which the nano-alumina is dissolved may be further ultrasonically shaken, for example, in a KQ-100KDE type ultrasonic cleaner, and ultrasonically shaken in a water bath at about 70 degrees for about 10 minutes.
  • step 102 the cellulose insulating paper (ie, ordinary cellulose insulating paper) is dissociated in the fiber disintegrator at about 21,000 revolutions per time based on a known insulating paper handsheet forming platform. At least once, for example 5 times, to form a pulp solution. After the solution in which the nano-alumina is dissolved is added to the pulp solution, the synthesized solution is ultrasonically shaken and stirred at uniform for at least 10 minutes, step 103.
  • the dissociation modes in step 102 and step 103 may be the same, for example, or the number of rotations and the rotation mode in step 102 or step 103 may be arbitrarily adjusted as needed to meet the preparation requirements.
  • step 104 the dissociated synthetic solution is first formed and uncoated by a paper sheet former to obtain a semi-formed paper; and the semi-formed paper is vacuum dried, for example, a semi-formed paper is placed in a vacuum. Drying in a drying chamber at about 105 ° C for about 5 minutes to remove water and ethanol in the semi-formed paper; after that, the vacuum-dried semi-formed paper is placed in a water of the zipper bag for a predetermined time, such as 24 hours, to The preparation is completed to form a nano-alumina modified insulating paper.
  • the nano-alumina modified insulating paper preparation method 100 of the present invention may further comprise surface treating the nano-oxidation with a silane coupling agent prior to doping (ie, step 101 above).
  • the step of aluminum may further comprise surface treating the nano-oxidation with a silane coupling agent prior to doping (ie, step 101 above).
  • the step of surface treating the nano-alumina with a silane coupling agent may further comprise: silane coupling agent (based on linking nano-alumina and cellulose and increasing the degree of dispersion of the nano-alumina, preferably ammonia-based silane coupling Agent KH-550) is added to an ethanol solution (for example, a 95% ethanol solution) and then stirred; during the stirring process, nano-alumina is added, wherein the mass of the nano-alumina is preferably the mass of the KH-550 silane coupling agent At least 5 times, more preferably 10 times (for example, 5 g of nano-alumina and 0.5 g of KH-550 silane coupling agent are added to about 300 ml of a 95% ethanol solution for stirring); after stirring, KH- is mixed.
  • silane coupling agent based on linking nano-alumina and cellulose and increasing the degree of dispersion of the nano-alumina, preferably ammonia-based silane coupling Agent KH-550
  • KH-550 is added
  • Ultrasonic shaking of a solution bath of 550 silane coupling agent and nano-alumina for example, in the above-mentioned example in which 5 g of nano-alumina and 0.5 g of KH-550 silane coupling agent are added to a solution of about 300 ml of 95% ethanol for stirring, Ultrasonic shaking in a water bath at about 70 degrees for about 5 hours); and surface-treated nano-alumina is obtained after washing and drying, for example, the washing and drying steps can be repeated several times.
  • the modified insulating paper with different nano-alumina content (0.2%, 0.5%, 1%, 2%, 4%, 7%) is prepared and not
  • the modified ordinary insulating paper is subjected to vacuum immersion treatment, and the AC breakdown strength of the insulating paper is tested by a laboratory AC breakdown test platform, and the relative dielectric constant and dielectric loss of the insulating paper are tested by the laboratory Concept 80 broadband dielectric meter. Factor.
  • the relationship between the parameters and the change of nano-alumina content is shown in Figure 2-4.
  • the AC breakdown strength of the insulating paper As shown in Fig. 2, for the AC breakdown strength of the insulating paper, as the content of nano-alumina increases, the AC breakdown strength of the insulating paper gradually increases, and the breakdown strength reaches a maximum when the content reaches 1% (66.14). kV/mm), which is 10.8% higher than ordinary insulating paper (59.68kV/mm). Then, as the content of nano-alumina increases, the breakdown strength decreases rapidly, and after the content increases to 4%, the breakdown strength of the insulating paper is lower than that of the unmodified ordinary insulating paper.
  • the relative dielectric constant and dielectric loss factor of the insulating paper are continuously reduced with the increase of nano-alumina, especially at the power frequency, the 1% content of the nano-modified paper has Significantly lower. Its relative dielectric constant and dielectric loss factor were reduced from 2.43, 1.38x10 -2 (ordinary insulating paper) to 2.26, 0.739x10 -2 (modified insulating paper). In summary, compared with ordinary insulating paper, the dielectric constant of the modified insulating paper with a nano-alumina content of 1% is reduced by 7%, and the power-frequency dielectric loss factor is reduced by 46.4%.
  • the inventors of the present invention found that the content of nano-alumina in the modified insulating paper is about 0.2 ⁇ . At 2%, the doping can improve the breakdown performance of the insulating paper. In particular, the optimum addition ratio of nano-alumina in insulating paper is 1%. At this time, the alternating breakdown field strength of the modified insulating paper can be increased by 10.8%, the dielectric frequency dielectric constant can be reduced by 7%, and the power frequency dielectric loss can be reduced. The factor can be reduced by 46.4%.
  • the present invention utilizes nano-alumina to modify the insulating paper to improve the AC breakdown strength of the insulating paper and reduce the power-frequency relative dielectric constant and dielectric loss factor of the insulating paper.
  • This not only improves the breakdown resistance of the insulating paper, but also makes the relative dielectric constant of the insulating paper and the transformer mineral oil closer.
  • the distribution of the applied electric field in the oil-paper medium is more uniform, and the overall electrical properties of the oil-paper composite insulation system. The strength is higher; at the same time, the active and reactive losses of the insulating paper are reduced, thereby reducing the probability of occurrence of insulation failure.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Insulating Materials (AREA)
  • Inorganic Insulating Materials (AREA)
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Abstract

A method for preparing nanometer aluminium oxide modified insulation paper, comprising: preparing a nanometer aluminium oxide solution, dissociating cellulose insulation paper at least once to prepare a pulp solution, mixing the nanometer aluminium oxide solution with the pulp solution, mechanically oscillating and uniformly stirring the same, and preparing the nanometer aluminium oxide modified insulation paper. The content of the nanometer aluminium oxide in the modified insulation paper is 0.2-2%. The nanometer aluminium oxide is used to modify the insulation paper, thus increasing an alternating current breakdown strength of the insulation paper, and reducing a relative dielectric constant and dielectric loss factor of a power frequency.

Description

纳米氧化铝改性绝缘纸及其制备方法Nano alumina modified insulating paper and preparation method thereof 技术领域Technical field
本发明涉及一种绝缘纸产品及其制备工艺，尤其涉及一种可以提升纤维素绝缘纸的击穿性能的纳米氧化铝改性绝缘纸及其制备方法。The invention relates to an insulating paper product and a preparation process thereof, in particular to a nano-alumina modified insulating paper capable of improving the breakdown performance of cellulose insulating paper and a preparation method thereof.
背景技术Background technique
绝缘纸是广泛应用于电缆、线圈等各项电器设备的绝缘材料，其一般具有良好的绝缘性能和机械强度。在现有技术中已经出现了考虑通过掺杂的方式改善绝缘纸的电气特性的研究。Insulating paper is an insulating material widely used in various electrical equipment such as cables and coils, and generally has good insulation properties and mechanical strength. Studies have been made in the prior art to improve the electrical properties of insulating paper by means of doping.
例如，“蒙脱土改性绝缘纸的制备及其电气特性研究”(高电压技术,2014,40(1):33-39，廖瑞金,袁磊,张福州,杨丽君,汪可,段炼)中探究了蒙脱土的掺杂对绝缘纸电气特性的影响。该文献以实验室自制绝缘纸手抄片为原料制备出绝缘纸/蒙脱土复合材料，并根据改性绝缘纸的击穿场强和抗张强度随蒙脱土添加量的变化规律，确定了9％的蒙脱土最佳掺杂量。然后，从工频击穿场强、相对介电常数及局部放电三个方面对掺杂9％蒙脱土的改性绝缘纸的电气性能进行了研究。得到蒙脱土的掺杂能显著提高绝缘纸的击穿强度，降低绝缘纸的相对介电常数，有效抑制油纸绝缘系统局部放电的产生和发展。该文献所添加的蒙脱土为微纳米级别的物质。此外，对于绝缘纸的介电特性，该文献仅仅考察了蒙脱土对绝缘纸的相对介电常数的影响，未考察其对绝缘纸的介质损耗tanδ的影响。For example, "Preparation of montmorillonite modified insulating paper and its electrical properties" (High Voltage Technology, 2014, 40(1): 33-39, Liao Ruijin, Yuan Lei, Zhang Fuzhou, Yang Lijun, Wang Ke, Duan Lian) The influence of the doping of montmorillonite on the electrical properties of insulating paper was explored. In this paper, the insulating paper/montmorillonite composite material was prepared by using laboratory self-made insulating paper handsheet as raw material, and the breaking field strength and tensile strength of modified insulating paper were determined according to the variation law of montmorillonite addition amount. The optimum doping amount of 9% of montmorillonite. Then, the electrical properties of the modified insulating paper doped with 9% montmorillonite were studied from three aspects of power frequency breakdown field strength, relative dielectric constant and partial discharge. The doping of montmorillonite can significantly improve the breakdown strength of the insulating paper, reduce the relative dielectric constant of the insulating paper, and effectively suppress the generation and development of partial discharge of the oil-paper insulation system. The montmorillonite added in this document is a substance on the micro-nano level. In addition, for the dielectric properties of insulating paper, this paper only examines the influence of montmorillonite on the relative dielectric constant of insulating paper, and its influence on the dielectric loss tan δ of insulating paper is not examined.
发明内容Summary of the invention
本发明的发明人另辟蹊径，通过纳米氧化铝对绝缘纸进行改性，以获得改良的电气性能。特别是，发明人通过考察不同纳米氧化铝含量对绝缘纸的交流击穿场强、相对介电常数及介质损耗因数的影响，提出纳米氧化铝的少量添加可改善绝缘纸的击穿性能的优选方案。The inventors of the present invention have taken a different approach to modify the insulating paper by nano-alumina to obtain improved electrical properties. In particular, the inventors investigated the effects of different nano-alumina content on the AC breakdown field strength, relative dielectric constant and dielectric loss factor of insulating paper, and proposed that the addition of nano-alumina can improve the breakdown performance of insulating paper. Program.
根据本发明的一个方面，提供了一种纳米氧化铝改性绝缘纸制备方法，包括：According to an aspect of the invention, a method for preparing a nano-alumina modified insulating paper, comprising:
a.将纳米氧化铝溶解以形成一溶液； a. dissolving the nano-alumina to form a solution;
b.将纤维素绝缘纸解离至少一次，以形成纸浆溶液；b. dissociating the cellulose insulation paper at least once to form a pulp solution;
c.将溶解有纳米氧化铝的溶液加入该纸浆溶液后将所合成的合成溶液机械振荡并匀速搅拌；c. adding the solution in which the nano-alumina is dissolved to the pulp solution, and mechanically oscillating the synthesized solution to be stirred at a constant speed;
d.用经机械振荡并匀速搅拌的该合成溶液形成纳米氧化铝改性绝缘纸。d. Forming a nano-alumina modified insulating paper with the synthetic solution mechanically oscillated and uniformly stirred.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该溶液是乙醇溶液，且该步骤a进一步包括将该溶解有纳米氧化铝的乙醇溶液进行水浴超声振荡。Preferably, in the above method for preparing nano-alumina modified insulating paper, the solution is an ethanol solution, and the step a further comprises ultrasonically oscillating the ethanol solution in which the nano-alumina is dissolved in a water bath.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，在该步骤a之前，该纳米氧化铝改性绝缘纸制备方法还包括用硅烷偶联剂表面处理该纳米氧化铝。Preferably, in the above method for preparing nano-alumina modified insulating paper, before the step a, the method for preparing the nano-alumina modified insulating paper further comprises surface treating the nano-alumina with a silane coupling agent.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该用硅烷偶联剂表面处理该纳米氧化铝的步骤进一步包括：Preferably, in the above method for preparing nano-alumina modified insulating paper, the step of surface treating the nano-alumina with a silane coupling agent further comprises:
将KH-550硅烷偶联剂加入乙醇溶液后进行搅拌；KH-550 silane coupling agent is added to the ethanol solution and stirred;
在搅拌过程中加入纳米氧化铝；Adding nano-alumina during the stirring process;
在搅拌后，将混合有KH-550硅烷偶联剂和纳米氧化铝的溶液水浴超声振荡；以及After stirring, ultrasonically oscillate a solution water bath mixed with a KH-550 silane coupling agent and nano-alumina;
经洗涤、干燥后得到经表面处理的纳米氧化铝。After washing and drying, surface-treated nano-alumina is obtained.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该纳米氧化铝的质量至少为该硅烷偶联剂的质量的5倍。Preferably, in the above method for preparing nano-alumina modified insulating paper, the nano-alumina has a mass of at least 5 times the mass of the silane coupling agent.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该步骤b进一步包括以每次2.1万转的方式在纤维解离器中将该纤维素绝缘纸解离5次。Preferably, in the above method for preparing nano-alumina modified insulating paper, the step b further comprises dissociating the cellulose insulating paper 5 times in a fiber disintegrator at a time of 21,000 revolutions.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该步骤c进一步包括以每次2.1万转的方式在纤维解离器中将该合成溶液超声振荡并匀速搅拌至少10分钟。Preferably, in the above method for preparing nano-alumina modified insulating paper, the step c further comprises ultrasonically oscillating and synthesizing the synthetic solution in the fiber disintegrator at a time of 21,000 revolutions for at least 10 minutes.
较佳地，在上述的纳米氧化铝改性绝缘纸制备方法中，该步骤d进一步包括：Preferably, in the above method for preparing nano-alumina modified insulating paper, the step d further comprises:
将经解离的该合成溶液成型为半成纸；Dissolving the dissociated synthetic solution into a semi-formed paper;
对该半成纸进行真空干燥；Vacuuming the semi-formed paper;
将经真空干燥的半成纸置于自封袋水平衡一预定时间，以完成制备。The vacuum dried semi-finished paper is placed in a water of the zipper bag for a predetermined time to complete the preparation.
根据本发明的另一方面，提供一种纳米氧化铝改性绝缘纸，纳米氧化铝在该纳米氧化铝改性绝缘纸中的含量为0.2～2％。 According to another aspect of the present invention, a nano-alumina modified insulating paper is provided, and the content of the nano-alumina in the nano-alumina modified insulating paper is 0.2 to 2%.
较佳地，在上述的纳米氧化铝改性绝缘纸中，该纳米氧化铝在该纳米氧化铝改性绝缘纸中的含量为1％。Preferably, in the above nano-alumina modified insulating paper, the content of the nano-alumina in the nano-alumina modified insulating paper is 1%.
综上所述，本发明利用纳米氧化铝对绝缘纸进行改性，以提高绝缘纸的交流击穿强度，降低绝缘纸的工频相对介电常数及介质损耗因数。这不仅可以提高绝缘纸的耐击穿能力；而且可以使绝缘纸与变压器矿物油的相对介电常数更接近，外施电场在油纸介质中的分布就更趋均匀，油纸复合绝缘系统的整体电气强度就更高；同时，减少绝缘纸的有功及无功损耗，从而降低绝缘故障发生的概率。In summary, the present invention utilizes nano-alumina to modify the insulating paper to improve the AC breakdown strength of the insulating paper and reduce the power-frequency relative dielectric constant and dielectric loss factor of the insulating paper. This not only improves the breakdown resistance of the insulating paper, but also makes the relative dielectric constant of the insulating paper and the transformer mineral oil closer. The distribution of the applied electric field in the oil-paper medium is more uniform, and the overall electrical properties of the oil-paper composite insulation system. The strength is higher; at the same time, the active and reactive losses of the insulating paper are reduced, thereby reducing the probability of occurrence of insulation failure.
应当理解，本发明以上的一般性描述和以下的详细描述都是示例性和说明性的，并且旨在为如权利要求所述的本发明提供进一步的解释。The foregoing description of the preferred embodiments of the present invention
附图说明DRAWINGS
包括附图是为提供对本发明进一步的理解，它们被收录并构成本申请的一部分，附图示出了本发明的实施例，并与本说明书一起起到解释本发明原理的作用。附图中：The accompanying drawings are included to provide a further understanding of the embodiments of the invention In the figure:
图1示出了本发明的纳米氧化铝改性绝缘纸制备方法的基本步骤的流程图。BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 is a flow chart showing the basic steps of a method for preparing a nano-alumina modified insulating paper of the present invention.
图2示出了交流击穿强度随纳米氧化铝含量变化的关系。Figure 2 shows the relationship between the AC breakdown strength as a function of nano-alumina content.
图3示出了不同纳米氧化铝含量下的相对介电常数的曲线。Figure 3 shows the relative dielectric constant curves for different nano-alumina contents.
图4示出了不同纳米氧化铝含量下的介质损耗因数的曲线。Figure 4 shows a plot of dielectric loss factor for different nano-alumina contents.
具体实施方式detailed description
现在将详细参考附图描述本发明的实施例。Embodiments of the present invention will now be described in detail with reference to the drawings.
本发明的发明人再已知绝缘纸手抄片制备平台的基础上探索了纳米粒子改性绝缘纸的制备工艺，并通过对制备好的添加不同纳米氧化铝含量的改性绝缘纸及未改性的普通绝缘纸进行真空浸油处理、测试各绝缘纸的交流击穿场强、相对介电常数及介质损耗因数，从而进一步得到了可显著改善绝缘纸电气性能的相关制备工艺及其工艺参数。 The inventors of the present invention furtherly studied the preparation process of the nanoparticle modified insulating paper based on the preparation platform of the insulating paper handsheet, and adopted the modified insulating paper which is prepared by adding different nanometer alumina contents and has not been modified. The ordinary insulating paper is vacuum immersed in oil, and the AC breakdown field strength, relative dielectric constant and dielectric loss factor of each insulating paper are tested, thereby further obtaining a related preparation process and process parameters which can significantly improve the electrical properties of the insulating paper. .
首先参考图1，该图示出了本发明的纳米氧化铝改性绝缘纸制备方法100的基本步骤。该纳米氧化铝改性绝缘纸制备方法100主要包括：将纳米氧化铝(例如，β型、30nm、多孔性、高分散、高活性的纳米氧化铝)溶解，以形成一溶液(步骤101)；将纤维素绝缘纸解离至少一次，以形成纸浆溶液(步骤102)；将溶解有纳米氧化铝的溶液加入该纸浆溶液后将所合成的合成溶液机械振荡并均匀搅拌，为了使改性纳米氧化铝均匀分布(步骤103)；以及用经机械振荡并均匀搅拌的该合成溶液形成纳米氧化铝改性绝缘纸(步骤104)。Referring first to Figure 1, there is shown the basic steps of a method 100 of making a nano-alumina modified insulating paper of the present invention. The nano alumina modified insulating paper preparation method 100 mainly comprises: dissolving nano alumina (for example, β type, 30 nm, porous, highly dispersed, high activity nano alumina) to form a solution (step 101); Dissolving the cellulose insulating paper at least once to form a pulp solution (step 102); adding the solution in which the nano-alumina is dissolved to the pulp solution, and mechanically oscillating and synthesizing the synthesized synthetic solution for the purpose of modifying the nano-oxidation The aluminum is uniformly distributed (step 103); and the nano-alumina modified insulating paper is formed using the synthetic solution mechanically oscillated and uniformly stirred (step 104).
以下结合一个具体示例来讨论图1所示的纳米氧化铝改性绝缘纸制备方法的一种具体实施方式。A specific embodiment of the method for preparing nano-alumina modified insulating paper shown in FIG. 1 is discussed below in conjunction with a specific example.
例如，在步骤101中，先根据要制备的绝缘纸所需的氧化铝含量称取一定质量的经表面处理(该表面处理将在以下更详细地讨论)的纳米氧化铝，将该纳米氧化铝溶解于乙醇溶液，例如浓度为约95％的乙醇溶液。接着，在步骤101中可以进一步将该溶解有纳米氧化铝的乙醇溶液水浴超声振荡，例如置于KQ-100KDE型超声波清洗器中在约70度下水浴超声振荡约10分钟。For example, in step 101, a certain amount of nano-alumina that has been surface treated (this surface treatment will be discussed in more detail below) is weighed according to the alumina content required for the insulating paper to be prepared, and the nano-alumina is Dissolved in an ethanol solution, such as a solution of ethanol at a concentration of about 95%. Next, in step 101, the ethanol solution in which the nano-alumina is dissolved may be further ultrasonically shaken, for example, in a KQ-100KDE type ultrasonic cleaner, and ultrasonically shaken in a water bath at about 70 degrees for about 10 minutes.
接着，在步骤102中，基于已知的绝缘纸手抄片抄造平台，在纤维解离器中以约每次2.1万转的方式将纤维素绝缘纸(即普通的纤维素绝缘纸)解离至少一次，例如5次，以形成纸浆溶液。将溶解有纳米氧化铝的溶液加入该纸浆溶液后将所合成的合成溶液超声振荡并匀速搅拌至少10分钟，步骤103。步骤102和步骤103中的解离方式例如可以相同的，或者也可以根据需要而任意调整步骤102或步骤103中的旋转次数和旋转方式以满足制备要求。Next, in step 102, the cellulose insulating paper (ie, ordinary cellulose insulating paper) is dissociated in the fiber disintegrator at about 21,000 revolutions per time based on a known insulating paper handsheet forming platform. At least once, for example 5 times, to form a pulp solution. After the solution in which the nano-alumina is dissolved is added to the pulp solution, the synthesized solution is ultrasonically shaken and stirred at uniform for at least 10 minutes, step 103. The dissociation modes in step 102 and step 103 may be the same, for example, or the number of rotations and the rotation mode in step 102 or step 103 may be arbitrarily adjusted as needed to meet the preparation requirements.
最后，在步骤104中，先通过纸片成型器将经解离的该合成溶液成型、揭纸，以获得半成纸；再对该半成纸进行真空干燥，例如将半成纸置于真空干燥室中在约105℃下真空干燥约5分钟，以便去除半成纸中的水和乙醇；之后，将经真空干燥的半成纸置于自封袋水平衡一预定时间，比如24小时，以完成制备，形成纳米氧化铝改性绝缘纸。Finally, in step 104, the dissociated synthetic solution is first formed and uncoated by a paper sheet former to obtain a semi-formed paper; and the semi-formed paper is vacuum dried, for example, a semi-formed paper is placed in a vacuum. Drying in a drying chamber at about 105 ° C for about 5 minutes to remove water and ethanol in the semi-formed paper; after that, the vacuum-dried semi-formed paper is placed in a water of the zipper bag for a predetermined time, such as 24 hours, to The preparation is completed to form a nano-alumina modified insulating paper.
特别是，由于纳米氧化铝属于无机材料而纤维素绝缘纸中纤维素属于有机物质，如果直接将纳米氧化铝掺杂至该纤维素绝缘纸中，由于两相间的不相容性，可能会影响无机粒子的分散，进而影响两相间的形态结构和界面性质。因 此，根据本发明的一个优选实施例，在掺杂(即上述的步骤101)之前，本发明的该纳米氧化铝改性绝缘纸制备方法100可以进一步包括用硅烷偶联剂表面处理该纳米氧化铝的步骤。In particular, since nano-alumina is an inorganic material and cellulose in cellulose-insulated paper is an organic substance, if nano-alumina is directly doped into the cellulose-insulating paper, it may be affected due to incompatibility between the two phases. The dispersion of inorganic particles, in turn, affects the morphological structure and interfacial properties between the two phases. Cause Thus, in accordance with a preferred embodiment of the present invention, the nano-alumina modified insulating paper preparation method 100 of the present invention may further comprise surface treating the nano-oxidation with a silane coupling agent prior to doping (ie, step 101 above). The step of aluminum.
例如，该用硅烷偶联剂表面处理该纳米氧化铝的步骤可以进一步包括：将硅烷偶联剂(基于连接纳米氧化铝和纤维素并提升纳米氧化铝分散程度的原因，优选氨类硅烷偶联剂KH-550)加入乙醇溶液(例如浓度为95％的乙醇溶液)后进行搅拌；在搅拌过程中加入纳米氧化铝，其中该纳米氧化铝的质量优选为该KH-550硅烷偶联剂的质量的至少5倍，更优选为10倍(例如，选取5g纳米氧化铝和0.5g KH-550硅烷偶联剂加入约300ml的95％乙醇溶液中进行搅拌)；在搅拌后，将混合有KH-550硅烷偶联剂和纳米氧化铝的溶液水浴超声振荡(例如，在上述的选取5g纳米氧化铝和0.5g KH-550硅烷偶联剂加入约300ml的95％乙醇溶液中进行搅拌的示例中，在约70度下水浴超声振荡约5小时)；以及经洗涤、干燥后得到经表面处理的纳米氧化铝，例如该洗涤和干燥步骤可以重复执行数次。For example, the step of surface treating the nano-alumina with a silane coupling agent may further comprise: silane coupling agent (based on linking nano-alumina and cellulose and increasing the degree of dispersion of the nano-alumina, preferably ammonia-based silane coupling Agent KH-550) is added to an ethanol solution (for example, a 95% ethanol solution) and then stirred; during the stirring process, nano-alumina is added, wherein the mass of the nano-alumina is preferably the mass of the KH-550 silane coupling agent At least 5 times, more preferably 10 times (for example, 5 g of nano-alumina and 0.5 g of KH-550 silane coupling agent are added to about 300 ml of a 95% ethanol solution for stirring); after stirring, KH- is mixed. Ultrasonic shaking of a solution bath of 550 silane coupling agent and nano-alumina (for example, in the above-mentioned example in which 5 g of nano-alumina and 0.5 g of KH-550 silane coupling agent are added to a solution of about 300 ml of 95% ethanol for stirring, Ultrasonic shaking in a water bath at about 70 degrees for about 5 hours); and surface-treated nano-alumina is obtained after washing and drying, for example, the washing and drying steps can be repeated several times.
在纳米改性绝缘纸的击穿性能测试过程中，对制备好的添加不同纳米氧化铝含量(0.2％、0.5％、1％、2％、4％、7％)的改性绝缘纸及未改性的普通绝缘纸进行真空浸油处理，利用实验室交流击穿测试平台测试绝缘纸的交流击穿强度，利用实验室的Concept 80宽频介电仪测试绝缘纸的相对介电常数及介质损耗因数。各参数随纳米氧化铝含量变化的关系图如图2-4所示。In the process of testing the breakdown performance of nano-modified insulating paper, the modified insulating paper with different nano-alumina content (0.2%, 0.5%, 1%, 2%, 4%, 7%) is prepared and not The modified ordinary insulating paper is subjected to vacuum immersion treatment, and the AC breakdown strength of the insulating paper is tested by a laboratory AC breakdown test platform, and the relative dielectric constant and dielectric loss of the insulating paper are tested by the laboratory Concept 80 broadband dielectric meter. Factor. The relationship between the parameters and the change of nano-alumina content is shown in Figure 2-4.
如图2所示，对于绝缘纸的交流击穿强度，随着纳米氧化铝含量的增加，绝缘纸的交流击穿强度逐步增大，当含量达到1％时击穿强度达到极大值(66.14kV/mm)，相比普通绝缘纸(59.68kV/mm)提高了10.8％。之后随着纳米氧化铝含量的增加，击穿强度快速下降，并且在含量增大至4％后，绝缘纸的击穿强度低于未改性的普通绝缘纸。As shown in Fig. 2, for the AC breakdown strength of the insulating paper, as the content of nano-alumina increases, the AC breakdown strength of the insulating paper gradually increases, and the breakdown strength reaches a maximum when the content reaches 1% (66.14). kV/mm), which is 10.8% higher than ordinary insulating paper (59.68kV/mm). Then, as the content of nano-alumina increases, the breakdown strength decreases rapidly, and after the content increases to 4%, the breakdown strength of the insulating paper is lower than that of the unmodified ordinary insulating paper.
另一方面，如图3和图4所示，绝缘纸的相对介电常数及介质损耗因数随着纳米氧化铝的增加而不断减小，尤其在工频下1％含量的纳米改性纸有明显的降低。其相对介电常数和介质损耗因数分别从2.43，1.38x10-2(普通绝缘纸)，降低到2.26，0.739x10-2(改性绝缘纸)。综上，相比于普通绝缘纸，纳米氧化铝含量为1％的改性绝缘纸工频介电常数降低了7％，工频介质损耗因数降低了 46.4％。On the other hand, as shown in Fig. 3 and Fig. 4, the relative dielectric constant and dielectric loss factor of the insulating paper are continuously reduced with the increase of nano-alumina, especially at the power frequency, the 1% content of the nano-modified paper has Significantly lower. Its relative dielectric constant and dielectric loss factor were reduced from 2.43, 1.38x10 -2 (ordinary insulating paper) to 2.26, 0.739x10 -2 (modified insulating paper). In summary, compared with ordinary insulating paper, the dielectric constant of the modified insulating paper with a nano-alumina content of 1% is reduced by 7%, and the power-frequency dielectric loss factor is reduced by 46.4%.
通过综合比较不同纳米氧化铝含量对绝缘纸的交流击穿场强、相对介电常数及介质损耗因数的影响，本发明的发明人发现当改性绝缘纸中的纳米氧化铝含量为约0.2～2％时，其掺杂均可提升绝缘纸的击穿性能。特别是，纳米氧化铝在绝缘纸中的最佳添加比例为1％，此时改性绝缘纸的交流击穿场强可以提高10.8％、工频介电常数可以降低7％、工频介质损耗因数可以降低46.4％。By comprehensively comparing the effects of different nano-alumina contents on the AC breakdown field strength, relative dielectric constant and dielectric loss factor of the insulating paper, the inventors of the present invention found that the content of nano-alumina in the modified insulating paper is about 0.2 ～. At 2%, the doping can improve the breakdown performance of the insulating paper. In particular, the optimum addition ratio of nano-alumina in insulating paper is 1%. At this time, the alternating breakdown field strength of the modified insulating paper can be increased by 10.8%, the dielectric frequency dielectric constant can be reduced by 7%, and the power frequency dielectric loss can be reduced. The factor can be reduced by 46.4%.
综上所述，本发明利用纳米氧化铝对绝缘纸进行改性，以提高绝缘纸的交流击穿强度，降低绝缘纸的工频相对介电常数及介质损耗因数。这不仅可以提高绝缘纸的耐击穿能力；而且可以使绝缘纸与变压器矿物油的相对介电常数更接近，外施电场在油纸介质中的分布就更趋均匀，油纸复合绝缘系统的整体电气强度就更高；同时，减少绝缘纸的有功及无功损耗，从而降低绝缘故障发生的概率。In summary, the present invention utilizes nano-alumina to modify the insulating paper to improve the AC breakdown strength of the insulating paper and reduce the power-frequency relative dielectric constant and dielectric loss factor of the insulating paper. This not only improves the breakdown resistance of the insulating paper, but also makes the relative dielectric constant of the insulating paper and the transformer mineral oil closer. The distribution of the applied electric field in the oil-paper medium is more uniform, and the overall electrical properties of the oil-paper composite insulation system. The strength is higher; at the same time, the active and reactive losses of the insulating paper are reduced, thereby reducing the probability of occurrence of insulation failure.
本领域技术人员可显见，可对本发明的上述示例性实施例进行各种修改和变型而不偏离本发明的精神和范围。因此，旨在使本发明覆盖落在所附权利要求书及其等效技术方案范围内的对本发明的修改和变型。 It is apparent to those skilled in the art that various modifications and variations can be made in the above-described embodiments of the present invention without departing from the spirit and scope of the invention. Therefore, it is intended that the present invention cover the modifications and modifications of the invention

Claims (10)

  1. 一种纳米氧化铝改性绝缘纸制备方法，其特征在于，包括：A method for preparing nano-alumina modified insulating paper, which comprises:
    a.将纳米氧化铝溶解以形成一溶液；a. dissolving the nano-alumina to form a solution;
    b.将纤维素绝缘纸解离至少一次，以形成纸浆溶液；b. dissociating the cellulose insulation paper at least once to form a pulp solution;
    c.将溶解有纳米氧化铝的溶液加入所述纸浆溶液后将所合成的合成溶液机械振荡并匀速搅拌；c. adding the solution in which the nano-alumina is dissolved to the pulp solution, and mechanically oscillating the synthesized solution to be stirred at a constant speed;
    d.用经机械振荡并匀速搅拌的所述合成溶液形成纳米氧化铝改性绝缘纸。d. Forming a nano-alumina modified insulating paper with the synthetic solution mechanically oscillated and stirred at a constant rate.
  2. 如权利要求1所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，所述溶液是乙醇溶液，且所述步骤a进一步包括将所述溶解有纳米氧化铝的乙醇溶液进行水浴超声振荡。The method for preparing nano-alumina modified insulating paper according to claim 1, wherein the solution is an ethanol solution, and the step a further comprises performing ultrasonic bath shaking in the ethanol solution in which the nano-alumina is dissolved. .
  3. 如权利要求1所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，在所述步骤a之前，所述纳米氧化铝改性绝缘纸制备方法还包括用硅烷偶联剂表面处理所述纳米氧化铝。The method for preparing nano-alumina modified insulating paper according to claim 1, wherein before the step a, the method for preparing the nano-alumina modified insulating paper further comprises surface treating the surface with a silane coupling agent. Nano alumina.
  4. 如权利要求3所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，所述用硅烷偶联剂表面处理所述纳米氧化铝的步骤进一步包括：The method for preparing a nano-alumina modified insulating paper according to claim 3, wherein the step of surface treating the nano-alumina with a silane coupling agent further comprises:
    将KH-550硅烷偶联剂加入乙醇溶液后进行搅拌；KH-550 silane coupling agent is added to the ethanol solution and stirred;
    在搅拌过程中加入纳米氧化铝；Adding nano-alumina during the stirring process;
    在搅拌后，将混合有KH-550硅烷偶联剂和纳米氧化铝的溶液水浴超声振荡；以及After stirring, ultrasonically oscillate a solution water bath mixed with a KH-550 silane coupling agent and nano-alumina;
    经洗涤、干燥后得到经表面处理的纳米氧化铝。After washing and drying, surface-treated nano-alumina is obtained.
  5. 如权利要求4所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，所述纳米氧化铝的质量至少为所述硅烷偶联剂的质量的5倍。 The method for preparing nano-alumina modified insulating paper according to claim 4, wherein the nano-alumina has a mass of at least 5 times the mass of the silane coupling agent.
  6. 如权利要求1所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，所述步骤b进一步包括以每次2.1万转的方式在纤维解离器中将所述纤维素绝缘纸解离5次The method for preparing nano-alumina modified insulating paper according to claim 1, wherein said step b further comprises dissociating said cellulose insulating paper in a fiber disintegrator in a manner of 21,000 revolutions each time. 5 times
  7. 如权利要求1所述的纳米氧化铝改性绝缘纸制备方法，其特征在于，所述步骤c进一步包括以每次2.1万转的方式在纤维解离器中将所述合成溶液超声振荡并匀速搅拌至少10分钟。The method for preparing nano-alumina modified insulating paper according to claim 1, wherein the step c further comprises ultrasonically oscillating and synthesizing the synthetic solution in a fiber disintegrator in a manner of 21,000 revolutions each time. Stir for at least 10 minutes.
  8. 如权利要求1所述的纳米氧化铝改性纳米氧化铝改性绝缘纸制备方法，其特征在于，所述步骤d进一步包括：The method for preparing a nano-alumina modified nano-alumina modified insulating paper according to claim 1, wherein the step d further comprises:
    将经解离的所述合成溶液成型为半成纸；Forming the dissociated synthetic solution into a semi-formed paper;
    对所述半成纸进行真空干燥；Vacuuming the semi-formed paper;
    将经真空干燥的半成纸置于自封袋水平衡一预定时间，以完成制备。The vacuum dried semi-finished paper is placed in a water of the zipper bag for a predetermined time to complete the preparation.
  9. 一种纳米氧化铝改性绝缘纸，其特征在于，纳米氧化铝在所述纳米氧化铝改性绝缘纸中的含量为0.2～2％。A nano-alumina modified insulating paper, characterized in that the content of nano-alumina in the nano-alumina modified insulating paper is 0.2 to 2%.
  10. 如权利要求9所述的纳米氧化铝改性绝缘纸，其特征在于，所述纳米氧化铝在所述纳米氧化铝改性绝缘纸中的含量为1％。 The nano-alumina modified insulating paper according to claim 9, wherein the content of the nano-alumina in the nano-alumina modified insulating paper is 1%.
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